bluuebunny/crossref_metadata_2025_split huggingface dataset:
Automated Technique for Sampling Milk from Farm Bulk Tanks: Collaborative Study
Authors: Packard Vernal S , Ginn Roy E , Metzger Dick T 
Published: February 2020

Abstract
An automated, in-line, mechanical technique for sampling milk from farm bulk tanks was evaluated in a collaborative study. The automated sampling device, which is mounted on the milk intake line, contains an electronically controlled peristaltic pump. The device takes a representative sample of the entire volume pumped through the system. Samples taken can be analyzed for both composition and microbiological quality. The study was performed in 3 phases. In the first 2 phases, samples taken by manual and automated methods were compared in analyses for somatic cell count, antibiotics, fat, protein, lactose, and solids-not-fat. The third phase, using a modified procedure, was designed to compare sampling methods in analyses for total bacteria count (standard plate count), psychrotrophic bacteria count, and coliform count. Evaluation of the data by a nested ANOVA indicated no difference between results for samples taken by the automated and manual methods (P = 0.05) in Phases 1 and 2, irrespective of whether the bulk milk was agitated before sampling. By introducing a sanitizing step between farms in Phase 3, the automated method also provided samples comparable with those taken manually for microbial analyses. The automated method has been adopted first action by AOAC International.
Analysis of Testosterone Esters by Tandem Mass Spectrometry
Authors: Cairns Thomas , Siegmund Emil G , Rader Bobby 
Published: February 2020

Abstract
The electron ionization (El) and chemical ionization (CI) mass spectra of 12 representative testosterone esters were examined to explore the various analytical options available for identification and confirmation of the esters. Using El, a number of fragment ions indicated the identification of the testosterone moiety, but structural confirmation of the individual esters often required the observance of the molecular ion at very low relative abundance ratios. The acceptable analytical method involved CI/tandem mass spectrometry based on the production of the 2 generic product ions derived from the protonated molecule ion.
Liquid Chromatographic Assay of Bentazon Formulations
Authors: Schmitt Thomas M 
Published: February 2020

Abstract
A reversed-phase liquid chromatographic method is presented for determining the active agent in technical bentazon and in aqueous formulations of the sodium salt of bentazon. The procedure is an isocratic, external standard method specifying an octadecylsilyl column, an acetate-buffered mobile phase of methanol-water, and UV detection. The 340 nm detection wavelength eliminates interference from formulation impurities.
Niacin I: Dissolution Profiles of Sustained-Release Niacin Products by Automated and Manual Procedures
Authors: Kirchhoefer Ross D , Hipp Sharon 
Published: February 2020

Abstract
Automated and manual procedures were developed to obtain dissolution profiles of sustained-release niacin formulations. The procedures are based on the United States Pharmacopeia XXII apparatus 1 (basket) at 100 rpm with 900 mL 0.1 N HCI as the dissolution medium. Filtered aliquots are read at 260 nm. No interference was found from excipients. The procedures are straightforward and will discriminate between sustained-release and regular niacin formulations.
Analysis of Milk-Based Infant Formula. Phase V. Vitamins A and E, Folic Acid, and Pantothenic Acid: Food and Drug Administration-Infant Formula Council: Collaborative Study
Authors: Tanner James T , Barnett Stephen A , Mountford Mardi K ,   Collaborators:, Angyal G , Beare-Rogers J L , Boyer K W , Bueno M P , DeAngelis N , DeVries J W , Dube D , Ellefson W , Fisher P , Landen W O , Navis J , Pearson D , Reynolds S L , Richards P , Soliman A-G , Thompson J N , Thomson W 
Published: February 2020

Abstract
In 1982, the U.S. Food and Drug Administration, the Infant Formula Council and its member companies, contract laboratories, and other government laboratories began a study of analytical methods for the nutrients listed in the Infant Formula Act of 1980 (P.L. 96-359). Four phases of the study have been completed and are discussed in earlier reports. The present report provides data on Phase V, in which 13 laboratories collaboratively studied individual methods for folic acid, pantothenic acid, and vitamin E, in addition to 2 methods for vitamin A. Vitamins A and E are determined by liquid chromatography. Folic acid and pantothenic acid are determined by microbiological methods using acidimetric and/or turbidimetric assays as the determinative step. In most cases, relative standard deviations for repeatability, RSDr, and reproducibility, RSDR, are as good as those that would be predicted from other collaborative studies. RSDr and RSDR values obtained for the 5 methods are 9.35 and 25.44% for folic acid, 4.59 and 10.23% for pantothenic acid, 8.46 and 11.69% for vitamin E, 3.62 and 9.72% for vitamin A (retinol isomers), and 4.9 and 10.5% for vitamin A (retinol). The 5 methods have been adopted first action by AOAC International.
Sample Preparation Bias in Carbon Stable Isotope Ratio Analysis of Fruit Juices and Sweeteners
Authors: Krueger Dana A 
Published: February 2020

Abstract
Two sample preparation methods are commonly used for carbon stable isotope ratio analysis (SIRA). One involves combustion of the sample with oxygen at 850° C the other involves combustion of the sample with CuO in an evacuated glass tube at 550°C. I observed in our laboratory that these 2 methods yield different results for sugarbased products such as fruit juices, sweeteners, and vanillin. The CuO method yields results approximately 1© more positive than the oxygen combustion method. This bias is also observed in other laboratories, as shown in an analysis of the results of the AOAC collaborative studies of carbon SIRA of maple syrup, orange juice, honey, and honey protein. The oxygen combustion method is the AOAC method for honey, apple juice, and orange juice; both methods are incorporated into the AOAC method for maple syrup. I recommend that data generated by the CuO combustion method be appropriately corrected to yield results concordant with the official oxygen combustion method.
Stability-Indicating Proton Nuclear Magnetic Resonance Spectroscopic Assay Method for Furosemide in Tablets and Injections
Authors: Hanna George M , Lau-Cam Cesar A 
Published: February 2020

Abstract
A simple, specific, and accurate proton nuclear magnetic resonance (1H-NMR) spectroscopic method has been developed for the identification and assay of furosemide and its degradation product, 4-chloro-5-sulfamoylanthranilic acid (CSA), in tablets and injections. Dissolution of the sample in D20-NaOD resulted in a solution yielding the required separation among the resonance signals of furosemide, CSA, and ferf-butyl alcohol, the internal standard. The mean ± SD recovery values of furosemide and CSA from 10 synthetic formulations were 99.6 ± 0.8 and 98.9 ± 1.7%, respectively. Commercial tablets (6 lots) and injections (5 lots) of furosemide were assayed by the proposed method and found to contain 53.1-99.8% furosemide and 0.3-45.2% CSA.
Carboxylic Acid Composition of Authentic Varietal and Commercial Grape Juices
Authors: Fuleki Tibor , Pelayo Estela , Palabay Rodrigo B 
Published: February 2020

Abstract
Quantities were determined of tartaric, malic, citric, lactic, succinic, and shikimic acid present in juices produced by cold and hot pressing from 56 grape cultivars grown in Ontario for the 1988 and 1989 seasons. The individual acids were separated by liquid chromatography (LC) and detected at 210 or 250 nm. Lactic and succinic acids were determined enzymatically. The ranges of acid concentrations found were as follows: tartaric, 4.19-13.51 g/L; malic, 1.68-15.36 g/L; citric, 0.305-1.158 g/L; lactic, 0.015-0.388 g/L; succinic, 0.002-0.075 g/L; and shikimic, 0-0.102 g/L. Tartaric and malic acids were the major acids in every cultivar. The tartaric:malic acid ratio ranged from 0.52 to 4.36, but it was &gt;1.0 in most cases. Genotype had significant effect only on the shikimic acid content. Hot pressing of red cultivars yielded juice with significantly higher pH and tartaric, citric, lactic, and total acid contents than cold pressing. Vintage had no significant effect on acid composition. The total acid content determined by LC was always considerably higher than the titratable acidity, but good correlation existed between the 2 measurements. Most commercial grape juice had similar composition to that of authentic juices. However, tartaric acid content was lower in the majority of commercial juices because of losses during the detartration process. Also, indications of acidulation existed in some of the commercial juices.
Hydroxyamidines as New Extracting Reagents for Spectrophotometric Determination of Cadmium with 4-(2-Pyridylazo)naphthol in Industrial Effluents, Coal, and Fly Ash
Authors: Chakravarty Sumon , Deb Manas Kanti , Mishra Rajendra Kumar 
Published: February 2020

Abstract
A simple, sensitive, and selective extractive spectrophotometric method for the determination of cadmium in trace quantities with N1-hydroxy-N1,N2- diphenylbenzamidine (HDPBA) and 4-(2-pyridylazo) naphthol (PAN) is described. The method is based on the extraction of cadmium with HDPBA into chloroform at pH 9.0 ± 0.2 and simultaneous spectrophotometric determination wiith PAN. The binary Cd(ll)-HDPBA complex extracted into chloroform has a molar absorptivity of 1.96 x 104L/ mol/cm at λmax 400 nm. The sensitivity of the yellow Cd(ll)-HDPBA complex was increased remarkably by the addition of PAN to the binary complex. With 6 different hydroxyamidines tested, the red-orange complex in chloroform exhibited maximum absorbance at 530-550 nm, with molar absorptivity values of 3.2-5.6 x 104L/mol/cm. The method adheres to Beer’s law up to 1.5 μg cadmium/mL organic phase. The detection limit of the method is 0.02 μg Cd/mL. Investigations of the effect of foreign ions revealed that the present method is free from matrix interference of most of the common ions (e.g., Fe(lll), Ni(ll), Cu(ll), Mn(ll), V(V), Co(ll), Al(lll), Cu(ll), Mg(ll), and Mo(VI)). The relative standard deviation for 10 repetitive analyses of the metal was 1.4%. The validity of the method was tested successfully with various environmental samples.
Liquid Chromatographic Determination of RH-5992, an Ecdysone Agonist, in Some Forestry Matrixes
Authors: Sundaram Kanth Maran Somu , Jiusheng Zhu , Nott Reginald 
Published: February 2020

Abstract
A liquid chromatographic method is described for the analysis of RH-5992 (N'-t-butyl-N'-[3,5-dimethylbenzoyl]- N-[4-ethylbenzoyl] hydrazine) from various terrestrial and aquatic forestry matrixes and stream water. The processed soils, Hitter, oak foliage, sediment, aquatic plants, and fish were extracted with a mixture of acetone and water; balsam fir needles were extracted with acidified methanol solution; stream water was extracted with dichloromethane. Aliquots of crude extracts were solvent partitioned, concentrated, and cleaned up by using Florisil or Prepsep-NH2 columns. After fractional elution of the columns with hexane-ethyl acetate as the eluent, the eluates were analyzed on a liquid chromatograph equipped with a diode-array UV detector set at 236 nm, using an RP-8,10 μm column with a mobile phase of acetonitrile- dioxane-water. Fir needles required methanol in addition to the 3 solvents in the mobile
Influence of Water on the Near Infrared Spectra of Model Compounds
Authors: Reeves III James B 
Published: February 2020

Abstract
The application of near infrared spectroscopy (NIRS) to high-moisture samples (i.e., silages) has shown that accuracy does not match that of dried materials. Examination of spectra does not indicate absorbance levels to be the problem. The objective of this effort was to determine the effect of water on the spectra of model compounds. Near infrared spectra were taken using a Digi-Lab FTS-65 Fourier transform spectrometer. Liquids were examined by transmission and solids by reflectance. Examination of organic acids, alcohols, ketones, amines, and amides showed that the presence of water causes shifts in spectral wavelengths not related to OH or NH groups. The most significant shifts were for alcohols and ketones (up to 10+ nm at 90% H2O) and least for acids. These peak shifts increased with increasing amounts of water and varied within individual spectra and among the compounds tested. As solids, sugars and amino acids had many sharp peaks in their spectra. As solutions, however, the sharp spectral features disappeared, resulting in large broad peaks. The spectra of polymers such as starch, cellulose, and casein did not appear to be significantly altered by the presence of water (0-50%, w/w), although they often appear to alter the water spectra. Variations in water content, physical state, and concentrations of components, when combined with these results, may help
Determination of Metals in Foodstuffs by Atomic Absorption Spectrophotometry after Dry Ashing: NMKL Interlaboratory Study of Lead, Cadmium, Zinc, Copper, Iron, Chromium, and Nickel
Authors: Jorhem Lars ,   Collaborators:, Afthan G , Cumont G , Dypdahl H P , Gadd K , Havre G N , Julshamn K , Kaverud K , Lind B , Loimaranta J , Merseburg M , Olsson A , Piepponen S , Sundstrom B , Uppstad B J , Waaler T , Winnerstam L 
Published: February 2020

Abstract
An interlaboratory study of a method for determination of lead, cadmium, zinc, copper, iron, chromium, and nickel in foodstuffs by atomic absorption spectrophotometry (AAS) after dry ashing at 450°C was conducted in 16 laboratories. The study was preceded by a practice round of familiarization samples and another round in which solutions were distributed and the metals were determined directly by AAS. The study included 5 different foods (liver paste, apple sauce, minced fish, wheat bran, and milk powder) and 2 composite diets. A single analysis was carried out on each sample. Suitable sample combinations were used as split level combinations for determination of the repeatability standard deviation. The relative reproducibility standard deviation for each of the elements ranged as follows: lead, 74-18% at 0.025-0.28 mg/kg; cadmium, 80-11% (0.002-0.51 mg/kg); zinc, 12-7% (44- 72 mg/kg); copper, 47-10% (0.48-41 mg/kg); iron, 35-9% (2-228 mg/kg); chromium, 48-21 % (0.008- 0.22 mg/kg); nickel, 64-39% (0.025-0.39 mg/kg).
Determination of Formaldehyde in Fresh and Retail Milk by Liquid Column Chromatography
Authors: Kaminski Jerzy , Atwal Avtar S , Mahadevan Subramaniam 
Published: February 2020

Abstract
A quantitative method is described for the determination of formaldehyde (CH2O) in milk by liquid chromatography. Aldehyde derivatization-extraction was carried out in situ with 2,4-dinitrophenylhydrazine in 2-phase reaction medium. Average recovery of added CH2O (0.1 μg/mL) was 89.9 ± 3.9% with an estimated detection limit of 0.009 mg/kg. The technique was used for the determination of CH2O in commercial 2% milk and in fresh milk of cows fed on a typical North American dairy diet. The average concentrations of CH2O in fresh and commercial milk were 0.027 and 0.164 mg/kg, respectively. Several methods for CH2O determination in milk are compared.
Methyl Bromide Determination in Selected Foods by Headspace Technique
Authors: Daft James L 
Published: February 2020

Abstract
A headspace method used earlier for determining methyl bromide (MB) in assorted nuts and peanut butters has been successfully applied to other foods that could potentially contain traces of this toxic fumigant. The foods tested include 63 off-theshelf spices and seasonings, 83 table-ready items (grain-based, dried, or highly seasoned), 30 dried fruits and trail mixes, and 38 oil-based items (oilseeds, cooking oils, or spicy oil-based dressings). Sample headspace gas is produced by blending ≤50 g sample in 250±50 mL aqueous solution in a sealed 1000 mL blender cup. After equilibration at 25C, the headspace is sampled with a gas-tight syringe and injected into a dual column-dual detector gas chromatograph. One determination is made with a 20% OV-101 packed column and a 63Ni electron capture detector (ECD), the other with a GS-Q wide-bore capillary column and a Hall electrolytic conductivity detector (HECD). Of the approximately 200 samples tested, none contained detectable MB residue at a quantitation limit &lt;100 ng/g sample. All fortified samples yielded MB recovery. Samples were fortified at levels ranging from 78 to 3250 ng MB/g. Recoveries ranged from a mean high of 56% for spices and seasonings to a mean low of 30% for oil-based foods. The overall recovery and CV, including the results from assorted nuts and peanut butters, were 46 and 33%, respectively.
Gas Chromatographic/Nitrogen-Phosphorus Detection Method for Determination of Ethylene Thiourea in Finished Drinking Waters: Collaborative Study
Authors: Longbottom James E , Edgell Kenneth W , Erb Elizabeth J , Lopez-Avila Viorica ,   Collaborators:, Brooks M , Byrne C , Clark D , Docus S , Kary K , Parker G , Perkins K , Pierri A , Quick F E , Simmons K , Torma L , Zimmerman D 
Published: February 2020

Abstract
A joint U.S. Environmental Protection Agency (USEPA)-AOAC interlaboratory method validation study was conducted on USEPA National Pesticide Survey (NPS) Method 6, "Determination of Ethylene Thiourea (ETU) in Finished Drinking Water by Gas Chromatography with a Nitrogen-Phosphorus Detector." The purpose of the study was to determine and compare the mean recoveries and precision for determination of ETU in reagent water and finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with ETU at 6 concentrations levels, prepared as 3 Youden pairs. In the method, the test water is extracted by passing the sample through an absorbent matrix type tube. ETU is recovered from the tube with methylene chloride, the extract is solvent-exchanged to ethyl acetate, and an aliquot of each extract is analyzed by gas chromatography using a nitrogen-phosphorus detector. Twelve laboratories participated in the study. Data were analyzed using a USEPA computer program, which measured recovery and precision for ETU and compared the performance of the method between the 2 water types. Over the concentration range tested, the mean percent recoveries of ETU were 82-92% in reagent water and 85-98% in finished drinking water. The range of the betweenlaboratory relative standard deviations (RSDR) for the 6 concentrations was 5-24% in reagent water, but was only 4-9% in finished drinking water. The range of the within-laboratory relative standard deviations (RSDr) was 6-14% for reagent water and 6- 10% for finished drinking water. Results for the 2 water matrixes showed no statistically significant differences. The method has been adopted first action by AOAC International for determination of ETU in finished drinking waters.
Modified Method for the Determination of Ivermectin Residues in Animal Tissues
Authors: Salisbury Craig D C 
Published: February 2020

Abstract
A simple, reliable method for determining residues of ivermectin in animal tissues is described combining existing sample cleanup procedures for muscle and for feed. Sample extracts are purified on alumina, C18, and silica solid-phase extraction cartridges, and ivermectin is determined by liquid chromatography with fluorescence detection. The average recovery of ivermectin from cattle, swine, and sheep muscle and liver was 87%, in the range of 5-25 ppb. Recovery from fish muscle was 77%, in the range of 5-30 ppb. The detection limit in tissue is 2 ppb.
Rapid Test for Semiquantitative Determination of Nitrate in Forages: Intralaboratory Study
Authors: Jain Anant V 
Published: February 2020

Abstract
A method is described for the semiquantitative determination of nitrate in forages by use of a commercially available test strip. A finely ground sample is extracted with deionized water. The color of the reaction zone on the test strip changes from white to pink or purple depending on the nitrate concentration in sample extract. The color on the test strip is compared with the color scale on the test strip container. An intralaboratory study demonstrated the applicability of the test strip to forages with nitrate concentrations from 200 to &gt;10 000ppm.
Solubility of Antibiotics Used in Animal Feeds in Selected Solvents
Authors: Salvatore Michael J , Katz Stanley E 
Published: February 2020

Abstract
The solubility of antibiotics used in animal feeds in organic solvents was determined. The solubility data could be used in identification of classes and in some cases individual members of the same class of antibiotics, and in differential step(s) in the analysis of these antibiotics. A universal solvent was developed to extract ail antibiotics from animal feeds.
Variability Among Peanut Subsamples Prepared for Aflatoxin Analysis with Four Mills
Authors: Dorner Joe W , Cole Richard J 
Published: February 2020

Abstract
The variability in aflatoxin concentration among peanut subsamples ground with 4 different mills was evaluated. Twenty 2 kg samples of naturally contaminated peanuts were ground in a Dickens subsampling mill (DM), a Stephan model UM-12 vertical cutter mixer (SM), and a Robot Coupe model RSI6Y-1 vertical cutter mixer (RC1). Twenty 4 kg samples were ground in the DM, SM, and a Robot Coupe model R10P vertical cutter mixer (RC2). From each 2 kg sample, ten 100 g subsamples were withdrawn, and from each 4 kg sample, ten 200 g subsamples were withdrawn. Subsamples were analyzed for aflatoxin by liquid chromatography. The coefficient of variation (CV) among each set of 10 subsamples was determined for each sample, and the CVs for each sample size were ranked and analyzed by the Kruskal-Wallis test of ranks. For 2 kg samples, the CVs for the samples ground in RC1 ranked significantly lower than those for samples ground in DM and SM. For 4 kg samples, the CVs for samples ground in RC2 and SM were significantly lower than that for samples ground in DM. The averages of the CVs for 2 kg samples were 17.2% (RC1), 32.8% (SM), and 40.6% (DM). The averages of the CVs for 4 kg samples were 21.2% (RC2), 26.0% (SM), and 47.0% (DM).