bluuebunny/crossref_metadata_2025_split huggingface dataset:
Report of Ad Hoc Committee on Vitamin D Methodology, AOAC
Authors: Quackenbush Forrest W , Banes Daniel , Derse Philip H 
Published: February 2020

Abstract
In a collaborative study 6 samples of vitamin D3 resins were analyzed chemically by 9 laboratories and tested biologically by 3 laboratories to determine whether there exists a discrepancy between chemical and biological methods of measuring potency of these materials. The chemical methods employed saponification with and without subsequent maleic anhydride treatment. The biological method was the AOAC official final action rat assay, 39.149–39.162. The results showed good agreement between laboratories in the chemical analysis and relatively poor agreement in the biological tests. However, based upon the mean values as reported by the different laboratories, the chemical method employing saponification alone consistently overestimated biopotency, whereas the chemical method including maleic anhydride treatment gave results which averaged much closer to the mean biopotency values. There was no evidence that maleic anhydride treatment reduced values significantly below biopotency values.
Collaborative Study of a Method for the Extraction of Light Filth from Crushed Red Peppers
Authors: Thrasher Joel J 
Published: February 2020

Abstract
A new method was developed for the extraction of light filth from crushed red peppers. The method utilizes an isopropanol defatting of the product followed by separation of light filth elements with mineral oil and n-heptane (85+15) in a 2 L trap flask. Collaborative studies resulted in good recoveries of light filth spike elements and clean extraction papers. The method has been adopted as official first action.
Collaborative Study of a Method for the Extraction of Light Filth from Whole, Cracked, or Flaked and Ground Spices
Authors: Glaze Larry E 
Published: February 2020

Abstract
An improved method has been developed for the extraction of light filth from whole, cracked, or flaked spices (basil, bay leaves, celery leaves, chervil, chives, dill weed, mint flakes, parsley, rosemary, sage, tarragon, thyme, and vegetable flakes) and from ground spices (cloves, cumin, marjoram, mustard seed, oregano, sage, and thyme). The method involves a chloroform or isopropanol defatting, followed by a direct flotation from 40% isopropanol with Tween 80-EDTA (1+1) and mineral oil-heptane (85+15). Collaborative results show that the proposed method is more rapid to perform and yields better filth recoveries than the official first action methods for ground spices, 44.116, and whole, cracked, or flaked spices, 44.129. The method has been adopted as official first action.
Collaborative Study of a Method for the Extraction of Light Filth from Ground Turmeric
Authors: Glaze Larry E 
Published: February 2020

Abstract
An improved method has been developed for the extraction of light filth from ground turmeric. The method involves an isopropanol defatting followed by a direct flotation from 40% isopropanol with Tween 80-EDTA (1+1) and hot mineral oil. Collaborative results show that the method is rapid and yields better filth recoveries than the official first action method, 44.118. The method has been adopted as official first action to replace 44.118.
Multiple Automated Analyses for Orange Juice Content: Determination of Total Sugars, Reducing Sugars, Total Acidity, Total Amino Acids, and Phenolics
Authors: Vandercook Carl E , Price Ruth L , Harrington Christina A 
Published: February 2020

Abstract
Developing methods for determining orange juice content in orange products requires the analyses of many samples. To speed up and simplify the acquisition of data, an automated analytical system was devised whereby 5 constituents were measured on a single manifold. Sample preparation involves diluting to single strength, if necessary, and removing any large pulp particles by filtering or centrifuging. Converting from one analysis to another requires only a change in the colorimeter filter, reagents, and 1 or 2 tubes. The automated procedures were tested on 150 samples of California, Florida, and foreign orange juices. Averages and standard deviations for all samples were 10.2±0.9 g/100 ml, 6.1±0.7 g/100 ml, 12.2±2.8 mequiv./lOO ml, 2.52±0.89 mequiv./lOO ml, and 109±31 mg phenol equiv./lOO ml, for total sugars, reducing sugars, total acidity, total amino acids, and phenolics, respectively. Ratios of the data were calculated for the various juice types and sources.
Gas-Liquid Chromatographic Determination of Docosenoic Acid in Fats and Oils: Collaborative Study
Authors: Conacher Henry B S 
Published: February 2020

Abstract
A gas-liquid chromatographic method for the determination of docosenoic acid in fats and oils was studied collaboratively, using 2 corn oil mixtures spiked with 3.73 and 5.59% methyl erucate, respectively, and 10 oil mixtures containing docosenoic acid at levels between 2 and 30%. Average recoveries from the 2 spiked corn oil samples were 96.5 and 98.7% with coefficients of variation of 4.0 and 3.1%, respectively. With the 10 oil mixtures coefficients of variation ranged from 1.9% at 28.1% docosenoic acid level to 11.1% at 2.7% docosenoic acid level. The method has been adopted as official first action.
Collaborative Study of a Gas-Liquid Chromatographic Method for the Analysis of Chlorobenzilate and Chloropropylate
Authors: Hofberg Arthur H , Heinrichs Lee C , Gentry Gene A 
Published: February 2020

Abstract
A gas-liquid chromatographic method for the determination of chlorobenzilate and chloropropylate in liquid formulations containing about 46 and 26% active ingredient, respectively, was collaboratively studied, using a matched pair scheme. The samples were dissolved in acetone containing dibenzyl succinate as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector. Analyses of 4 samples by 13 collaborators using peak height measurements showed the following results: chlorobenzilate—2.5% overall coefficient of variation, 1.0% coefficient of variation for the random error; and 0.7% systematic error; chloropropylate—2.0, 1.4, and 0.4%, respectively. The method has been adopted as official first action.
Rapid Method for Extracting Aldrin, Dieldrin, and Endrin from Visceral Material
Authors: Kurhekar Madhao P , D’Souza Francis C , Meghal Sharadchandra K 
Published: February 2020

Abstract
A simple method is described for purifying aldrin, dieldrin, and endrin from visceral material by using a Celite column. Celite retains all interfering materials including lipids whereas the chlorinated insecticides are eluted from the column with n-hexane. This extract can be used directly for gas chromatographic analysis.
Determination of Residues from the Herbicide 2,4-Dichloro-l-(4-nitrophenoxy)-benzene in Rice and Wheat by Electron Capture Gas-Liquid Chromatography
Authors: Adler Irving L , Wargo Joseph P 
Published: February 2020

Abstract
A residue method has been developed which is capable of determining not only 2,4-dichloro-1-(4-nitrophenoxy)-benzene but a majority of the known metabolites of this compound. The residues are reduced to a common amine intermediate which is further derivatized and quantitatively measured by electron capture gasliquid chromatography. The method is sensitive to 0.01 ppm and is readily suited to routine use. The method has been used on rice and wheat samples.
Determination of Hexachlorobenzene and Mirex in Fatty Products
Authors: Bong Rodney L 
Published: February 2020

Abstract
A procedure is described for the isolation and cleanup of hexachlorobenzene (HCB) and mirex in fats and oils for gas-liquid chromatographic (GLC) analysis. The fat or oil is distributed on unactivated Florisil, and the HCB and mirex are eluted with acetonitrile. The pesticides are then partitioned into petroleum ether. Elution through activated Florisil with methylene chloride-hexane (20+80) is used for the final cleanup. HCB and mirex are then measured by GLC, using the appropriate electron capture conditions with a 15% OV-210 column for HCB and a 3% OV-101 column for mirex. The method demonstrates recoveries greater than 90% for HCB and mirex and allows screening at or below the 0.1 ppm level in fats with a 3 mg fat injection.
New Confirmatory Test for Aflatoxins B1 and B2
Authors: Ashoor Samy H , Chu Fun Sun 
Published: February 2020

Abstract
A new confirmatory test for anatoxins B1 and B2 is described. The test involves treatment of aflatoxins with excess sodium borohydride for 10 min at room temperature, to yield a fluorescent trihydroxy derivative of each aflatoxin. The test is sensitive and simple and gives no side reactions. The test is also applicable to aflatoxins G1 and G2.
Indirect Method for the Determination of Density of Solutions at Various Temperatures
Authors: Basker Dov 
Published: February 2020

Abstract
For solutions of solutes other than strong electrolytes, the density at temperature t2 may be derived from the density at t1, the refractive index at t1 and t2, and the refractive index of the solvent at t1, and t2. Good agreement was obtained between direct and indirect determinations of the density of sucrose solutions.
Metabolic Alterations in Organ Function
Authors: Plaa Gabriel L 
Published: February 2020

Abstract
When the standardization of procedures is envisioned, problems arise regarding the selection of the test procedure and its ability to detect changes in organ function. Dose-response curves can be derived for the parameters used for assessing dysfunction. These curves can be useful for selecting equitoxic doses of substances to be compared with each other. They can also be useful for estimating relative safety as well as absolute toxic potency. Enzyme inducers can be used to determine whether metabolic transformations are involved in toxic reactions. However, all enzyme inducers do not produce the same effect. It is necessary to clearly define the enzyme inducers that have to be employed. Interactions leading to enhanced toxic effects can occur by pathways other than enzyme induction. It is necessary to determine if the toxic interaction is the result of a change in the sensitivity of the organ to the presence of the toxic moiety. The experimental environment can also affect toxicity. The presence of pathology in laboratory animals may alter the response. Body temperature can also markedly alter the response to a toxic agent.
Toxicology Experimental Design and Conduct as Measured by Interlaboratory Collaborative Studies
Authors: Weil Carrol S 
Published: February 2020

Abstract
Interlaboratory variability in certain acute, toxicological procedures was discussed. Three collaborative studies have been performed. One study concerned a determination of acute peroral toxicity and 2 collaborative studies have involved eye and/or skin irritation. All have indicated that, while the majority of the laboratories produced relatively consistent results, some were definitely outliers and others were quite variable. Recommendations were made to counteract and correct this interlaboratory variability; it was suggested that these be accomplished before standardization of techniques be promulgated. A brief discussion was presented on the faulty conclusions that can result from improperly planned and executed repeated-dose toxicological studies. Furthermore, the estimation of risk at the low-response end of a doseresponse curve was discussed. The relative variability of the measurement of the slope of such a curve was compared to the variability of the measurement of the midpoint. The danger of extrapolation of animal dose-response results, using a constant slope, was deprecated.
Isobutane Chemical Ionization Mass Spectrographic Examination of Explosives
Authors: Saferstein Richard , Chao Jew-Ming , Manura John J 
Published: February 2020

Abstract
The detection of explosive residues in debris is difficult because of the thermal instability of many explosives along with the high sensitivity requirements of the analyses. The isobutane chemical ionization (CI) mass spectra of common civilian and military explosives were obtained under different instrumental parameters. The intent of the study was to determine the feasibility of applying CI to residue detection. The CI spectra of the explosives 1,3,5-trinitro-1,3,5-triazocydohexane, 1,3,5,7-tetraazocyclooctane, and pentaerythritol tetranitrate were shown to be particularly sensitive to the conditions of source temperature and reagent gas pressure. These parameters were adjusted to yield the least complex CI spectra for the explosives studied. The simplicity of the CI spectra obtained makes it a feasible technique for detecting explosive residues in the presence of extraneous materials found in the acetone extracts of debris material. Placement of the extract into the direct probe of the CI mass spectrometer eliminates the need for prior chromatographic treatment of the extract and would optimize the high sensitivity of the CI technique.
Collaborative Study of a Rapid Method for Determining Aflatoxins in Cottonseed Products
Authors: Pons Walter A 
Published: February 2020

Abstract
Eleven laboratories collaboratively studied a modification of the official final action AOAC method, 26.048–26.056, for determining aflatoxins in cottonseed products. An aflatoxinnegative meal, 6 contaminated meals, 4 contaminated meats (kernels) samples, and 2 ammonia-inactivated meals were used. Mean a (latoxin values, μg/kg, ranged from 6 to 223 (B1), 2 to 44 (B2), and 7 to 266 (total: B1 + B2). Only one laboratory reported a false-positive for the negative meal. The mean coefficients of variation for B1, B2, and total were 28, 56, and 29%, respectively, for meals; 35, 54, and 37%, respectively, for meats; and 35, 58, and 38%, respectively, for ammoniated meals. Statistical treatment of data from triplicate sets of meals and meats showed evidence for systematic error between laboratories. Since the modified method is considerably faster than the official method and yields precision estimates consistent with previous AOAC collaborative studies on determining aflatoxins, the method has been adopted as official first action.
Gas-Liquid Chromatographic Determination of Diethylstilbestrol in Molasses-Based Liquid Feed Supplements
Authors: Jain Anant V , Schall Elwyn D 
Published: February 2020

Abstract
A gas-liquid chromatographic (GLC) method is described for the determination of diethylstilbestrol (DES) in molasses-based liquid feed supplements, using dienestrol diacetate as the internal standard. A sample equivalent to 110 μg DES was diluted, acidified with dilute sulfuric acid, extracted with chloroform, and subjected to basic sodium acetate cleanup. The bis-(trimethylsilyl) acetamide derivative was prepared and determined by GLC. Interfering peaks and/or low recoveries were found to be related to emulsions and the procedure incorporates centrifugation to minimize these.
Fluorescent Antibody Method for the Detection of Salmonella: Development, Evaluation, and Collaborative Study
Authors: Fantasia Leonard D , Schrade John P , Yager James F , Debler Diane 
Published: February 2020

Abstract
In preliminary studies, several commercial polyvalent fluorescent antibody (FA) preparations were evaluated for specificity and crossreactivity and an FA method was developed for the screening of Salmonella in products. Approximately 4000 product samples were tested by the FA method and the results were compared to those from the official final action AOAC method, 46.013–46.026. Only 4 FA falsenegatives were found for a total of 619 confirmed positive Salmonella samples. The FA false-positive rate was 7%. The method was then subjected to a 2-phase collaborative study. In Phase I, 22 analysts tested 5 inoculated and 5 uninoculated samples of dried milk. In Phase II, 5 naturally contaminated and 5 presumably uncontaminated foods were analyzed. The study was designed to compare results from 11 analysts experienced in FA methodology with those from 11 analysts with little or no experience. Selenite cystine (SC) and tetrathionate (TT) broths were used for enrichment and both were inoculated into SC for post-enrichment. All 4 combinations (SC, TT, SC-SC, and TT-SC) were used with the FA method to determine the best technique. Results were compared to the analysis with TT and SC by the AOAC culture method. In all studies, FA analysis with SC-SC gave the highest correlation with the AOAC method. In a total of 200 samples, the experienced group found 125 AOAC positives and 127 FA positives ; no FA false-negatives and only 2 falsepositives were reported. The inexperienced group reported 9 FA false-negatives and 5 FA false-positives. All false-negatives occurred in only 3 of the inexperienced laboratories. These studies showed that enrichment and post-enrichment in SC gave the best FA results and that training in FA methodology is required for correlation with existing AOAC methodology. The FA method for the detection of Salmonella has been adopted as official first action.
Collaborative Study of an On-Column Periodate Reaction Method for the Determination of Ephedrine Sulfate in Sirups
Authors: Clark Charles C 
Published: February 2020

Abstract
Fifteen laboratories collaboratively studied a method for the quantitative ultraviolet determination of ephedrine sulfate in sirups. Ephedrine is separated from water-soluble impurities and strong acids by elution from a weakly basic Celite column. Further cleanup is accomplished by retention of the ephedrine on a weakly acidic column while the weak acids, weak bases, and organic-soluble neutral compounds are eluted. Ephedrine is eluted from the column after neutralization with NH3 and is converted to benzaldehyde via an on-column periodate reaction. The samples collaboratively studied consisted of 2 commercial ephedrine-containing sirups and 2 commercial non-ephedrine-containing sirups to which ephedrine was added. Recoveries for the spiked sirups averaged 100.7 and 100.3% for mixtures containing 2.5 and 5.0 mg ephedrine sulfate/ml, respectively. The means and standard deviations for the commercial preparations were 4.088 ± 0.068 and 2.375 ± 0.053 mg/ml. The method has been adopted as official first action and has been incorporated into the official method for phenylpropanolamine hydrochloride, 38.199–38.203.
Quantitative Determination of Relative Isomeric Ratios of IH- and 2H-Tetrazole-l-Acetic Acids and Their Ester Analogs by Nuclear Magnetic Resonance Spectroscopy
Authors: Staiger David B , Warren Richard J , Zarembo John E , Post Alex 
Published: February 2020

Abstract
A fast and accurate nuclear magnetic resonance spectroscopic method for the quantitative determination of IH- and 2H-tetrazole acetic acid isomeric mixtures is presented. The method takes advantage of the significant difference in chemical shift of the methylene groups or the ring protons in the 1- and 2-tetrazole acetic acid analogs. The relative ratio of the isomers is determined from the measured intensities of the methylene groups.
Gas-Liquid Chromatographic Determination of Technical Chlordane Residues in Food Crops: Interpretation of Analytical Data
Authors: Cochrane William P , Lawrence James F , Lee Young W , Maybury Ronald B , Wilson Brian P 
Published: February 2020

Abstract
An interlaboratory investigation of technical chlordane residues in food crops was carried out to determine the most practical and consistent method of reporting results. Using a technical chlordane reference standard, 8 gas chromatographic stationary phases were studied for their resolution capabilities. The best separations were obtained with SE-30 and its OV-1 equivalent. Using these columns and electron capture detection, potatoes and carrots from supervised field experiments were analyzed in duplicate and quantitated by using 4 methods of calculation. The data were statistically treated to determine the precision and bias for each method. Also, 1 sample was analyzed in duplicate on 2 different occasions by 6 laboratories to substantiate the initial conclusions. Based on the criterion of high precision it is suggested that a comparison of total area under the chromatogram of the sample with total area of a standard technical chlordane be the method of quantitation. Only peaks which are common to both standard and sample have any significance in this type of calculation.
Estimation of the Bioavailability of Iron
Authors: Fritz James C , Pla Gwendolyn W , Harrison Bertha N , Clark Geneva A 
Published: February 2020

Abstract
Eight laboratories conducted a test for the estimation of the bioavailability of iron from 4 sources, using depleted male albino rats. Ferrous sulfate was used as the reference standard. Ferric orthophosphate was found to have a relative biological value of 11 (range 6–22), an old sample of hydrogen-reduced iron 27 (range 15–41), and ferric citrate 96 (range 75–125). Good results were obtained with a simplified basal diet prepared without ingredients that had previously contributed variable quantities of iron. There was no apparent advantage in using the change in hemoglobin during the repletion period instead of the final homoglobin value as the criterion of response to iron supplements. Several statistical treatments of the data yielded similar conclusions regarding relative biological values of the iron sources.
Methods for the Detection of Trichothecenes
Authors: Eppley Robert M 
Published: February 2020

Abstract
The trichothecenes are a group of fungal metabolites with a tetracyclic, sesquiterpenoid ring system and include a number of compounds which are highly toxic. These compounds are produced by various species of the imperfect fungi including members of the following genera: Calonectria, Fusarium, Myrothecium, Stachybotrys, Trichoderma, and Trichothecium. Both biological and chemical methods for detection of various trichothecenes are reviewed. Some of the bioassay techniques in use for the detection of the various trichothecenes include the rabbit dermal toxicity test, cytotoxicity, and inhibition of protein synthesis tests; these are highly sensitive but lack specificity. The sensitivity of these tests for the T-2 toxin are 0.005 μg for rabbit skin toxicity, 0.03 μg/ml for inhibition of protein synthesis in rabbit reticulocytes, and &lt;1 μg/ml for cytotoxicity to human karyoblast cells. In the present state of development of the chemical assay methods, thin layer and gas-liquid chromatography are specific for various trichothecenes but lack sensitivity. The lower detection limit of the trichothecenes on thin layer plates varies from 0.2 to 2–3 μg/spot while gas-liquid chromatography has a reported sensitivity of approximately 0.05 μg/injection.
Patulin Production in Apples Stored in a Controlled Atmosphere
Authors: Lovett Joseph , Thompson Ruben G , Boutin Brenda K 
Published: February 2020

Abstract
Red Delicious apples were inoculated with Penicillium expansum NRRL 973 or P. expansutn 1071 (fresh apple isolate), and incubated in air at 33°F and in a controlled atmosphere of 1% carbon dioxide, 3% oxygen, and 96% nitrogen at 33°F. Both fungal strains produced the carcinogen, patulin, in the air-incubated lots, but only the freshly isolated strain (1071) produced detectable patulin in controlled atmosphere lots. Thin layer chromatography was used to assay ethyl acetate extracts of juice pressed from blended apple tissue. We conclude that naturally occurring P. expansum strains are capable of producing significant levels of patulin in apples stored from 3 to 6 months under controlled atmospheric conditions.