Abstract:
Methods are provided for rapidly determining the presence or absence of large numbers of contaminants in a test sample, such as a raw material intended for use in the preparation of a nutraceutical. The disclosed methods employ gas chromatography-mass spectrometry techniques together with the specific use of software in combination with a database to analyze data collected after ionization of the sample and determine the presence or absence of the contaminants in the sample.

Description:
REFERENCE TO RELATED APPLICATIONS 
       [0001]    This application claims priority to U.S. provisional patent application No. 61/718,607, filed Oct. 25, 2012. 
     
    
     TECHNICAL FIELD 
       [0002]    The present disclosure relates to methods for rapidly determining the presence or absence of multiple contaminants in a test sample, such as a raw material intended for use in the preparation of a nutraceutical, using gas chromatography-mass spectrometry techniques. 
       BACKGROUND 
       [0003]    As the use of nutraceuticals, such as multivitamins and other dietary supplements, has become more commonplace, concerns over the levels of purity, quality, consistency and potency of such supplements have increased. Ensuring that nutritional and dietary supplements are free of contaminants is particularly important when the supplements are intended for use by children and/or individuals with health problems, environmental sensitivities, etc. The US Food and Drug Administration (FDA) regulates dietary supplements as a category of foods and not as drugs, meaning that dietary supplements do not need to be specifically pre-approved by the FDA. In 2007, the FDA implemented a current Good Manufacturing Practices (cGMP) policy in an attempt to ensure that dietary supplements do not contain contaminants or impurities and are accurately labeled. However, the level of non-compliance with the cGMP is very high. Based on audits completed by the FDAs compliance division in 2011 and 2012, it has been estimated that nearly 70% of dietary supplement manufacturers are non-compliant with the cGMP policy. Significant concerns thus remain over the quality of nutritional and dietary supplements on the market today. 
         [0004]    Many supplement companies obtain the raw materials for their supplements from a variety of suppliers, and then use those materials to formulate supplements for sale. Over 80% of the raw materials used in nutraceuticals sold in the US come from China and other non-US countries, leading to additional concerns over potential levels of contamination. 
         [0005]    Methods that are typically employed to check for contaminants in raw materials, such as those used in nutraceuticals, are time consuming and expensive. There thus remains a need for methods that can rapidly and cost-effectively identify the presence or absence of, and/or determine the levels of, a large number of contaminants in raw materials intended for use in one or more dietary supplements. 
       SUMMARY 
       [0006]    The present invention provides methods for rapidly and accurately determining the presence or absence of, and/or quantifying the amount of, a large number of contaminants, such as pesticides, in a sample. In certain embodiments, the methods disclosed herein are employed to test for the presence or absence of contaminants, such as pesticides, in raw materials intended for use in nutraceuticals, such as vitamins and dietary supplements. Such raw materials include, but are not limited to, minerals and plant-based materials such as those listed in Table 1, below. 
         [0007]    In one embodiment, methods for detecting the presence or absence of a plurality of contaminants in a sample are provided, such methods comprising: (a) extracting the sample with a water-miscible solvent in the presence of a high concentration of salts to provide a sample extract; (b) shaking and centrifuging the sample extract to provide a supernatant; (c) exchanging the water-miscible solvent in the supernatant for an organic, preferably non-water miscible, solvent methylene chloride to provide a treated supernatant; (d) analyzing the treated supernatant using gas chromatography-mass spectrometry (GC-MS) to provide a total ion chromatogram; (e) deconvoluting the total ion chromatogram to provide non-overlapping spectra; and (f) comparing the non-overlapping spectra with standard mass spectra for the plurality of contaminants, wherein the standard mass spectra are contained in a retention time-locked database. In certain embodiments, the water-miscible solvent is selected from the group consisting of: acetonitrile, ethyl acetate or acetone. In a preferred embodiment, the water-miscible solvent is acetonitrile. In certain embodiments, the organic non-water-miscible solvent is selected from the group consisting of: methylene chloride, hexane and toluene. In a preferred embodiment, the non-water-miscible solvent is methylene chloride. 
         [0008]    Such methods can be used to quickly detect the presence or absence of at least 50, 100, 150, 200, 250, 300, 350, 400, 450, 500, 550, 600, 650, 700, 750, 800, 850 or 900 contaminants. In certain embodiments, the disclosed methods are employed to detect the presence or absence of a plurality of compounds selected from those listed in Table 2, below. 
         [0009]    In one embodiment, an initial analysis is performed to determine whether or not one or more specific contaminants are present in a sample (i.e. to give a simple “yes or no” result). If this initial analysis indicates that the contaminant is indeed present, a second analysis is performed to determine the amount of the contaminant in the sample. In certain embodiments, the second analysis is performed using GC-MS. 
       DEFINITIONS 
       [0010]    As used herein, the term “deconvolution” refers to a mathematical technique that separates overlapping mass spectra (i.e. overlapping peaks in a total ion chromatogram (TIC)) into clean spectra of individual components. 
         [0011]    As used herein, the term “high concentration of salts” refers to an amount of salts sufficient to provide a solution having a percentage composition by mass of salts between 40% and 90%, such as between 50% and 80% or between 60% and 70%. In certain embodiments, the term “high concentration of salts” refers to an amount of salts sufficient to provide a salt solution having approximately 65% composition by mass of salts. In one specific embodiment, the methods disclosed herein employ 4 g MgSO 4 , 1 g NaCl, 1 g trisodium citrate dehydrate and 0.5 g disodium hydrogen citrate sesquihydrate in 10 ml of solution. 
         [0012]    As used herein, the term “nutraceutical” refers to food, or parts of food, that provide medical or health benefits, including the prevention and treatment of disease, and that are intended for consumption by a human or other mammal. The term nutraceutical encompasses, but is not limited to, dietary supplements including botanicals, vitamins, minerals, co-enzyme Q, carnitine, ginseng, gingko biloba, Saint John&#39;s Wort, saw palmetto, prebiotics and probiotics. 
         [0013]    As used herein, the term “retention time-locking” refers to the matching of a first set of retention times obtained using a known chromatographic method having a defined set of column parameters and operating parameters to a second set of retention times obtained using a new, different, chromatographic method having a new, different, set of column parameters, wherein the second set of retention times are matched, or locked, to the first set of retention times. 
     
    
     DETAILED DESCRIPTION 
       [0014]    As outlined above, the present disclosure provides rapid and cost-effective methods for detecting the presence or absence of multiple contaminants in a sample, such as raw materials for use in the preparation of a nutraceutical. Prior to analysis using GC-MS, the sample is extracted using a modified QuEChERS (Quick Easy Cheap Effective Rugged Safe) technique described in detail below. QuEChERS is a method for testing for pesticides that was developed by Michelangelo Anastassiades (Anastassiades et al., J. AOAC Int., 86:412-431 (2003)). This method entails solvent extraction of samples with acetonitrile, ethyl acetate or acetone, and partitioning with magnesium sulfate, either alone or in combination with other salts followed by clean-up using dispersive solid phase extraction (DSPE). More specifically, the sample is first extracted with a water-miscible solvent, such as acetonitrile, in the presence of a high concentration of salts (e.g. sodium chloride and magnesium sulfate) and buffering agents (e.g. citrate) to induce liquid separation and stabilize acidic and basic labile pesticides, respectively. After shaking and centrifugation, an aliquot of the organic phase is subjected to further clean up using DSPE. The resulting mixture is centrifuged and the resulting supernatant can either be analyzed directly or subjected to a concentration and solvent exchange step, if necessary, prior to analysis. 
         [0015]    The extracted samples are then subjected to GC-MS analysis using methods well known to those of skill in the art and described below. The total ion chromatogram is deconvoluted as necessary using publicly available software, such as AMDIS (Automated Mass Spectral Deconvolution and Identification System; available from the National Institute of Standards and Technology (NIST)), Chemstation™ and/or DRS (Agilent Technologies, Inc. Santa Clara, Calif.). 
         [0016]    The resulting spectra are compared with standard mass spectra for the contaminants of interest that are contained within a database that includes internal calibrations, such as a retention time-locked (RTL) database. Methods for automated retention time-locking are known in the art and include, for example those taught in U.S. Pat. No. 5,987,959. In certain embodiments, the resulting spectra are compared with those contained in a RTL pesticide database, such as the RTL Pesticide Library available from Agilent Technologies, Inc. This database contains locked retention time, compound name, CAS number, molecular weight and mass spectrum for 927 compounds, including pesticides, metabolite and endocrine disrupters, and other known contaminants. Using a RTL database eliminates the need to re-calibrate the GC-MS system for each potential contaminant and thus significantly reduces the time required to test a sample for the presence or absence of multiple contaminants. 
         [0017]    Raw materials that can be analyzed using the methods disclosed herein include, but are not limited to, those shown in Table 1, below. 
         [0000]    
       
         
               
               
             
           
               
                   
                 TABLE 1 
               
               
                   
                   
               
             
             
               
                   
                 Acetyl L-Carnitine HCL 
               
               
                   
                 Adipic Acid FCC 
               
               
                   
                 Alpha Ketoglutaric Acid 
               
               
                   
                 Ascorbic Acid (Vit. C-90) 
               
               
                   
                 Ascorbic Acid (Vit. C-90) 
               
               
                   
                 Ascorbic Acid Crystals (Vit. C) 
               
               
                   
                 Astragalus Root Extract Powder 
               
               
                   
                 Beta Carotene 
               
               
                   
                 Beta Carotene 10% 
               
               
                   
                 Beta Carotene 20% 
               
               
                   
                 Calcium Alpha Ketoglutarate 
               
               
                   
                 Calcium Caprylate 
               
               
                   
                 Calcium Carbonate Granular 
               
               
                   
                 Calcium Carbonate Powder 
               
               
                   
                 Calcium Carbonate Powder(CE Low Lead) 
               
               
                   
                 Calcium Citrate Powder 
               
               
                   
                 Calcium Citrate Tetrahydrate Granular 
               
               
                   
                 Calcium D-Glucarate 
               
               
                   
                 Calcium Folinate (Folinic Acid) 
               
               
                   
                 Calcium Glycinate Chelate 
               
               
                   
                 Calcium Magnesium Phytate 
               
               
                   
                 Calcium Pantothenate (B-5) 
               
               
                   
                 Choline Dihydrogen Citrate 
               
               
                   
                 Citric Acid Anhydrous Granular 
               
               
                   
                 Citric Acid Anhydrous Powder 
               
               
                   
                 Cobamamide (Vit. B-12 Coenzyme) 
               
               
                   
                 Cod Liver Oil (Vitamin A Assay) 
               
               
                   
                 Coenzyme Q10 
               
               
                   
                 Cupric Oxide 
               
               
                   
                 Cyanocobalamin Crystals (Vit. B-12) 
               
               
                   
                 D-Biotin 1% 
               
               
                   
                 D-Biotin Pure 
               
               
                   
                 DHEA (Dehydroepiandrosterone) 
               
               
                   
                 Di-Calcium Phosphate Dihydrate 
               
               
                   
                 Di-Calcium Phosphate Powder 
               
               
                   
                 Di-magnesium Malate Granular 
               
               
                   
                 Dimethylaminoethanol (DMAE) 
               
               
                   
                 Dimethylglycine HCL (DMG) 
               
               
                   
                 Disodium EDTA 
               
               
                   
                 Elderberry PE 
               
               
                   
                 Ferrous Fumarate 
               
               
                   
                 Folic Acid 10% Trituration 
               
               
                   
                 Folic Acid USP 
               
               
                   
                 GABA 
               
               
                   
                 Glucosamine Sulfate Potassium Chloride 
               
               
                   
                 Glycine USP 
               
               
                   
                 Golden Seal Extract 
               
               
                   
                 Grape Seed Extract 
               
               
                   
                 Grapefruit Seed Powdered Extract 
               
               
                   
                 Idebenone 
               
               
                   
                 Inositol Granular 
               
               
                   
                 Inositol Hexanicotinate 
               
               
                   
                 Iron Amino Acid Chelate (Ferrochel) 
               
               
                   
                 Iron Choline Citrate Powder 
               
               
                   
                 L-Arginine HCL 
               
               
                   
                 L-Asparagine Monohydrate FCC 
               
               
                   
                 L-Carnosine 
               
               
                   
                 L-Creatine Monohydrate 
               
               
                   
                 L-Glutamine 
               
               
                   
                 L-Glutamine 
               
               
                   
                 L-Glutathione Reduced 
               
               
                   
                 Lipoic Acid 
               
               
                   
                 L-Isoleucine 
               
               
                   
                 Lithium Citrate 
               
               
                   
                 L-Leucine 
               
               
                   
                 L-Lysine Mono HCL 
               
               
                   
                 L-Methionine 
               
               
                   
                 L-Phenylalanine 
               
               
                   
                 L-Proline 
               
               
                   
                 L-Serine 
               
               
                   
                 L-Threonine 
               
               
                   
                 L-Tyrosine 
               
               
                   
                 L-Valine 
               
               
                   
                 Magnesium Alpha Ketoglutarate 
               
               
                   
                 Magnesium Ascorbate 
               
               
                   
                 Magnesium Chloride Hexahydrate 
               
               
                   
                 Magnesium Citrate 
               
               
                   
                 Magnesium Citrate Anhydrous 
               
               
                   
                 Magnesium Citrate Tribasic 
               
               
                   
                 Magnesium Glycinate Buffered 
               
               
                   
                 Magnesium Oxide Powder 
               
               
                   
                 Magnesium Oxide USP 
               
               
                   
                 Magnesium Stearate 
               
               
                   
                 Magnesium Sulfate USP 
               
               
                   
                 Magnesium Taurinate 
               
               
                   
                 Manganese Citrate 
               
               
                   
                 Manganese Sulfate Monohydrate 
               
               
                   
                 Marshmallow Root 
               
               
                   
                 Melatonin 
               
               
                   
                 Mesodimercaptosuccinic Acic (DMSA) 
               
               
                   
                 Methylcobalamin (Vit. B-12) 
               
               
                   
                 Methylcobalamin (Vit. B-12) 1% Trit in DCP 
               
               
                   
                 Methylcobalamin (Vit. B12) Pure 
               
               
                   
                 Methylparaben 
               
               
                   
                 Milk Thistle Powder 
               
               
                   
                 N-Acetyl Glucosamine 
               
               
                   
                 N-Acetyl L-Cysteine 
               
               
                   
                 Natural Beta Carotene in Sunflower 
               
               
                   
                 Niacinamide (Vit. B3) Rocoat 
               
               
                   
                 Niacinamide Granular USP (Vit. B-3) 
               
               
                   
                 Olive Leaf Extract 
               
               
                   
                 Oregano Extract 
               
               
                   
                 Para Amino Benzoic Acid (PABA) 
               
               
                   
                 Pau D′ Arco Bark Extract 
               
               
                   
                 Potassium Ascorbate Powder 
               
               
                   
                 Potassium Iodide 
               
               
                   
                 Potassium Sorbate 
               
               
                   
                 Propylparaben 
               
               
                   
                 Pycnogenol Extract 
               
               
                   
                 Pyridoxal-5-Phosphate (P5P) 
               
               
                   
                 Pyridoxine (Vit. B-6) HCL Powder 
               
               
                   
                 Pyridoxine HCL (Vit. B6) Granular 
               
               
                   
                 Pyrodoxine HCL (Vit. B-6) Rocoat 
               
               
                   
                 Quercetin Dihydrate 
               
               
                   
                 Resveratrol 
               
               
                   
                 Riboflavin (Vit. B-2) Phosphate 
               
               
                   
                 Riboflavin (Vit. B-2) Rocoat 
               
               
                   
                 Riboflavin USP (Vit. B-2) 
               
               
                   
                 Slippery Elm Bark 
               
               
                   
                 Sodium Ascorbate Crystalline 
               
               
                   
                 Sodium Ascorbate Powder 
               
               
                   
                 Sodium Benzoate Powder NF/FCC 
               
               
                   
                 Sodium Citrate Dihydrate 
               
               
                   
                 Sodium CMC 
               
               
                   
                 Sodium Fluoride USP 
               
               
                   
                 Stearic Acid (Veg. Grade) 
               
               
                   
                 Stevia Leaf Extract 
               
               
                   
                 Taurine (Ajinomoto) 
               
               
                   
                 Taurine (Pharmline) 
               
               
                   
                 Thiamine (Vit. B-1) Mononitrate 
               
               
                   
                 Thiamine HCL Powder USP 
               
               
                   
                 Thiamine Mononitrate (Vit. B-1) Rocoat 
               
               
                   
                 Thiamine Mononitrate Powder (Vit. B-1) 
               
               
                   
                 Trimethylglycine Powder (TMG) 
               
               
                   
                 Turmeric Root Extract 
               
               
                   
                 Vitacel 
               
               
                   
                 Vitamin A Acetate 
               
               
                   
                 Vitamin A Palmitate 
               
               
                   
                 Vitamin B-12 1% Trit in Mannitol 
               
               
                   
                 Vitamin D-3 100 MIU/g 
               
               
                   
                 Vitamin D-3 Pure 
               
               
                   
                 Vitamin E Acetate 50% 
               
               
                   
                 Vitamin E Acetate 75% 
               
               
                   
                 Vitamin E Acetate Oil 
               
               
                   
                 Vitamin K-1 5% SD, Dry 
               
               
                   
                 Zinc Amino Acid Chelate 
               
               
                   
                 Zinc Citrate Dihydrate 
               
               
                   
                 Zinc Ketoglutarate 
               
               
                   
                 Zinc Picolinate Powder 
               
               
                   
                 Zinc Sulfate 
               
               
                   
                   
               
             
          
         
       
     
         [0018]    Table 2 shows a list of potential contaminants that can be detected using the methods disclosed herein, as published in Wylie, “Screening for 926 Pesticides and Endocrine Disruptors by GC/MS with Deconvolution Reporting Software and a New Pesticide Library” Application Note, Agilent Technologies, Inc., 2006. 
         [0000]    
       
         
               
               
             
           
               
                   
                 TABLE 2 
               
               
                   
                   
               
             
             
               
                   
                 1,2,4-Trichlorobenzene 
               
               
                   
                 1,2-Dibromo-3-chloropropane 
               
               
                   
                 1,3,5-Tribromobenzene 
               
               
                   
                 1,3-Dichlorobenzene 
               
               
                   
                 17a-Ethynylestradiol 
               
               
                   
                 1-naphthalenol 
               
               
                   
                 2-(1-naphthyl)actamido 
               
               
                   
                 2-(2-Butoxyethoxy)ethyl thiocyanate 
               
               
                   
                 2-(Octylthio)ethanol 
               
               
                   
                 2,3,4,5-Tertrachloronitrobenzene 
               
               
                   
                 2,3,4,5-Tetrachlorophenol 
               
               
                   
                 2,3,4,6-Tetrachlorophenol 
               
               
                   
                 2,3,5,6-Tetrachlorophenol 
               
               
                   
                 2,3,5,6-Tetrachloro-p-terphenyl 
               
               
                   
                 2,3,5-Trichlorophenol 
               
               
                   
                 2,3,5-Trimethacarb 
               
               
                   
                 2,3,6-Trichloroanisole 
               
               
                   
                 2,3,7,8-Tetrachlorodibenzofuran 
               
               
                   
                 2,3,7,8-Tetrachlorodibenzo-p-dioxin 
               
               
                   
                 2,4,5,6-Tetrachloro-m-xylene 
               
               
                   
                 2,4,5-T methyl ester 
               
               
                   
                 2,4,5-Trichloroaniline 
               
               
                   
                 2,4,5-Trichlorophenol 
               
               
                   
                 2,4,5-Trichloro-p-terphenyl 
               
               
                   
                 2,4,5-Trimethylaniline 
               
               
                   
                 2,4,6-Tribromoanisole 
               
               
                   
                 2,4,6-Tribromophenol 
               
               
                   
                 2,4,8-Trichloroanisoln 
               
               
                   
                 2,4,8-Trichlorophenol 
               
               
                   
                 2,4-D methyl ester 
               
               
                   
                 2,4-D sac-butyl ester 
               
               
                   
                 2,4-DB methyl ester 
               
               
                   
                 2,4′-Dichlorobenzophenone (2,4′-Dicalol 
               
               
                   
                 decomposition product) 
               
               
                   
                 2,4-Dichlorophenol 
               
               
                   
                 2,4-Dichlorophenyl benzenesulfonate 
               
               
                   
                 2,4-Dimethylaniline 
               
               
                   
                 2,4-Dimethylphenol 
               
               
                   
                 2,8-Dichlorobenzamide 
               
               
                   
                 2,8-Dichlorobenzonitrile 
               
               
                   
                 2,6-Dimethylaniline 
               
               
                   
                 2-[3-Chlorophenoxy]propionamide 
               
               
                   
                 2-Chlorophenol 
               
               
                   
                 2-Ethyl-1,3-hexanediol 
               
               
                   
                 2-ethyl-8-methylaniline 
               
               
                   
                 2-Hydroxyestradiol 
               
               
                   
                 2-Methyl-4,6-dinitrophenol 
               
               
                   
                 2-Methylphenol 
               
               
                   
                 2-Nitrophenol 
               
               
                   
                 2-Phenoxypropionic acid 
               
               
                   
                 3,4,5-Trimethacarb 
               
               
                   
                 3,4-Dichloroaniline 
               
               
                   
                 3,4-Dichloroaniline 
               
               
                   
                 3-Aminophenol 
               
               
                   
                 3-Chloro-4-fluoroaniline 
               
               
                   
                 3-Chloro-4-methoxyaniline 
               
               
                   
                 3-Chloroaniline 
               
               
                   
                 3-Hydroxycarbofuran 
               
               
                   
                 3-Indolylacetonitrile 
               
               
                   
                 3-Trifluormethylaniline 
               
               
                   
                 4,4′-Dichlorobenzophenone 
               
               
                   
                 4,4′-Oxydianiline 
               
               
                   
                 4,6-Dinitro-o-cresol (DNDC) 
               
               
                   
                 4-Aminodiphenyl 
               
               
                   
                 4-Bromoaniline 
               
               
                   
                 4-Chloro-2-methylaniline 
               
               
                   
                 4-Chloro-3-methylphenol 
               
               
                   
                 4-Chloroaniline 
               
               
                   
                 4-Chlorophenyl-isocyanate 
               
               
                   
                 4-Isopropylaniline 
               
               
                   
                 4-Methylphenol 
               
               
                   
                 4-Nitrophenol 
               
               
                   
                 4-Nonylphenol 
               
               
                   
                 5,7-Dihydroxy-4′-methoxyisoflavone 
               
               
                   
                 9,10-Anthraquinone 
               
               
                   
                 Acenaphthane 
               
               
                   
                 Acenaphthylene 
               
               
                   
                 Acephate 
               
               
                   
                 Acequinocyl 
               
               
                   
                 acetamiprid 
               
               
                   
                 Acetochlor 
               
               
                   
                 Acifluorfen methyl ester 
               
               
                   
                 Aclariffen 
               
               
                   
                 Accinathrin 
               
               
                   
                 Alachlor 
               
               
                   
                 Aldrin 
               
               
                   
                 Allidochlor 
               
               
                   
                 Amelyn 
               
               
                   
                 Amidithion 
               
               
                   
                 Aminocarb 
               
               
                   
                 Amitraz 
               
               
                   
                 Amitraz metabolite [Methanimidamide, N- 
               
               
                   
                 (2,4-dimethylphenyl)-N′-methyl-] 
               
               
                   
                 Ancymidol 
               
               
                   
                 Anilazine 
               
               
                   
                 Aniline 
               
               
                   
                 Anilofos 
               
               
                   
                 Anthracene 
               
               
                   
                 Aramite I 
               
               
                   
                 Aramite II (CAS # 140-57-8) 
               
               
                   
                 Atraton 
               
               
                   
                 Atrazine 
               
               
                   
                 Atrazine-desethyl 
               
               
                   
                 Azaconazole 
               
               
                   
                 Azamethiphos 
               
               
                   
                 Azibenzolar-S-methyl 
               
               
                   
                 Azinphos-ethyl 
               
               
                   
                 Azinphos-methyl 
               
               
                   
                 Aziprotryn metabolite [2-Amino- 
               
               
                   
                 4-isopropylamino-6-methylthio- 
               
               
                   
                 1,3,5-triazine] 
               
               
                   
                 Aziprotryne 
               
               
                   
                 Azobenzene 
               
               
                   
                 Azoxybenzene 
               
               
                   
                 Azoxystrobin 
               
               
                   
                 Barben 
               
               
                   
                 Bellubutamid 
               
               
                   
                 Benalaxyl 
               
               
                   
                 Benazolin-ethyl 
               
               
                   
                 Bendiocarb 
               
               
                   
                 Benfluralin 
               
               
                   
                 Benfuracarb 
               
               
                   
                 Benferesate 
               
               
                   
                 Benetanil 
               
               
                   
                 Benoxacor 
               
               
                   
                 Bentazone 
               
               
                   
                 Bentazone methyl derivative 
               
               
                   
                 Benthiocarb 
               
               
                   
                 Benzene, 1,3-bis(bromomethyl)- 
               
               
                   
                 Benzenesulfonamide 
               
               
                   
                 Benzidine 
               
               
                   
                 Benzo(a)anthracene 
               
               
                   
                 Benzo(a)pyrene 
               
               
                   
                 Benzo[b]fluoranthene 
               
               
                   
                 Benzo[g,h,i]parylene 
               
               
                   
                 Benzo[k]fluoranthene 
               
               
                   
                 Benzophenone 
               
               
                   
                 Benzoximate metabolite 
               
               
                   
                 Benzoylprop ethyl 
               
               
                   
                 Benzyl benzoate 
               
               
                   
                 b-Estradiol 
               
               
                   
                 BHC alpha isomer 
               
               
                   
                 BHC beta isomer 
               
               
                   
                 BHC delta isomer 
               
               
                   
                 BHC epsilon isomer 
               
               
                   
                 Bifenazate metabolite 
               
               
                   
                 (5-Phenyl-o-anisidine) 
               
               
                   
                 Bifenox 
               
               
                   
                 Bifenthrin 
               
               
                   
                 Binapacryl 
               
               
                   
                 Bioallethrin 
               
               
                   
                 Bioallethrin S-cyclopentenyl isomer 
               
               
                   
                 Bioresmethrin 
               
               
                   
                 Biphenyl 
               
               
                   
                 Bis(2,3,3,3-tetrachloropropyl) ether 
               
               
                   
                 Bis(2-butoxyethyl) phthalate 
               
               
                   
                 Bis(2-ethylhexyl)phthalate 
               
               
                   
                 Bisphenol A 
               
               
                   
                 Bitertanol I 
               
               
                   
                 Bitertanol II (CAS # 55179-31-2) 
               
               
                   
                 Boscalid (Niobifan) 
               
               
                   
                 Bromocil 
               
               
                   
                 Bromfenvinphos-(E) 
               
               
                   
                 Bromfenvinphos-(Z) 
               
               
                   
                 Bromobutide 
               
               
                   
                 Bromocyclan 
               
               
                   
                 Bromophos 
               
               
                   
                 Bromophos-ethyl 
               
               
                   
                 Bromopropylate 
               
               
                   
                 Bromoxynil 
               
               
                   
                 Bromoxynil octanoic acid ester 
               
               
                   
                 Bromoconazole I 
               
               
                   
                 Bromoconazole II (CAS # 116255-48-2) 
               
               
                   
                 Bufencarb 
               
               
                   
                 Bupiliniate 
               
               
                   
                 Buprofezin 
               
               
                   
                 Butachlor 
               
               
                   
                 Butafenacil 
               
               
                   
                 Butamilos 
               
               
                   
                 Butoxycarboxim 
               
               
                   
                 Butralin 
               
               
                   
                 Butyl benzyl phthalate 
               
               
                   
                 Butylate 
               
               
                   
                 Butylated hydroxyanisole 
               
               
                   
                 Cadusafos 
               
               
                   
                 Cafenstrole 
               
               
                   
                 Caffeine 
               
               
                   
                 Captafol 
               
               
                   
                 Captan 
               
               
                   
                 Carboryl 
               
               
                   
                 Carbetamide 
               
               
                   
                 Carbofuran 
               
               
                   
                 Carbofuran-3-keto 
               
               
                   
                 Carbofuran-7-phenol 
               
               
                   
                 Carbophenethion 
               
               
                   
                 Carbosulfen 
               
               
                   
                 Carboxin 
               
               
                   
                 Carfentrazone-ethyl 
               
               
                   
                 Carpropamid 
               
               
                   
                 Carvone 
               
               
                   
                 Cashmeran 
               
               
                   
                 Cekalix 
               
               
                   
                 Celestolide 
               
               
                   
                 Chinomethionet 
               
               
                   
                 Chloramben methyl ester 
               
               
                   
                 Chloronocryl 
               
               
                   
                 Chlorbenside 
               
               
                   
                 Chlorbenside sulfone 
               
               
                   
                 Chlorbicyclen 
               
               
                   
                 Chlorbromuron 
               
               
                   
                 Chlorbulam 
               
               
                   
                 Chlordecone 
               
               
                   
                 Chlordene, trans- 
               
               
                   
                 Chlordimeform 
               
               
                   
                 Chlorethoxyfos 
               
               
                   
                 Chlorfenapyr 
               
               
                   
                 Chlorfenethol 
               
               
                   
                 Chlorfenprop-methyl 
               
               
                   
                 Chlorfenson 
               
               
                   
                 Chlorfenvinphos 
               
               
                   
                 Chlorfenvinphos, cis- 
               
               
                   
                 Chlorfenvinphos. trans- 
               
               
                   
                 Chlorflurecol-methyl ester 
               
               
                   
                 Chlormefos 
               
               
                   
                 Chlomitrofen 
               
               
                   
                 Chlorobenzilate 
               
               
                   
                 Chloraneb 
               
               
                   
                 Chloropropylate 
               
               
                   
                 Chlorothalonil 
               
               
                   
                 Chlorotoluron 
               
               
                   
                 Chlorpropham 
               
               
                   
                 Chlorpyrifos 
               
               
                   
                 Chlorpyrifos Methyl 
               
               
                   
                 Chlorthal-dimethyl 
               
               
                   
                 Chlorthiamid 
               
               
                   
                 Chlorthion 
               
               
                   
                 Chlorthiophos 
               
               
                   
                 Chlorthiophos sulfone 
               
               
                   
                 Chlorthiophos sulfoxide 
               
               
                   
                 Chlozolinate 
               
               
                   
                 Chrysene 
               
               
                   
                 Cinerin I 
               
               
                   
                 Cinerin II 
               
               
                   
                 Cinidon-ethyl 
               
               
                   
                 cis-Chlodane 
               
               
                   
                 Clodinafop-propargyl 
               
               
                   
                 Clornazone 
               
               
                   
                 Cloquintocet-methyl 
               
               
                   
                 Coumaphos 
               
               
                   
                 Crinkline 
               
               
                   
                 Crotoxyphos 
               
               
                   
                 Crufomate 
               
               
                   
                 Cyanazine 
               
               
                   
                 Cyanofenphos 
               
               
                   
                 Cyanophos 
               
               
                   
                 Cyclafuramid 
               
               
                   
                 Cycloate 
               
               
                   
                 Cyclopentadecanone 
               
               
                   
                 Cycluron 
               
               
                   
                 Cyllufenamid 
               
               
                   
                 Cylluthrin I 
               
               
                   
                 Cyllurhrin II (CAS # 68359-37-5) 
               
               
                   
                 Cylluthrin III (CAS # 68359-37-5) 
               
               
                   
                 Cylluthrin IV (CAS # 68359-37-5) 
               
               
                   
                 Cyhalofop-butyl 
               
               
                   
                 Cyhalothrin I (lambda) 
               
               
                   
                 Cyhalothrin (Gamma) 
               
               
                   
                 Cymiazole 
               
               
                   
                 Cymoxanil 
               
               
                   
                 Cypermethrin I 
               
               
                   
                 Cypermethrin II (CAS # 52315-07-8) 
               
               
                   
                 Cypermethrin III (CAS # 52315-07-8) 
               
               
                   
                 Cypermethrin IV (CAS # 52315-07-8) 
               
               
                   
                 Cyphenothrin cis- 
               
               
                   
                 Cyphenothrin trans-(CAS # 39515-40-7) 
               
               
                   
                 Cyprazine 
               
               
                   
                 Cyproconazole 
               
               
                   
                 Cyprodinil 
               
               
                   
                 Cyprofuram 
               
               
                   
                 Cyromazine 
               
               
                   
                 d-(cis-trans)-Phenothrin-I 
               
               
                   
                 d-(cis-trans)-Phenothrin-II 
               
               
                   
                 (CAS # 260002-80-2) 
               
               
                   
                 Dazomet 
               
               
                   
                 DDMU [1-Chloro-2,2-bis(4′,chlorophenyl]) 
               
               
                   
                 Decachlorobiphenyl 
               
               
                   
                 Deltamethrin 
               
               
                   
                 Demaphion 
               
               
                   
                 Demeton-S 
               
               
                   
                 Demeton-S-methylsulfon 
               
               
                   
                 Desbromo-bromobutide 
               
               
                   
                 Desmediphan 
               
               
                   
                 Desmetryn 
               
               
                   
                 Dialifos 
               
               
                   
                 Di-allato I 
               
               
                   
                 Di-allate II (CAS # 2303-16-4) 
               
               
                   
                 Diamyl phthalate 
               
               
                   
                 Diazinon 
               
               
                   
                 Diazinon-oxon 
               
               
                   
                 Dibenz[a,b]anthracene 
               
               
                   
                 Dicamba 
               
               
                   
                 Dicamba methyl ester 
               
               
                   
                 Dicapthon 
               
               
                   
                 Dichlofenthion 
               
               
                   
                 Dichlofluanid 
               
               
                   
                 Dichlofluanid metabolite (DMSA) 
               
               
                   
                 Dichlone 
               
               
                   
                 Dichlormid 
               
               
                   
                 Dichlorophen 
               
               
                   
                 Dichlorprop 
               
               
                   
                 Dichlorprop methyl ester 
               
               
                   
                 Dichlorves 
               
               
                   
                 Diclobutrazol 
               
               
                   
                 Diclocymet I 
               
               
                   
                 Diclocymet II (CAS # 139920-32-4) 
               
               
                   
                 Diclofop methyl 
               
               
                   
                 Dicloran 
               
               
                   
                 Dicrotophos 
               
               
                   
                 Dicyclohexyl phthalate 
               
               
                   
                 Dicyclopentadieno 
               
               
                   
                 Dieldrin 
               
               
                   
                 Diethatyl ethyl 
               
               
                   
                 Diethofencarb 
               
               
                   
                 Diethyl dithiobis(thionoformate) (EXD) 
               
               
                   
                 Diethyl phthalate 
               
               
                   
                 Diethylene glycol 
               
               
                   
                 Diethylstilbestrol 
               
               
                   
                 Difenoconazol I 
               
               
                   
                 Difenoconazol II (CAS # 119446-68-3) 
               
               
                   
                 Difenoxuton 
               
               
                   
                 Diflufenican 
               
               
                   
                 Diisobutyl phthalate 
               
               
                   
                 Dimelox 
               
               
                   
                 Dimepiperate 
               
               
                   
                 Dimethachlor 
               
               
                   
                 Dimethametryn 
               
               
                   
                 Dimethenomid 
               
               
                   
                 Dimethipin 
               
               
                   
                 Dimethoate 
               
               
                   
                 Dimethomorph-(E) 
               
               
                   
                 Dimethomorph-(Z) (CAS # 110488-70-5) 
               
               
                   
                 Dimethylphthalate 
               
               
                   
                 Dimethylvinphos(z) 
               
               
                   
                 Dimetilan 
               
               
                   
                 Dimoxystrobin 
               
               
                   
                 Di-n-butylphthalate 
               
               
                   
                 Di-n-hexyl phthalate 
               
               
                   
                 Diniconazole 
               
               
                   
                 Dinitramine 
               
               
                   
                 Di-n-nonyl phthalate 
               
               
                   
                 Dinobuton 
               
               
                   
                 Dinocap I 
               
               
                   
                 Dinocap II (CAS # 39300-45-3) 
               
               
                   
                 Dinocap III (CAS # 39300-45-3) 
               
               
                   
                 Dinocap IV (CAS # 39300-45-3) 
               
               
                   
                 Di-n-octyl phthalate 
               
               
                   
                 Dinoseb 
               
               
                   
                 Dinoseb acetate 
               
               
                   
                 Dinoseb methyl ether 
               
               
                   
                 Dinoterb 
               
               
                   
                 Dinoterb acetate 
               
               
                   
                 Di-n-propyl phthalate 
               
               
                   
                 Diofenolan I 
               
               
                   
                 Diofenolan II (CAS # 63837-33-2) 
               
               
                   
                 Dioxabenzofos 
               
               
                   
                 Dioxacarb 
               
               
                   
                 Dioxathion 
               
               
                   
                 Diphacinone 
               
               
                   
                 Diphenamid 
               
               
                   
                 Diphenyl pththalate 
               
               
                   
                 Diphenylamine 
               
               
                   
                 Dipropetryn 
               
               
                   
                 Dipropyl isocinchomeronate 
               
               
                   
                 Disulfoton 
               
               
                   
                 Disulfoton sulfone 
               
               
                   
                 Ditalimfos 
               
               
                   
                 Dithiopyr 
               
               
                   
                 Diuron 
               
               
                   
                 Diuron Metabolite [3,4-Dichlorophenyl 
               
               
                   
                 isecyanate] 
               
               
                   
                 Dodemorph I 
               
               
                   
                 Dodemorph II (CAS # 1593-77-7) 
               
               
                   
                 Drazoxolon 
               
               
                   
                 Edifenphos 
               
               
                   
                 Empenthrin I 
               
               
                   
                 Empenthrin II (CAS # 54406-48-3) 
               
               
                   
                 Empenthrin III (CAS # 54408-48-3) 
               
               
                   
                 Empenthrin IV (CAS # 54406-48-3) 
               
               
                   
                 Empenthrin V (CAS # 54406-48-3) 
               
               
                   
                 Endosulfan (alpha isomer) 
               
               
                   
                 Endosulfan (beta isomer) 
               
               
                   
                 Endosulfan ether 
               
               
                   
                 Endosulfan lactone 
               
               
                   
                 Eadosulfan sulfate 
               
               
                   
                 Endrin 
               
               
                   
                 Endrin aldehyde 
               
               
                   
                 Endrin ketone 
               
               
                   
                 EPN 
               
               
                   
                 Epoxiconazole 
               
               
                   
                 EPTC 
               
               
                   
                 Erbon 
               
               
                   
                 Esfenvalarate 
               
               
                   
                 Esprocarb 
               
               
                   
                 Etaconazole 
               
               
                   
                 Ethalfluralin 
               
               
                   
                 Ethidimuron 
               
               
                   
                 Ethiofencarb 
               
               
                   
                 Ethiolate 
               
               
                   
                 Ethion 
               
               
                   
                 Ethofenprox 
               
               
                   
                 Ethofumesate 
               
               
                   
                 Ethofumesate, 2-Keto 
               
               
                   
                 Ethoprophos 
               
               
                   
                 Ethoxyfen-ethyl 
               
               
                   
                 Ethoxyquin 
               
               
                   
                 Ethylenethiourea 
               
               
                   
                 Etoxazole 
               
               
                   
                 Etridiazole 
               
               
                   
                 Etridiazole, deschloro-(5-ethoxy- 
               
               
                   
                 3-dichloromethyl-1,2,4-thiadiazole) 
               
               
                   
                 Etrimfos 
               
               
                   
                 Eugenol 
               
               
                   
                 Exaltolida (1,5-Pentadecanolide) 
               
               
                   
                 Famoxadon 
               
               
                   
                 Famphur 
               
               
                   
                 Fenamidone 
               
               
                   
                 Fenamiphos sulfoxide 
               
               
                   
                 Fenamiphos-sulfone 
               
               
                   
                 Fenarimol 
               
               
                   
                 Fenazaflor 
               
               
                   
                 Fenazaflor metabolite 
               
               
                   
                 Fenazaquin 
               
               
                   
                 Fenbuconazole 
               
               
                   
                 Fenchlorazole-ethyl 
               
               
                   
                 Fenchlorphos 
               
               
                   
                 Fenchlorphos-oxon 
               
               
                   
                 Fenclarim 
               
               
                   
                 Fenfuram 
               
               
                   
                 Fenhexamid 
               
               
                   
                 Fenitrothion 
               
               
                   
                 Fenitrothion-oxon 
               
               
                   
                 Fenobucarb 
               
               
                   
                 Fenoprop 
               
               
                   
                 Fenoprop methyl ester 
               
               
                   
                 Fenothiocarb 
               
               
                   
                 Fenoxanil 
               
               
                   
                 Fenoxaprop-ethyl 
               
               
                   
                 Fenoxycarb 
               
               
                   
                 Fenpiclonil 
               
               
                   
                 Fenpropathrin 
               
               
                   
                 Fenpropidin 
               
               
                   
                 Fenson 
               
               
                   
                 Fensulfothion 
               
               
                   
                 Fensulfothion-oxon 
               
               
                   
                 Fensulfothion-oxon-sulfone 
               
               
                   
                 fensulfothion-sulfone 
               
               
                   
                 Fenthion 
               
               
                   
                 Fenthion sulfoxide 
               
               
                   
                 Fenthion-sulfone 
               
               
                   
                 Fenuron 
               
               
                   
                 Fenvalerate I 
               
               
                   
                 Fenvalerate II (CAS # 51630-58-1) 
               
               
                   
                 Fepropimorph 
               
               
                   
                 Fipronil 
               
               
                   
                 Fipronil, desulfinyl- 
               
               
                   
                 Fipronil-sulfide 
               
               
                   
                 Fipronil-sulfona 
               
               
                   
                 Flamprop-isoprppyl 
               
               
                   
                 Flamprop-methyl 
               
               
                   
                 Fluacrypyrim 
               
               
                   
                 Fluazilop-p-butyl 
               
               
                   
                 Fluazinam 
               
               
                   
                 Fluazolate 
               
               
                   
                 Flubenzimine 
               
               
                   
                 Fluchloralin 
               
               
                   
                 Flucythrinate I 
               
               
                   
                 Flucythrinate II (CAS # 70124-77-5) 
               
               
                   
                 Fludioxonil 
               
               
                   
                 Flufenacot 
               
               
                   
                 Flumetralin 
               
               
                   
                 Flumiclorac-pentyl 
               
               
                   
                 Flumioxazin 
               
               
                   
                 Fluometuron 
               
               
                   
                 Fluoranthane 
               
               
                   
                 Fluorane 
               
               
                   
                 Fluorodifen 
               
               
                   
                 Fluoroglycofen-ethyl 
               
               
                   
                 Fluoroimide 
               
               
                   
                 Fluotrimazole 
               
               
                   
                 Fluoxastrobin cis- 
               
               
                   
                 Fluquinconazole 
               
               
                   
                 Flurenol-butyl ester 
               
               
                   
                 Flurenol-methylester 
               
               
                   
                 Fluridone 
               
               
                   
                 Flurochloridone I 
               
               
                   
                 Flurochloridone II (CAS # 61213-25-0) 
               
               
                   
                 Flurochloridone, deschloro0 
               
               
                   
                 Fluroxypyr-1-methylheptyl ester 
               
               
                   
                 Flurprimidol 
               
               
                   
                 Flurtamone 
               
               
                   
                 Flusilazole 
               
               
                   
                 Fluthiacat-methyl 
               
               
                   
                 Flutolanil 
               
               
                   
                 Flutrialol 
               
               
                   
                 Fluvalinate-tau-I 
               
               
                   
                 Fluvalinate-tau-II (CAS # 102851-06-9) 
               
               
                   
                 Folpet 
               
               
                   
                 Fonofos 
               
               
                   
                 Formothion 
               
               
                   
                 Fosthiazate I 
               
               
                   
                 Fosthiazate II (CAS # 98888-44-3) 
               
               
                   
                 Futheridazole 
               
               
                   
                 Furalaxyl 
               
               
                   
                 Furathiocarb 
               
               
                   
                 Furilazole 
               
               
                   
                 Furmacyclox 
               
               
                   
                 Halfenprox 
               
               
                   
                 Haloxyfop-methyl 
               
               
                   
                 Heptachlor 
               
               
                   
                 Heptachlor epoxide isomer A 
               
               
                   
                 Heptachlor exo-epoxide isomer B 
               
               
                   
                 Heptenophos 
               
               
                   
                 Hexabromobenzene 
               
               
                   
                 Hexachlorobenzene 
               
               
                   
                 Hexachlorophene 
               
               
                   
                 Hexaconazole 
               
               
                   
                 Hexazinone 
               
               
                   
                 Hexestrol 
               
               
                   
                 Hydroprene 
               
               
                   
                 Imazaill 
               
               
                   
                 Imazamethabenz-methyl I 
               
               
                   
                 Imazamethabenz-methyl II 
               
               
                   
                 (CAS # 81405-85-8) 
               
               
                   
                 Imibenconazole 
               
               
                   
                 Imibenconazole-desbenzyl 
               
               
                   
                 Indeno[1,2,3-cd]pyrene 
               
               
                   
                 Indoxacarb and Dioxacarb decomposition 
               
               
                   
                 product [Phenol, 2-(1,3-dioxolan-2-yl)-] 
               
               
                   
                 Ioxynil 
               
               
                   
                 Ioxynil octanoate 
               
               
                   
                 Ipconazole 
               
               
                   
                 Iprohenfos 
               
               
                   
                 Iprodiene 
               
               
                   
                 Iprovalicarb I 
               
               
                   
                 Iprovalicarb II (CAS # 140923-25-7) 
               
               
                   
                 Irgarol 
               
               
                   
                 Isazophos 
               
               
                   
                 Isobenzon 
               
               
                   
                 Isobornyl thiocyanoacetate 
               
               
                   
                 Isocarbamide 
               
               
                   
                 Isocarbophos 
               
               
                   
                 Isodrin 
               
               
                   
                 Isofenphos 
               
               
                   
                 Isofenphos-oxon 
               
               
                   
                 Isomethiozin 
               
               
                   
                 Isoprocarb 
               
               
                   
                 Isopropalin 
               
               
                   
                 Isoprothiolane 
               
               
                   
                 Isoproturon 
               
               
                   
                 Isoxaben 
               
               
                   
                 Isoxadifen-ethyl 
               
               
                   
                 Isoxaflutole 
               
               
                   
                 Isoxathion 
               
               
                   
                 Jasmolin I 
               
               
                   
                 Jasmolin II 
               
               
                   
                 Jodfenphos 
               
               
                   
                 Kinoprene 
               
               
                   
                 Kresoxim-methyl 
               
               
                   
                 Lactolen 
               
               
                   
                 Lenacil 
               
               
                   
                 Leptophos 
               
               
                   
                 Leptophos oxon 
               
               
                   
                 Lindane 
               
               
                   
                 Linuron 
               
               
                   
                 Malathion 
               
               
                   
                 Malathion-o-analog 
               
               
                   
                 MCPA methyl ester 
               
               
                   
                 MCPA-butoxyethyl ester 
               
               
                   
                 MCPB methyl ester 
               
               
                   
                 m-Cresol 
               
               
                   
                 Mecarbam 
               
               
                   
                 Mecoprop methyl ester 
               
               
                   
                 Mefenacet 
               
               
                   
                 Mefenpyr-diethyl 
               
               
                   
                 Melluidide 
               
               
                   
                 Menazon 
               
               
                   
                 Mepanipyrim 
               
               
                   
                 Mephosfalen 
               
               
                   
                 Mepronil 
               
               
                   
                 Metalaxyl 
               
               
                   
                 Metamitron 
               
               
                   
                 Metasystox thiol 
               
               
                   
                 Metazachlor 
               
               
                   
                 Metconazole I 
               
               
                   
                 Metconazole II (CAS # 125116-23-6) 
               
               
                   
                 Methabenzthiazuron [decomposition 
               
               
                   
                 product] 
               
               
                   
                 Methacrilos 
               
               
                   
                 Methamidophos 
               
               
                   
                 Methfuroxam 
               
               
                   
                 Methidathion 
               
               
                   
                 Methiocarb 
               
               
                   
                 Methiocarb sulfone 
               
               
                   
                 Methiocarb sulfoxide 
               
               
                   
                 Methomyl 
               
               
                   
                 Methoprene I 
               
               
                   
                 Methoprene II (CAS # 40596-69-8) 
               
               
                   
                 Methoprotryne 
               
               
                   
                 Methoxychlor 
               
               
                   
                 Methoxychlor olelin 
               
               
                   
                 Methyl (2-naphthoxy)acetate 
               
               
                   
                 Methyl paraoxon 
               
               
                   
                 Methyl parathion 
               
               
                   
                 Methyl-1-naphthalene acetate 
               
               
                   
                 Methyldymron 
               
               
                   
                 Metobromuron 
               
               
                   
                 Metolachlor 
               
               
                   
                 Metolcarb 
               
               
                   
                 Metominostrobin (E) 
               
               
                   
                 Metominostrobin (Z) 
               
               
                   
                 (CAS # 133408-50-1) 
               
               
                   
                 Metrafenone 
               
               
                   
                 Metribuzin 
               
               
                   
                 Mevinphos 
               
               
                   
                 Mirex 
               
               
                   
                 Molinate 
               
               
                   
                 Monalide 
               
               
                   
                 Monocrotophos 
               
               
                   
                 Monolinuron 
               
               
                   
                 Musk amberalta 
               
               
                   
                 Musk Ketone 
               
               
                   
                 Musk Moskene 
               
               
                   
                 Musk Tibetene (Moschustibeten) 
               
               
                   
                 Musk xylene 
               
               
                   
                 Myclobutanil 
               
               
                   
                 N,N-Diethyl-m-toluamide 
               
               
                   
                 N-1-Naphthylacetamide 
               
               
                   
                 Nalad 
               
               
                   
                 Naphthalene 
               
               
                   
                 Naphthalic anhydride 
               
               
                   
                 Naproanilide 
               
               
                   
                 Napropamide 
               
               
                   
                 Nicotine 
               
               
                   
                 Nitralin 
               
               
                   
                 Nitrapyrin 
               
               
                   
                 Nitrofen 
               
               
                   
                 Nitrothal-isopropyl 
               
               
                   
                 N-Methyl-N-1-naphthyl acetamide 
               
               
                   
                 Nonachlor, cis- 
               
               
                   
                 Nonachlor, trans- 
               
               
                   
                 Norflurazon 
               
               
                   
                 Norflurazon, desraethyl- 
               
               
                   
                 Nuarimol 
               
               
                   
                 o.p′-DDD 
               
               
                   
                 o.p′-DDE 
               
               
                   
                 o.p′-DDT 
               
               
                   
                 Octachlorostyrene 
               
               
                   
                 o-Dianisidine 
               
               
                   
                 o-Dichlorobenzene 
               
               
                   
                 Ofurace 
               
               
                   
                 Omethoate 
               
               
                   
                 o-Phenylphenol 
               
               
                   
                 Orbencarb 
               
               
                   
                 ortho-Aminoazotoluene 
               
               
                   
                 Oryzalin 
               
               
                   
                 Oxabetrinil 
               
               
                   
                 Oxadiazon 
               
               
                   
                 Oxadixyl 
               
               
                   
                 Oxamyl 
               
               
                   
                 Oxycarboxin 
               
               
                   
                 Oxychlordane 
               
               
                   
                 Oxydemeton-methyl 
               
               
                   
                 Oxyfluorfen 
               
               
                   
                 p.p′-DDD 
               
               
                   
                 p.p′-DDE 
               
               
                   
                 p.p′-DDM [bis(4-chlorophenyl)methane] 
               
               
                   
                 p.p′-DDT 
               
               
                   
                 p.p′-Dibromobenzophenone 
               
               
                   
                 p.p′-Dicofol 
               
               
                   
                 Paclobutrazol 
               
               
                   
                 Paraoxon 
               
               
                   
                 Parathion 
               
               
                   
                 PBB 52 Tetrabrombiphenyl 
               
               
                   
                 PBB 101 
               
               
                   
                 PBB 15 
               
               
                   
                 PBB 169 Hexabrombiphenyl 
               
               
                   
                 PCB 101 
               
               
                   
                 PCB 105 
               
               
                   
                 PCB 110 
               
               
                   
                 PCB 118 
               
               
                   
                 PCB 126 
               
               
                   
                 PCB 127 
               
               
                   
                 PCB 131 
               
               
                   
                 PCB 136 
               
               
                   
                 PCB 138 
               
               
                   
                 PCB 153 
               
               
                   
                 PCB 169 
               
               
                   
                 PCB 170 
               
               
                   
                 PCB 180 
               
               
                   
                 PCB 30 
               
               
                   
                 PCB 31 
               
               
                   
                 PCB 49 
               
               
                   
                 PCB 77 
               
               
                   
                 PCB 81 
               
               
                   
                 p-Dichlorobenzene 
               
               
                   
                 Pebulate 
               
               
                   
                 Penconazole 
               
               
                   
                 Pendimethalin 
               
               
                   
                 Pentachloroaniline 
               
               
                   
                 Pentachloroanisole 
               
               
                   
                 Pentachlorobenzene 
               
               
                   
                 Pentachloronitrobenzene 
               
               
                   
                 Pentachlorophenol 
               
               
                   
                 Pentanochlor 
               
               
                   
                 Permethrin I 
               
               
                   
                 Permethrin II (CAS # 52645-53-1) 
               
               
                   
                 Perthane 
               
               
                   
                 Phantolide 
               
               
                   
                 Phenamiphos 
               
               
                   
                 Phenanthrene 
               
               
                   
                 Phenanthrene-d10 
               
               
                   
                 Phenkapton 
               
               
                   
                 Phenol 
               
               
                   
                 Phenothiazine 
               
               
                   
                 Phenothrin I 
               
               
                   
                 Phenothrin II 
               
               
                   
                 Phenoxyacetic acid 
               
               
                   
                 Phenthoate 
               
               
                   
                 Phorate 
               
               
                   
                 Phorate sulfone 
               
               
                   
                 Phorate sulfoxide 
               
               
                   
                 Phorata-oxon 
               
               
                   
                 Phosalone 
               
               
                   
                 Phosfolan 
               
               
                   
                 Phosmet 
               
               
                   
                 Phosphamidon I 
               
               
                   
                 Phosphamidon II (CAS # 13171-21-6) 
               
               
                   
                 Phthalide 
               
               
                   
                 Phthalimide 
               
               
                   
                 Picloram methyl ester 
               
               
                   
                 Picolinefen 
               
               
                   
                 Picoxystrobin 
               
               
                   
                 Pindone 
               
               
                   
                 Piperalin 
               
               
                   
                 Piperonyl butoxide 
               
               
                   
                 Piperophos 
               
               
                   
                 Pirimicarb 
               
               
                   
                 Pirimiphos-ethyl 
               
               
                   
                 Pirimiphos-methyl 
               
               
                   
                 Plifenat 
               
               
                   
                 p-Nitrotoluene 
               
               
                   
                 Potasan 
               
               
                   
                 Prallethrin, cis- 
               
               
                   
                 Prallethrin, trans-(CAS # 23031-36-9) 
               
               
                   
                 Pretilachlor 
               
               
                   
                 Probenazole 
               
               
                   
                 Prochloraz 
               
               
                   
                 Procymidone 
               
               
                   
                 Prodiamine 
               
               
                   
                 Profenofos 
               
               
                   
                 Profenofos metabolite (4-Bromo- 
               
               
                   
                 2-chlorophenol) 
               
               
                   
                 Profluralin 
               
               
                   
                 Prohydrojasmon I 
               
               
                   
                 Prohydrojasmon II (CAS # 158474-72-7) 
               
               
                   
                 Promecarb 
               
               
                   
                 Promecarb artifact [5-isopropyl- 
               
               
                   
                 3-methylphenol] 
               
               
                   
                 Prometon 
               
               
                   
                 Prometryn 
               
               
                   
                 Propachlor 
               
               
                   
                 Propamocarb 
               
               
                   
                 Propanil 
               
               
                   
                 Propaphos 
               
               
                   
                 Propargite 
               
               
                   
                 Propargite metabolite (Cyclohexanol, 
               
               
                   
                 2-(4-tert-butylphenoxy)] 
               
               
                   
                 Propazine 
               
               
                   
                 Propetamphos 
               
               
                   
                 Prophem 
               
               
                   
                 Propiconazole-I 
               
               
                   
                 Propiconazole-II (CAS # 80207-90-1) 
               
               
                   
                 Propisochlor 
               
               
                   
                 Propoxur 
               
               
                   
                 Propyzamide 
               
               
                   
                 Prosulfocarb 
               
               
                   
                 Prothioconazofe-dosthio 
               
               
                   
                 Prothiofos 
               
               
                   
                 Prothoate 
               
               
                   
                 Pyracarbolid 
               
               
                   
                 Pyraclofos 
               
               
                   
                 Pyraflufen-ethyl 
               
               
                   
                 Pyrazon 
               
               
                   
                 Pyrazophos 
               
               
                   
                 Pyrazoxyfen 
               
               
                   
                 Pyrene 
               
               
                   
                 Pyrethrin I 
               
               
                   
                 Pyrethrin II 
               
               
                   
                 Pyributicarb 
               
               
                   
                 Pyridaben 
               
               
                   
                 Pyridaphenthion 
               
               
                   
                 Pyridate 
               
               
                   
                 Pyridinitril 
               
               
                   
                 Pyrifenox I 
               
               
                   
                 Pyrifenox II (CAS # 88283-41-4) 
               
               
                   
                 Pyriltalid 
               
               
                   
                 Pyrimethanil 
               
               
                   
                 Pyrimidifen 
               
               
                   
                 Pyriminobac-methyl (E) 
               
               
                   
                 Pyriminobac-methyl (Z) 
               
               
                   
                 (CAS # 136191-64-5) 
               
               
                   
                 Pyriproxyfen 
               
               
                   
                 Pyroquilon 
               
               
                   
                 Quinalphos 
               
               
                   
                 Quinoclamine 
               
               
                   
                 Quinoxyfen 
               
               
                   
                 Quintozene metabolite (pentachlorophenyl 
               
               
                   
                 methyl sulfide) 
               
               
                   
                 Quinzalofop-ethyl 
               
               
                   
                 Rabenzazole 
               
               
                   
                 Resmethrin 
               
               
                   
                 Resmethrine I 
               
               
                   
                 Resmethrine II (CAS # 10453-86-8) 
               
               
                   
                 Rotenone 
               
               
                   
                 S,S,S-Tributylphosphorotrithioate 
               
               
                   
                 Schradan 
               
               
                   
                 Sebuthylazine 
               
               
                   
                 Sebuthylazine-desethyl 
               
               
                   
                 Secbumeton 
               
               
                   
                 Silafluofen 
               
               
                   
                 Silthiopham 
               
               
                   
                 Simazine 
               
               
                   
                 Simeconazole 
               
               
                   
                 Simetryn 
               
               
                   
                 Spirodiclofen 
               
               
                   
                 Spiromesifen 
               
               
                   
                 Spiroxamine I 
               
               
                   
                 Spiroxamine II (CAS # 118134-30-8) 
               
               
                   
                 Spioxamine metabolite (4-tert-butylcyclo- 
               
               
                   
                 hexanone) 
               
               
                   
                 Sudan I 
               
               
                   
                 Sudan II 
               
               
                   
                 Sudan Red 
               
               
                   
                 Sulfallate 
               
               
                   
                 Sulfanilamide 
               
               
                   
                 Sulfentrazone 
               
               
                   
                 Sulfotep 
               
               
                   
                 Sulfur (SB) 
               
               
                   
                 Sulprofos 
               
               
                   
                 Swep 
               
               
                   
                 Tamoxifen 
               
               
                   
                 TCMTB 
               
               
                   
                 Tebuconazole 
               
               
                   
                 Tebufenpyrad 
               
               
                   
                 Tebupirimifos 
               
               
                   
                 Tebutam 
               
               
                   
                 Tabuthiuron 
               
               
                   
                 Tecnazene 
               
               
                   
                 Tefluthrin, cis- 
               
               
                   
                 Temephos 
               
               
                   
                 Terbacil 
               
               
                   
                 Terbucarb 
               
               
                   
                 Terbufos 
               
               
                   
                 Terbufos-oxon-sulfone 
               
               
                   
                 Terbufos-sulfone 
               
               
                   
                 Terbumeton 
               
               
                   
                 Terbuthylazine 
               
               
                   
                 Terbuthylazine-desethyl 
               
               
                   
                 Terbutryne 
               
               
                   
                 Tetrachlorvinphos 
               
               
                   
                 Tetraconazole 
               
               
                   
                 Tetradifon 
               
               
                   
                 Tetraethylpyrophosphate (TEPP) 
               
               
                   
                 Tetrahydrophthalimide, cis-1,2,3,6- 
               
               
                   
                 Tetramethrin I 
               
               
                   
                 Tetramethrin II (CAS # 7696-12-0) 
               
               
                   
                 Tetrapropyl thiodiphosphate 
               
               
                   
                 Tetrasul 
               
               
                   
                 Thenylchlor 
               
               
                   
                 Theobromine 
               
               
                   
                 Thiabendazole 
               
               
                   
                 Thiazopyr 
               
               
                   
                 Thifluzamide 
               
               
                   
                 Thiofanox 
               
               
                   
                 Thiomeron 
               
               
                   
                 Thionazin 
               
               
                   
                 Thymol 
               
               
                   
                 Tiocarbazil I 
               
               
                   
                 Tiocarbazil II (CAS # 36756-79-3) 
               
               
                   
                 Tolclofos-methyl 
               
               
                   
                 Tolfenpyrad 
               
               
                   
                 Tolylfluanid 
               
               
                   
                 Tolylfluanid metabolite (DMST) 
               
               
                   
                 Tolyltriazole [1H-Benzotriazole, 4-methyl-] 
               
               
                   
                 Tolyltriazole [1H-Benzotriazole, 5-methyl-] 
               
               
                   
                 Tonalide 
               
               
                   
                 Toxaphene Parlar 26 
               
               
                   
                 Toxaphene Parlar 50 
               
               
                   
                 Toxaphene Parlar 62 
               
               
                   
                 trans-Chlordane 
               
               
                   
                 Transfluthrin 
               
               
                   
                 Trassalide 
               
               
                   
                 Triadimefon 
               
               
                   
                 Triadimenol 
               
               
                   
                 Tri-allate 
               
               
                   
                 Triamiphos 
               
               
                   
                 Trispenthenol 
               
               
                   
                 Triazamate 
               
               
                   
                 Triazophos 
               
               
                   
                 Tributyl phosphate 
               
               
                   
                 Tributyl phosphorotrithioite 
               
               
                   
                 Trichlamide 
               
               
                   
                 Trichlorfon 
               
               
                   
                 Trichloronate 
               
               
                   
                 Triclopyr methyl ester 
               
               
                   
                 Triclosan 
               
               
                   
                 Triclosan-methyl 
               
               
                   
                 Tricresylphosphate, meta- 
               
               
                   
                 Tricresylphosphate, ortho- 
               
               
                   
                 Tricresylphosphate, para 
               
               
                   
                 Tricyclazole 
               
               
                   
                 Tridemorph, 4-tridecyl- 
               
               
                   
                 Tridiphane 
               
               
                   
                 Trietazine 
               
               
                   
                 Triethylphosphate 
               
               
                   
                 Trilenmorph 
               
               
                   
                 Trilloxystrobin 
               
               
                   
                 Trillumizole 
               
               
                   
                 Trilluralin 
               
               
                   
                 Triphenyl phosphate 
               
               
                   
                 Tris(2-butoxyethyl) phosphate 
               
               
                   
                 Tris(2-chloroethyl) phosphate 
               
               
                   
                 Tris(2-ethylhexyl) posphate 
               
               
                   
                 Triticonazole 
               
               
                   
                 Tryclopyrbutoxyethyl 
               
               
                   
                 Tycor (SMY 1500) 
               
               
                   
                 Uniconizole-P 
               
               
                   
                 Vamidithion 
               
               
                   
                 Vernolate 
               
               
                   
                 Vinclozolin 
               
               
                   
                 XMC (3,4-Dimethylphenyl 
               
               
                   
                 N-methylcarbama 
               
               
                   
                 XMC (3,5-Dimethylphenyl 
               
               
                   
                 N-methylcarbama 
               
               
                   
                 Zoxamide 
               
               
                   
                 Zoxamide decomposition product 
               
               
                   
                   
               
             
          
         
       
     
         [0019]    The following examples are intended to illustrate, but not limit, this disclosure. 
       EXAMPLES 
     Materials and Methods 
     1. Preparation of Samples for GC/MS Analysis 
       [0020]    Approximately 1.0 g of sample was placed in a 50 mL tube and the exact weight was recorded on a log sheet. For each sample, two quality control samples were prepared using 1 g muffled sand; these were labeled “MB” (Method Blank) and “LCS” (Laboratory Control Sample). 9.0 mL of deionized water was added to each of the tubes. Quality control standards were added as follows: 
         [0021]    (a) 50 uL of 20 ppm GC surrogate (tetrachlorometaxylene (TCMX), Decachlorobiphenyl (DCB), Tributyl phosphate and Triphenyl phosphate) in acetonitrile was added to all samples including the MB and LCS; 
         [0022]    (b) 100 uL of 20 ppm OC pest spiking solution (Organochlorine Pesticide Mix AB #1 (Restek Corp., Bellefonte, Pa.) containing aldrin, α-BHC, β-BHC, δ-BHC, γ-BHC (lindane), cis-chlordane, trans-chlordane, 4,4′-DDD, 4,4′-DDE, 4,4′-DDT dieldrin, endosulfan I, endosulfan II, endosulfan sulfate, endrin, endrin aldehyde, endrin ketone, heptachlor, heptachlor epoxide (isomer B) and methoxychlor) in acetonitrile was added to the LCS; and 
         [0023]    (c) 100 uL of 20 ppm Internal Standard solution in acetonitrile was added to all samples. 
         [0024]    The samples were shaken vigorously and allowed to equilibrate for 2 hours at room temperature. Extraction of the samples was then performed by adding 10 mL of acetonitrile and shaking for one minute, adding the contents of an extraction salt packet (Q-Sep™ Q110 QuEChERS extraction salt packet containing 4 g MgSO 4 , 1 g NaCl, 1 g trisodium citrate dehydrate, 0.5 g disodium hydrogen citrate sesquihydrate; Restek Corp.), shaking again for one minute and then centrifuging for 5 minutes. 
         [0025]    For samples needing clean-up (as determined for example, by previous difficulties with analysis, difficult matrix or darkly colored residues), the solvent extract was placed in a cleanup tube (Q-Sep™ dSPE 15 mL sample cleanup centrifuge tubes containing 900 mg MgSO4, 150 mg PSA and 45 mg GCB), shaken vigorously and centrifuged for 5 minutes, before being placed in an evaporation tube. The samples were then evaporated to near dry (less than 1 mL solvent) using a TurboVap™ evaporator, and 5 mL methylene chloride was added using a solvent pump. This process was repeated until the acetonitrile portion had been exchanged out for methylene chloride and the volume had reached less than 1 mL. Methylene chloride was then added to raise the volume in the sample back to 1 mL, and the sample was transferred into a labeled vial and cap using a crimper and aluminum cap. 
         [0026]    Blanks were run with every set of samples to ensure that laboratory media or equipment was not leading to false positives in any contaminants. These were made following the same process as for the extracts for analysis. 
       2. GC/MS Analysis 
       [0027]    Samples prepared as described above were analyzed for the presence of contaminants using an Agilent Technologies 5975C gas chromatograph/mass spectrometer (GC/MS) in combination with enhanced data analysis as described below. 
         [0028]    Prior to analysis of samples, the GC/MS was checked for any instrument problems that could seriously affect the quality of analysis using routine procedures well known to those of skill in the art. Each analysis sequence carried out on the GC/MS was bracketed by calibration verification samples, “initial calibration verification” samples or “continuing calibration verification” samples. These samples were made using concentrations equal to 0.1 ppm. The concentration of the standards in these samples was within 50% of the expected values. The method blank (MB) and laboratory control (LCS) samples were placed at the beginning of the sequence. 
         [0029]    The instrument was calibrated for target analytes, or contaminants, prior to reporting any target analyte concentration. Calibration was performed by running a set of samples containing a blank and five known concentrations, with the highest level corresponding to the highest expected results, through the screening method. The calibration set was quantitated using data analysis and deconvolution employing Deconvolution Reporting Software (DRS; Agilent Technologies, Inc). After each of the five calibration samples were quantitated, the new values were entered into the database. The curve shapes were checked for linearity. R̂2 values were 0.98 or greater. 
         [0030]    Analysis was performed on completed data sets using DRS and Enhanced Data Analysis software (Agilent Technologies, Inc.). After files were deconvoluted, they were reviewed using QEdit™ software. Peaks identified by AMDIS (Automated Mass Spectral Deconvolution and Identification System; available from the National Institute of Standards and Technology (NIST)) and Chemstation™ software were reviewed for quality. More specifically, peaks were reviewed based on comparison between library spectra, AMDIS extracted spectra and Chemstation™ spectra; qualifier peak match; and retention time. Generally peaks were considered true “hits” if they had a MF (molecular formula) match value above 75 and the three qualifier ion values were within 25% of expected. In general, a genuine match has a spectrum very similar to the library/database spectrum, shows a strong, sharp peak shape in both the Chemstation™ and AMDIS peak viewer windows, has a very high MF value, and will likely be identified by both the Chemstation™ and AMDIS softwares. 
         [0031]    There are times when Chemstation™ integrated a different peak than AMDIS. Because AMDIS has been rigorously developed to remove erroneous background suppression and use several statistical models to effectively “mine” the data, AMDIS was given higher priority than Chemstation™ when interpreting data. When a peak was accepted as genuine, it was either left alone or manually integrated. Since the GC/MS employed for these studies only uses a single quadrupole, it often has trouble resolving overlapping peaks. In such instances, the range of the correct peak was manually integrated. Once all of the peaks had been reviewed, the data was saved and a report generated. 
         [0032]    Reports were reviewed after analysis to ensure that data met specifications, specifically sequence data information, internal standard recovery, surrogate recovery percentages, calibrated analyte concentrations and semiquant compounds (i.e. those compounds found using AMDIS and DRS that have not been calibrated for) hits were checked. Due to limitations with the software, generated reports often listed detections for compounds that had qualifier ion mismatches. These peaks do not show up in the default view and are very difficult to track down and delete, but are always erroneous. These were simply deleted from the report. 
         [0033]    Internal standard recovery should have a minimum abundance of 1,000,000 counts, and should generally be within 50% of the calibrated abundance. Matrix effects can cause this number to vary somewhat, so data was generally accepted even if the recovery was outside of the 50% margin. 
         [0034]    Surrogate recoveries should also be within 50% of calibrated values, but variation may also be due to matrix effects, thus this was not generally used to reject data unless there were clear signs that the ability to generate quality data was compromised. 
         [0035]    Semiquant compounds that were found regularly in blanks were discarded from the screening list. These compounds, which included phthalates among a few others, were ignored when reporting data. Semiquant hits were not calibrated; unless they were calibrated, they can only be reported on a presence/absence basis. 
         [0036]    In order for calibrated compounds to be reported, they must fall within the range of the initial calibration curve. If they were outside of this range, the sample was diluted to be within this range and rerun. Calibrated compound concentrations were multiplied by the dilution factor and divided by the sample weight before being reported. 
       3. Quality Control 
     (a) Evaluation of Retention Time Windows 
       [0037]    The internal standard retention time was calibrated at 13.726 in accordance with the original AMDIS calibration. During the initial phase of calibration, the retention time was locked, which allowed AMDIS to accept or reject peaks based upon retention time. If the internal standard fell outside of the window and was not integrated by AMDIS, corrective action was taken and the sample was reanalyzed. 
       (b) Sample Cleanup 
       [0038]    Sample cleanup was performed on samples that were excessively thick or colored, or that, based on previous history, were expected to cause problems during analysis. 
       (c) Handling and Storage 
       [0039]    All standards were stored at −4° C. or below and were allowed to reach room temperature before use. 
       (d) Limits of Detection 
       [0040]    The limits of detection (LOD) determine the lowest concentration at which an analyte can be detected in an extracted sample. Since these measurements are not available for all compounds, the average of the LODs for calibrated compounds determines the estimated detection limit for uncalibrated compounds. The LOD is determined by the lowest concentration compound extracted with a signal to noise ratio of 2.5-5. These tests were performed periodically to determine any changes in instrument sensitivity. 
       (e) Calibration 
       [0041]    Initial calibration established a calibration curve used to determine the concentration of calibrated compounds and recoveries of surrogates. The average internal standard response was also used to determine the baseline response used for the internal standard calibration verification. Calibrations were run at seven levels: 0.01, 0.025, 0.05, 0.10, 0.5, 1.0, and 5.0 ppm. Using the data from this calibration, each compound should have a linear or quadratic curve with an R sq. value of 0.95 or greater. The lowest calibration level determines the limit of quantification (LOQ). If a compound failed calibration (i.e. did not have an R sq. value of 0.95 or greater) it was noted and corrected before any detections of this compound were quantitated. 
         [0042]    Internal standard calibration verification (ISCV) was used to verify instrument performance and internal standard response. This was prepared with 1.0 ppm internal standard in methylene chloride. The internal standard abundance should be 70%-170% of the response established with the initial calibration and within the AMDIS retention time window. If the response fell outside of this window, the aberration was investigated and corrected before analysis took place. The ISCV was also used to determine column condition. The abundance of ion 207 (siloxane bleed) at 40 minutes should be under 25,000. If the background did not improve in subsequent analyses, the column was replaced and the instrument recalibrated before sample analysis. 
         [0043]    Initial calibration verification (ICV) and continuing calibration verification (CCV) samples were used to verify that the analysis performance was within the parameters of the initial calibration. The CCV was run at the end of a set of samples to bracket either an initial calibration or ICV sample. The ICV was run in place of a set of calibration samples unless there were measures outside of limits requiring a new calibration set. 
         [0044]    Recovery control limits for surrogates and other calibrated compounds were set at 70-170%. These laboratory control spikes calculated percent recovery. If these fall outside of limits, it could be due to matrix suppression, problems with analysis or extraction. These issues were addressed as necessary. 
       4. Testing of Sodium Ascorbate 
       [0045]    Sodium ascorbate intended for use in nutraceuticals for human consumption was tested for the presence of multiple pesticide residues as described above. No pesticide residues in amounts above the USP &lt;561&gt; Articles of Botanical Origin reporting limits were found. 
         [0046]    While the present invention has been described with reference to the specific embodiments thereof, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the true spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation, material, composition of matter, method, method step or steps, for use in practicing the present invention. All such modifications are intended to be within the scope of the claims appended hereto. 
         [0047]    All of the publications, patent applications and patents cited in this application are herein incorporated by reference in their entirety to the same extent as if each individual publication, patent application or patent was specifically and individually indicated to be incorporated by reference in its entirety.