bluuebunny/crossref_metadata_2025_split huggingface dataset:
Rapid Reverse Phase Liquid Chromatographic Determination of Aflatoxin M1 in Milk
Authors: Yousef Ahmed E , Marth Elmer H 
Published: February 2020

Abstract
A rapid, economical, and reliable liquid chromatographic (LC) method is described for determination of aflatoxin M, in milk. The method includes an improved AOAC extraction procedure, cleanup of the extract on a silica cartridge, and LC quantitation. Alternatively, a rapid column cleanup procedure can be used. Milk artificially spiked with aflatoxin M1 at 0.05, 0.1, and 0.5 ppb was analyzed using both new approaches as well as an AOAC method coupled with LC for quantitation of the toxin. Recovery of aflatoxin M1 by the first approach of the new method ranged between 93.4 and 99.1%, and for the alternative procedure between 92.4 and 96.8%. The AOAC method gave lower recovery (85.6-90.7%) of toxin, but the results from this method had a somewhat smaller standard deviation for replicate analyses than did results of the new method.
Rapid Quantitative Method for Simultaneous Determination of Benzoic Acid, Sorbic Acid, and Four Parabens in Meat and Nonmeat Products by Liquid Chromatography
Authors: Ali Sher M 
Published: February 2020

Abstract
A liquid chromatographic (LC) method for the simultaneous determinations of benzoic acid, sorbic acid, and methyl, ethyl, propyl, and butyl parabens (methyl, ethyl, propyl, and butyl-p-hydroxybenzoates) in meat and nonmeat products was developed. Benzoic acid, sorbic acid, and parabens were extracted from meat and nonmeat products with 70% ethanol. After filtration, extracts were analyzed by reverse phase liquid chromatography. Homogeneously ground samples of fresh sausage and hamburger were fortified with benzoic acid, sorbic acid, and each paraben at 5 different concentrations. Average recovery (after discarding outliers) for each preservative at all 5 levels was greater than 95% with a coefficient of variation less than 5%.
Methods of Analysis for Infant Formula: Food and Drug Administration and Infant Formula Council Collaborative Study
Authors: Tanner James T , Barnett Stephen A 
Published: February 2020

Abstract
Because the U.S. Infant Formula Act of 1980 requires manufacturers to produce formula containing a specific minimum amount of nutrients, it became necessary to establish analytical methods for the nutrients listed in the Act. The Food and Drug Administration, the Infant Formula Council, its member companies, contract laboratories, and other government laboratories undertook a collaborative study of available methods; the specific nutrients studied to date include vitamins A, B6, C, riboflavin, and niacin, and the elements calcium, magnesium, iron, zinc, copper, manganese, sodium, and potassium. The coefficients of variation in most cases have been as good as those that could be predicted from other collaborative studies. The methods studied for these nutrients have been adopted official first action except the method for vitamin A.
Quantitation of Indomethacin, Naproxen, and Ibuprofen in Pharmaceutical Dosage Forms by First and Second Derivative Ultraviolet Spectrometry
Authors: Mahrous Mohamed S , Abdel-Khalek Magdi M , Abdel-Hamid Mohamed E 
Published: February 2020

Abstract
First and second derivative ultraviolet spectrometric methods are described for the estimation of indomethacin, naproxen, and ibuprofen in pharmaceutical dosage forms. The proposed methods permit the rapid, precise, and accurate determination of indomethacin capsules BP, naproxen capsules, and ibuprofen tablets BP. Matrix interference is successfully corrected. The results obtained by first and second derivative techniques are in accord with those obtained by the official assay method.
Liquid Chromatographic Determination of Organic Nitrogenous Bases in Dosage Forms: A Progress Report
Authors: Walker Samuel T 
Published: February 2020

Abstract
A liquid chromatographic (LC) method has been developed as a general procedure for the assay of the salts of organic nitrogenous bases in a variety of dosage forms. The method uses a nitrile-bonded reverse phase column, a methanol-0.003M ammonium acetate (90 + 10) mobile phase, and photometric detection at 254 nm. The sample is dissolved in the mobile phase and an aliquot is injected through a 20 μL injection loop. Average recovery values for duplicate assays were chlorpheniramine maleate injection 97.8%, chlorpheniramine maleate tablets 99.1%, cyclizine hydrochloride tablets 100.0%, doxylamine succinate tablets 103.3%, mesoridazine besylate tablets 100.4%, pentazocine hydrochloride tablets 103.0%, promethazine hydrochloride injection 98.4%, protriptyline hydrochloride tablets 101.2%, pyrilamine maleate tablets 97.8%, pyrimethamine tablets 100.0%, tripelennamine citrate elixir 100.0%, and tripelennamine hydrochloride tablets 97.2%. Results by this method were in good agreement with those obtained by the USP XX method. This study, which is being continued, will be expanded to include additional drugs.
Gas Chromatographic Determination of Metolachlor in Pesticide Formulations: Collaborative Study
Authors: Gale Thomas G , Hofberg Arthur H 
Published: February 2020

Abstract
A gas chromatographic (GC) procedure for the determination of metolachlor in emulsifiable concentrate formulations containing about 76% active ingredient was collaboratively studied using the matched pair scheme. Metolachlor was extracted from the formulation with acetone containing dipentyl phthalate as the internal standard, chromatographed on OV-101, and detected by flame ionization. Determinations on the 4 samples by 21 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 0.5%. Reproducibility was better than 1% for the formulation. The method has been adopted official first action.
Liquid Chromatographic Determination of Morantel Tartrate in Cattle Feed
Authors: Goras John T , Gauthier Allen R 
Published: February 2020

Abstract
A liquid chromatographic (LC) method is proposed for measuring 0.485-0.970% morantel tartrate in cattle feeds. The drug is leached from feed, diluted, separated from interfering substances on a silica column, and measured in the effluent stream by 313 nm spectrophotometric detection. Two potential degradation products, i.e., m-isomer of morantel tartrate and N-(3-methylaminopropyl)-/ra/w-3-(3-methyl- 2-thienyl)acrylamide, and a related anthelmintic, i.e., pyrantel tartrate, do not interfere. Average recovery of drug from liquid spiked samples and laboratory blends was 98-100% with a maximum coefficient of variation (CV) of 2.3%. Results for pelleted and crumbled commercial scale feeds ranged from 94 to 102% of label claim, with a maximum CV of 1.5%.
Calibration of Skim Milk-Test Bottles
Authors: Hankin Lester , Wickrosk Alphonse , Hornig Lois 
Published: February 2020

Abstract
The method described uses a 250 μL syringe to calibrate skim milktest bottles. Mercury is injected into the bore of the test bottle, and the amount is recorded. The bore of the bottle can contain 100 μL mercury, and those bottles shown to contain between 98 and 102 μL are acceptable for certification.
Negative Ion Chemical Ionization Mass Spectrometric Method for Confirmation of Identity of Aflatoxin B,: Collaborative Study
Authors: Park Douglas L , Diprossimo Vincent , Abdel-Malek Emil , Trucksess Mary W , Nesheim Stanley , Brumley William C , Sphon James A , Barry Thomas L , Petzinger Glenn 
Published: February 2020

Abstract
An interlaboratory study of a negative ion chemical ionization mass spectrometric (MS) confirmation procedure for aflatoxin B1 was conducted in laboratories in the United States, England, and West Germany. Twelve partially purified, dry film extracts from naturally and artificially contaminated roasted peanuts, cottonseed, and ginger root containing varying quantities of aflatoxin B1 were distributed to the participating laboratories. The extracts required additional cleanup before MS analysis, using either an acidic alumina column and preparative thin layer chromatography (TLC) or a 2-dimensional TLC procedure. Recovery of purified aflatoxin B1 was influenced by the degree of recovery of sample from acid alumina and/or the TLC plate and incomplete elution of aflatoxin Bt from silica gel. Factors affecting MS confirmation included the purity and recovery of aflatoxin and MS instrument sensitivity. Aflatoxin Bi identity was confirmed in 19.5, 90.9, and 100% of samples containing &lt;5,5-10, and &gt;10 ng aflatoxin B1/g product, respectively, by solid probe introduction using full mass scans. The MS method has been adopted official first action.
Interlaboratory Variability of Methods Used for Detection of Economic Adulteration in Apple Juice
Authors: Zyren John , Elkins Edgar R 
Published: February 2020

Abstract
Thirteen laboratories participated in a study to determine the interlaboratory variability of 4 methods used to detect economic adulteration in apple juice. The methods included the determination of individual sugars, 5-(hydroxymethyl)-2-furaldehyde, chlorogenic acid, organic acids, and L-malic acid. The coefficients of variation found depended on the method and level of analyte, but were often 5% or less. At this point, the most important test for detecting economic adulteration is the total malic/L-malic acid ratio. Any ratio of 0.9 or less would indicate a nonauthentic sample. The 0.9 ratio represents an addition of 20% synthetic malic acid in the unknown juice sample. A 0.75 ratio would indicate 50% adulteration, while a 0.5 ratio would indicate a totally synthetic juice. Fumaric acid, a minor contaminant in synthetically produced malic acid, shows great promise as an indicator of economic adulteration. The results support the view that the methods are now ready for AOAC collaborative study.
Effect of Cooking on Levels of Ethylene Dibromide Residues in Rice
Authors: Clower Marion , Mccarthy James P , Rains Diane M 
Published: February 2020

Abstract
Two studies were conducted to determine the effect that cooking has on the level of residues of ethylene dibromide (EDB) in rice. In the first study, 4 samples of long and medium grain polished white rice containing 113, 295, 956, and 1568 ppb EDB were cooked according to typical label directions. Three batches of cooked rice were prepared from each sample of polished rice and frozen until analysis; each batch was analyzed in duplicate. EDB levels in all cooked rice samples were &lt;10 ppb. In the second study, conducted jointly by the Food and Drug Administration (FDA) and the Environmental Protection Agency (EPA), a sample of medium grain polished white rice containing about 1600 ppb EDB was cooked by each laboratory. Overall average EDB levels in rice analyzed immediately after cooking were 16 and 37 ppb for FDA and EPA, respectively. The corresponding frozen samples contained 8 and 39 ppb EDB. The 2 laboratories exchanged these frozen samples and reanalyzed them to check variability in the analytical procedure. FDA found 49 ppb EDB in the sample cooked by EPA and EPA found 8 ppb EDB in the sample cooked by FDA, thus indicating that analytical methodology was not a major source of variability. The range of EDB levels was therefore attributed to minor differences in the way the rice was cooked or handled immediately after cooking.
Capillary Gas Chromatographic-Mass Spectrometric Determination of Fluoroacetate Residues in Animal Tissues
Authors: Casper Howard H , Mcmahon Terence L , Paulson Gaylord D 
Published: February 2020

Abstract
A method for the quantitative determination of fluoroacetate (FAC) residues in animal tissues is described. The procedure involves tungstic acid extraction, partitioning into ethyl acetate, evaporation of ethyl acetate, derivatization with pentafluorobenzyl bromide (PFB), and analysis of the resulting derivative (PFB-FAC) by capillary gas chromatography- mass spectrometry (CGC-MS) with specific ion monitoring (SIM). The tungstic acid system extracted 96.8 ± 4.2% of the endogenous 14C-1080 residues in rat tissues. Recovery of FAC during the extraction, purification, and derivatization procedures is established by use of a 14-FAC spike. 1,2-Dibromobenzene is used as an internal standard for the CGC-MS analysis. PFB-FAC is identified on the basis of comparative retention times and the relative intensities of m/z 257.9 and 181.0. PFB-FAC is quantitated by comparing the response at m/z 257.9 to a PFB-FAC standard curve. Routine sensitivity of the method allows determination of 10 ppb fluoroacetate in tissue.
Electron Capture Detection-Gas Chromatographic Determination of Diaminotoluenes in Polyurethane Foam as Heptafluorobutyryl Derivativ
Authors: Hirayama Teruhisa , Ono Mayumi , Uchiyama Kazumi , Nohara Motoshi , Fukui Shozo 
Published: February 2020

Abstract
A simple gas chromatographic (GC) method has been developed to determine 2,4- and 2,6-diaminotoluenes in polyurethane foam. Diaminotoluenes were reacted with heptafluorobutyric anhydride in toluene, and the products, bis-heptafluorobutyrates, were determined by GC, using a 3% silicone OV-330 column. The 2,4- and 2,6-diaminotoluenes can be detected as heptafluorobutyryl derivatives by using an electron capture detector at levels of 5 and 2 pg, respectively. Finally, 2.7-3.0 (μg/g of 2,4- and 1.3-1.9 (μg/g of 2,6-diaminotoluene were detected in 3 commercial polyurethane foams.
Gas Chromatographic Determination of CCRL583 Perfluorinated Alcohol Fumigant Residues
Authors: Zehner James M , Simonaitis Richard A 
Published: February 2020

Abstract
A gas chromatographic method is described for the determination of CCRL583 (l,l,l,3,3,4,4,4-octafluoro-2-(trifluoromethyl)-2-butanol). r The sample is extracted with acetonitrile and cleaned up by liquidliquid extraction, first with a basic aqueous solution and finally with an acid aqueous solution. The final organic layer is injected into a gas chromatograph equipped with a column packed with terephthalic acidterminated Carbowax 20M. Recovery of CCRL583 from fortified wheat and peanuts was 91-108%.
Correlation of Analytical Methods and Biological Activity of Various Sulfur-Coated Urea Fertilizer Products
Authors: Mcvey George R , Horn Douglas P , Scheiderer Edwin L , Davidson Allan D 
Published: February 2020

Abstract
Sulfur-coated urea (SCU) has become widely accepted as a fertilizer source for turf and certain other agricultural crops. A means of assessing SCU release characteristics is the Tennessee Valley Authority (TVA) 7-day dissolution rate (DR). The AOAC-accepted method is the waterinsoluble nitrogen (WIN) determination. Data are presented which show that neither of the 2 methods can be considered optimum at predicting biological activity. When testing SCU produced by only one of the 3 coating techniques now used by industry, acceptable correlations were obtained between analytical method and biological activity. However, when testing SCU produced by different coating technologies, the correlation of biological activity with analytical methods was significantly reduced. Based on the results presented here and in the literature, it is recommended that the TVA 7-day DR method not be collaboratively studied. The AOAC WIN method should be maintained until a more suitable method can be developed that has a higher correlation with biological activity.
Liquid Chromatographic Determination of Major Alkaloids in Gum Opium
Authors: Srivastava Vinod K , Maheshwari Mohan L 
Published: February 2020

Abstract
An isocratic reverse phase liquid chromatographic (LC) system has been developed for qualitative and quantitative assay of morphine, codeine, thebaine, papaverine, and narcotine in gum opium. Five extractions with 2.5% aqueous acetic acid quantitatively extracted the major alkaloids. A mixture of 1% aqueous sodium acetate (pH 6.78), acetonitrile, and 1,4-dioxane (75 + 20 + 5) is used as LC mobile phase | for better resolution of alkaloid peaks, especially those of morphine and codeine. The method is suitable for routine analysis of gum opium I samples.
Liquid Chromatographic Determination of Sulfasalazine in Tablets and Bulk Powder
Authors: Egli Keith L 
Published: February 2020

Abstract
A liquid chromatographic method has been developed that determines I the amount of sulfasalazine in tablets and bulk powder in the presence of residual synthesis by-products and excipients. The method was tested j on crude product containing large amounts of impurities. A C-18 1 reverse phase column with water-acetonitrile-acetic acid mobile phase ! was found to effectively separate the drug on the column. Six different commercial samples of 500 mg tablets were assayed. The results varied from 92.6 to 101.8% of the declared amount. Spectrohotometric determinations, which do not discriminate between the drug and impurities, gave 95.4—101.8% of declared. One commercial sample of bulk powder j was assayed.
Amino Acid Analysis of Feedstuff Hydrolysates by Cation Exchange High Performance
Liquid Chromatography
Authors: Elkin Robert G , Griffith Joseph E 
Published: February 2020

Abstract
Corn, peanut meal, and soybean meal samples were either untreated or oxidized with performic acid before hydrolysis; the amino acids were determined by cation exchange high performance liquid chromatography (LC) and conventional cation exchange LC using an amino acid analyzer (AAA). Reproducibility of each procedure was assessed by repeated injections of the same calibration standard solution over a period of several days. LC data were more precise with regard to coefficients of variation for amino acid retention times, but were more variable with regard to peak areas. Although some significant differences between methods were noted, feedstuff amino acid values obtained by LC and AAA compared very well. The only consistent differences observed within each feedstuff were that Phe and Tyr values were significantly lower when analyzed by LC compared with AAA. Results of this study suggest that modular LC instrumentation can be used to accurately and reproducibly analyze amino acids in feedstuff hydrolysates. Advantages of using ninhydrin derivatization for feedstuff analysis, as opposed to using o-phthalaldehyde or dansyl chloride, are discussed
Liquid Chromatographic Determination of Colchicine in Pharmaceuticals: Collaborative Study
Authors: Thompson Richard D 
Published: February 2020

Abstract
A liquid chromatographic (LC) method for the determination of colchicine in pharmaceutical dosage forms and the bulk drug was evaluated in an interlaboratory study which included 13 participating laboratories. The method involves extraction (or dissolution) of the active ingredient with methanol-water (1 + 1), followed by filtration of the extract and reverse phase LC using an octy lsilane bonded phase column and UV detection at 254 nm. The mobile phase consists of a methanolphosphate buffer mixture (pH = 5.5). Three commercial tablet formulations (0.5-0.6 mg colchicine/tablet), 1 synthetic injectable preparation (0.510 mg colchicine/mL), and 1 bulk drug sample were assayed in duplicate by the proposed method. The reproducibility and repeatability standard deviations based on nonpooled results for each sample ranged from 0.0062 mg/mL to 0.0147 mg/tablet and from 0.0037 mg/ mL to 0.0127 mg/tablet, respectively; the corresponding coefficients of variation ranged from 1.21 to 2.54% and from 0.73 to 2.19%, respectively. The mean recovery from the synthetic injectable formulation was 100.0%. The method has been adopted official first action
Performance Characteristics of Methods of Analysis Used for Regulatory Purposes. I. Drug Dosage Forms. E. Miscellaneous Methods
Authors: Horwitz William , Albert Richard 
Published: February 2020

Abstract
Precision parameters of miscellaneous methods for the analysis of drug dosage forms approved by AOAC since 1972, and not previously reviewed in this series, were recalculated on a consistent statistical basis by using the computer program FDACHEMIST. Seventeen published collaborative studies were reviewed; the studies encompassed 19 analytes in 80 different materials (dosage forms), 102 collaborative assays, approximately 10 laboratories per study, and principally direct spectrophotometric, polarographic, and spectroscopic methods, for a total of 1451 determinations. The average repeatability relative standard deviation (within-laboratories, RSD„) for the instrumental methods was 1.5%; the reproducibility relative standard deviation (among-laboratories, including within-, RSDX) was 2.6%; the ratio RSD„/RSDX of the averages was 0.57, with an average outlier rate of 2.7% of the reported determinations. The line of best fit of RSDX for the instrumental methods plotted against the negative logarithm of the concentration increases slightly with decreasing concentration, extending from an RSDX of approximately 2.0% at 100% concentration to an RSDX of 3.4% at 0.001% (10 ppm) concentration; this represents an RSDX change of approximately 0.3% (absolute) for each 10-fold decrease in concentration, independent of analyte, matrix, and method. A method for determining precipitated allergenic protein by the micro-Kjeldahl technique appeared to be outside this general relation, showing an RSDX of about 13% at a concentration of 0.015% (150 ppm) nitrogen.
Automated Methods for Determination of Fat and Moisture in Meat and Poultry Products: Collaborative Study
Authors: Bostian Marianne L , Fish, David L , Webb Neil B , Arey Judy J 
Published: February 2020

Abstract
A collaborative study was conducted to compare automated methods for rapid determination of fat and moisture in meat and poultry products with the official AOAC solvent extraction and forced-air oven methods, respectively. Fourteen products were tested, with fat and moisture contents ranging from 2 to 43% and 44 to 74%, respectively. Eight of the collaborating laboratories analyzed the products by using a moisture/fat analyzer; 4 laboratories used the AOAC methods. Standard deviations for within-laboratory repeatability, between-laboratory reproducibility, and bias for each product indicated that the rapid methods were acceptable. The moisture/fat analyzer methods have been adopted official first action for fat and moisture analyses in meat and poultry products.
Rapid Detection of Clostridium perfringens: Comparison of Lactose Sulfite Broth with Tryptose-Sulfite-Cycloserine Agar
Authors: Neut Christel , Pathak Jayant , Romond Charles , Beerens Henri 
Published: February 2020

Abstract
The lactose sulfite (LS) medium recommended for the detection and identification of Clostridium perfringens in foods was compared with a reference method using tryptose-sulfite-cycloserine (TSC) agar for the enumeration of this organism in a variety of foods and food ingredients. C. perfringens was detected and enumerated in 17 of the 54 samples examined with LS broth, but its presence could be confirmed in only 9 of the samples with TSC agar. In only 2 instances, C. perfringens was detected on TSC agar but not in LS broth. A positive response (FeS + and gas +) in LS broth incubated at 46°C always corresponded to the presence of C. perfringens; whereas the black colonies formed on TSC agar incubated at 37°C were frequently found to be Clostridium species other than C. perfringens. Thus, because of its highly selective nature, LS broth was superior to TSC agar for enumerating and confirming the small numbers of C. perfringens that were present in a majority of the samples. This was especially true when other Clostridia were also present. Besides its greater selectivity and sensitivity, LS broth had the additional advantages of requiring less work and giving confirmed results within 24-48 h compared with 3 days for the TSC agar method.