bluuebunny/crossref_metadata_2025_split huggingface dataset:
Gas-Liquid Chromatographic Determination of Bromoxynil Octanoate: Collaborative Study
Authors: Helfant Laurence J ,   Collaborators:, Audino J , Grimes G S , Karr J J , Muth G , King W , Norris J , Schapira J , Linde D C Vande , Winstead G 
Published: February 2020

Abstract
The assay of bromoxynil octanoate by a gasliquid chromatographic (GLC) procedure with din-n-butylphthalate as the internal standard was previously subjected to collaboration. The method had a standard deviation of 0.6% but results varied according to the complexity of the formulaation being tested. To reduce the systematic errors of the method, the internal standard was changed to n-docosane. The change in elution time of the marker simplified the chromatogram and reduced the standard deviation of the study to 0.3%. The revised method has been adopted as official first action for determining bromoxynil octanoate.
Analytical Characteristics of Late-Eluting Halogenated Flame Retardants
Authors: Miller Lee J , Puma Bartholomew J 
Published: February 2020

Abstract
The analytical characteristics of halogenated flame retardants were studied. Suitable electron capture gas-liquid chromatographic conditions were developed, and retention times and sensitivity responses were obtained. The behavior of these industrial chemicals through the AOAC multiresidue method for nonfatty foods was studied using fish as the test substrate. Of the 24 flame retardants investigated, 23 were recovered (85-110%) using the AOAC method.
Separation of Normal Paraffins and Evaluation of Petroleum Contamination in Foods
Authors: Saito Yukio , Takeda Mitsuharu , Uchiyama Mitsuru 
Published: February 2020

Abstract
A method for separating n-paraffins from petroleum hydrocarbons in foods was developed. The method consists of 5 initial steps: digestion of sample with alkali, silica gel column chromatography, molecular sieve adsorption, destruction of the sieve with HC1, and oxidation with KMnO4. Recoveries of n-paraffins added to 55 g oyster at a level of 0.36 ppm ranged from 80% for normal pentadecane to 100% for n-paraffins over 18 carbon atoms. This method also facilitated the analysis of iso-paraffins such as pristane (2,6,10,14-tetramethylpentadecane) and phytane (2,6,10,14-tetramethylhexadecane), and other hydrocarbons, which are thought to be good marker compounds for the estimation of petroleum pollution.
Automated High Pressure Liquid Chromatographic Determination of Uncombined Intermediates in FD&C Red No. 40 and FD&C Yellow No. 6
Authors: Singh Manjeet , Adams Gloria 
Published: February 2020

Abstract
An automated high pressure liquid chromatographic (HPLC) method is presented for the isolation and determination of uncombined intermediates in FD&C Red No. 40 (Allura Red AC) and FD&C Yellow No. 6 (CI No. 15985). Samples of FD&C Red No. 40 containing 0.1-0.4% cresidine sulfonic acid (4-amino-5-methoxy-2-methyl benzene sulfonic acid), 0.1-0.3% Schaeffer's salt (6-hydroxy-2-naphthalene sulfonic acid), 0.02- 0.08% 4,4'- (diazoamino) -bis (5-methoxy-2-methyl benzene sulfonic acid), and 0.1-1.0% 6,6'-oxybis (2-naphthalene sulfonic acid) were prepared and analyzed by this method. Recoveries ranged between 95 and 101%. Sixty samples of FD&C Red No. 40 were analyzed by the automated HPLC method. Results showed good agreement with those of the manual HPLC method. Samples of FD&C Yellow No. 6 containing 0.1-0.4% sulfanilic acid (4-aminobenzene sulfanilic acid), 0.1-0.3% Schaeffer's salt, 0.02-0.08% 4,4'-(diazoamino)-dibenzene sulfonic acid, and 0.2-1.0% 6,6'-oxybis (2-naphthalene sulfonic acid) were prepared and analyzed by this method. Recoveries ranged between 96 and 101%. Forty samples of FD&C Yellow No. 6 were analyzed by the automated HPLC method. Results showed good agreement with those of the manual HPLC method.
High Performance Liquid Chromatographic Determination of Sulfanilic Add, Schaeffer’s Salt, 4,4´-(Diazoamino)-DibenzenensuIfonic Acid, and 6,6´-Oxybis(2-Naphthalenesulfonic Acid) in FD&C Yellow No. 6: Collaborative Study
Authors: Cox Elizabeth A ,   Collaborators:, Beswick R , Bille L , Gasper G , Gunn M , Johnson W , King J , Penta F , Richfield-Fratz N 
Published: February 2020

Abstract
Eight laboratories participated in a collaborative study of a high performance liquid chromatographic procedure for determining sulfanilic acid, Schaeffer's salt, 4,4´-(diazoamino)-dibenzenesulfonic acid (DAADBSA), and 6,6´-oxybis(2-naphthalenesulfonic acid) (DONS) in FD&C Yellow No. 6. The standard deviations for one analysis in any one laboratory for sulfanilic acid at 0.2%, Schaeffer's salt at 0.26%, DAADBSA at 0.1%, and DONS at 1.0% were 0.015%, 0.014%, 0.018%, and 0.077%, respectively. The method has been adopted as official first action.
Fish Species Identification By Thin Layer Polyacrylamide Gel Isoelectric Focusing: Collaborative Study
Authors: Lundstrom Ronald C ,   Collaborators:, Barmore C R , Krzynowek J , LaTerza A F , Little B W , O'Leary G P , Robohm R A , Wiggin K 
Published: February 2020

Abstract
A method for fish species identification by isoelectric focusing of sarcoplasmic proteins on LKB Ampholine PAGplates, pH 3.5–9.5, was collaboratively studied to determine whether photographs of protein patterns from authentic species could be used to identify unknown samples. Seven collaborators were sent 8 unknown samples in duplicate to identify from an 8 × 10 in. photograph of an Ampholine PAGplate showing standard protein patterns from 14 species of fish. The 7 collaborators identified the unknown samples with 93% accuracy. Eight of 14 monkfish samples were not identified correctly and showed protein patterns different from the protein patterns shown in the photographic standard. All of the incorrectly identified samples showed the same protein pattern. The other 7 unknown species were all correctly identified. The method has been adopted as official first action.
Hydroxymethylfurfural and Honey Adulteration
Authors: White Jonathan W , Siciliano James 
Published: February 2020

Abstract
The value of the determination of hydroxymethylfurfural (HMF) in the detection of invert sirup adulteration of honey is examined. Analysis of 481 samples of extracted honey and 41 comb honeys from producers, and samples of honey before and after processing from 8 packers provided basic data for establishing guidelines for HMF content of honey. A sample containing 20 mg/100 g or more should be considered as possibly adulterated and subjected to additional analysis for confirmation of the presence or absence of adulteration. Extremely high (about 50 mg/100 g) values are conclusive, however.
High Pressure Liquid Chromatographic Separation and Identification of Estrogens
Authors: Roos Robert W 
Published: February 2020

Abstract
The use of high pressure liquid chromatography for separating mixtures of various estrogens is described. Separations of as many as 9 estrogens were studied using normal and reverse phase partition systems; the reverse phase system was the most useful. The estrogens were detected at 254 nm, a wavelength that favors their detection at low concentrations. The results of the separation studies were applied successfully to the separation and identification of estrogens in aqueous suspensions of estrogenic substances and to conjugated estrogens in tablets, following hydrolysis of the conjugates. Most estrogen peaks were identified using chromatographic mobilities; in some cases chemical reaction with the estrogen was used to form derivatives to aid identification. In one instance, the ultraviolet-absorbing properties of the estrogen were compared with literature data in order to assign an identity.
Food Safety in Canada—Past, Present, and Future
Authors: Mckinley W Perce 
Published: February 2020

Abstract
I consider analytical chemists the salt of the earth. Not only are they almost always uncommonly gifted—apart from those few who have had trouble confirming my results—they play a paramount role in enabling society to ensure the safety of its food, drugs, air, and water. Without analytical methods, we would still be in the hands of those barbarians the toxicologists (I will pay for this remark), who could carry out analyses in biological terms such as writhings per 100 food tasters but could not tell whether it was the contamination or the cooking.
Extraction of Light Filth from Barley, Oatmeal, and Mixed Dry Infant Cereals: Collaborative Study
Authors: Dent Russell G ,   Collaborators:, Floyd D M , Nagy J , Olsen A R , Quaife J T , Sandarg D E , Senff W A 
Published: February 2020

Abstract
A new method has been developed for the extraction of light filth from oatmeal, barley, and mixed dry infant cereals which involves HC1 digestion followed by wet sieving. The residue is defatted in a paper cup, using isopropanol, and transferred to a 2 L Wildman trap flask with 40% isopropanol. Filth elements are extracted with light mineral oil. Interlaboratory studies resulted in 92 and 86% average recoveries of rodent hairs and insect fragments, respectively. The proposed method has been adopted as official first action.
Pulsed Positive Ion-Negative Ion Chemical Ionization Mass Spectrometry of Animal Drugs: Sulfonamides
Authors: Roach John A G , Sphon James A , Hunt Donald F , Crow Frank W 
Published: February 2020

Abstract
The analysis of sulfa drugs, using pulsed positive ion-negative ion chemical ionization (PPINICI) mass spectrometry (MS), generates both positive and negative spectra in a single experiment. The spectra afforded by PPINICI-MS permit systematic interpretation and prediction of fragmentation for this class of compounds. Comparison of the electron impact and PPINICI spectra of 17 sulfa drugs and selected derivatives demonstrates that the useful information available with this new technique exceeds that afforded by electron impact analysis.
Modification of the Method for Vitamin A in Foods and Feeds for Use with Margarine and Butter: Collaborative Study
Authors: Parrish Donald B ,   Collaborators:, Abel M , Ameiko L , Asarch L , Baillies T , Bueno M , DeRitter E , Ellefson W , Guthrie J , Hamill T , Herod L , Hlavinka L , Hsu J , Kuervers T M , Kuhr P , Landen W O , Moffitt R A , Noel R , Rigby C , Roberts R , Sanchez A S , Sykora C , Thorpe V , Waltking A E , Woodruff M 
Published: February 2020

Abstract
An adaptation of the method for vitamin A in feeds and foods to margarine and butter was studied in 1977 and 1978. The principal change was the use of 2 extractions with an ether-hexane mixture instead of one with hexane. Results of the 1977 test were not good enough to recommend adoption. The 1978 analytical samples consisted of 4 margarines, including a known, and a butter. Data were reported by 11 analysts. Averages for vitamin A (μg/g) and coefficients of variation (%) were, respectively: A (known)—7.2, 5.7; 1—8.2, 11.1; 2—11.4, 3.9; 3—7.6, 10.7; butter—8.5, 13.3; and for carotene: A—5.6, 6.4; 1—6.0, 5.5; 2—0; 3—5.8, 3.8; butter—3.1, 11.8. Carotene results were grouped reasonably closely and tended to be distributed randomly, but vitamin A results had a less random trend. Trifluoroacetic acid was studied as an alternative colorimetric reagent for determining vitamin A, with overall satisfactory results. The modification for determining vitamin A and carotene in butter and margarine, and the use of trifluoroacetic acid as an alternative colorimetric reagent have been adopted as official first action.
Determination of Geotrichum Mold in Citrus Juices: Collaborative Study
Authors: Cichowicz Stanley M , Bandler Ruth ,   Collaborators:, Blacketer S , Kaminski J , Woodward B 
Published: February 2020

Abstract
The sieve mesh sizes (Nos. 8, 16, and 230) specified in the official method for the Geotrichum mold count of fruits and vegetables, 44.079, are inadequate for citrus juices. Citrus tissue passes through the larger mesh screens and clogs the fine mesh No. 230 sieve. The fine citrus tissue prevents the separation of the mold from the product and the liquid. The proposed method changes the sieve series to Nos. 40, 140, and 230 mesh. A compromise is reached which permits the concentration of mold along with the citrus tissue and the elimination of the excess liquid. The method has been adopted official first action.
Analysis of Foods for Lead, Cadmium, Copper, Zinc, Arsenic, and Selenium, Using Closed System Sample Digestion: Collaborative Study
Authors: Holak Walter ,   Collaborators:, Birri J , Colonel G J , Hebert R O , Izzi J , Lim F , McNerney F G , Orczech G , Sulek A , Tepedino N , Walter C C , Woodson A 
Published: February 2020

Abstract
A method for the determination of cadmium, lead, copper, arsenic, selenium, and zinc is presented. This method involves digesting a food sample with nitric acid under pressure and using aliquots of the solution for analysis by suitable techniques. Cadmium, lead, and copper are determined by anodic stripping voltammetry (ASV) after heating with equimolar sodium nitrate/potassium nitrate; arsenic and selenium are determined by atomic absorption spectrophotometry (AAS) after generation of their respective hydrides; zinc is determined by conventional AAS. The combined recoveries and reproducibilities (CVR) of the collaborative study on this multielement analysis are: Cd, 89.14 (17.65) at 0.10–1.0 μg/g; Zn, 96.53 (5.59) at 16.7 and 66.7 μg/g; As, 99.50 (17.02) at 0.5 and 2.0 μg/g; Se, 95.17 (16.52) at 0.5 and 2.0 μg/g; Pb, 92.57 (15.22) at 0.3–3.0 μg/g; Cu, 108.39 (18.30) at 1.0–10.0 μg/g. The method has been adopted as official first action for cadmium, lead, arsenic, selenium, and zinc.
Colorimetry and High Performance Liquid Chromatography of Atrazine Residues in Soil: Comparison of Methods
Authors: Vickrey Thomas M , Karlesky Dori L , Blackmer Gary L 
Published: February 2020

Abstract
The colorimetric method for determining residual atrazine levels in soil is compared with reverse phase high performance liquid chromatography (HPLC). The soil samples are extracted with water-acetonitrile (10 + 90) and the filtrate is partitioned with methylene chloride. For the colorimetric analysis the organic phase is filtered through activity V alumina, collected, and evaporated to dryness. The residue is dissolved first in ethyl ether, and then in water as the ether is removed. The atrazine solution is buffered (citric acid, pH 7.0) and heated with added pyridine. When the reaction is complete, the product is complexed with ethylcyanoacetate, and the solution absorbance is measured at 550 nm. The complex obeys Beer’s law and has a sensitivity of 230 ng for a 1% full scale deflection at 1 AUFS. For the HPLC method, the methylene chloride extract is dried, the chromatographic solvent is quantitatively added (either chloroform or methanol), and the solution is analyzed with a UV detector at 254 nm. Minimum amount detectable for a 1% full scale deflection is 5 ng at 0.01 AUFS. Soil background interferences were investigated for both methods, and buffering the pyridine-triazine reaction solution was the most efficient method for removing the background for colorimetry. The recovery efficiencies for the colorimetric and HPLC methods were 45.5 ± 3.8% and 94.4 ± 3.4%, respectively.
Improvements to Assisted Distillation Cleanup of Pesticide Residues in Animal Fats
Authors: Heath Andrew B , Black Robert R 
Published: February 2020

Abstract
The assisted distillation technique, which was developed for the cleanup of pesticide residues from animal fats, has been improved. Nitric acid cleaning of distillation tubes resulted in a significant improvement in the recoveries of hexachlorobenzene (HCB) and lindane (from 76 to 92% and 84 to 89%, respectively). A larger U-tube condenser was developed that condensed 100% of all pesticides studied. With this new condenser, a study of distillation tube flow rates showed that pesticide recoveries at 600 ml nitrogen/min were generally better than those obtained at any other flow rate although recoveries were satisfactory at 400 and 800 mt/min. Recoveries of pesticides at distillation temperatures of 210–240°C were obtained with tubes cleaned with nitric acid, and using the larger U-tube condenser. The distillation temperature of choice was again 230°C because there was little variation from 220 to 240°C.
Economic Method for Analysis of Fluid Milk for Organochlorine Residues at the 10 ppb Level
Authors: Veierov Dan , Aharonson Nadav 
Published: February 2020

Abstract
A procedure is described to isolate and clean up organochlorines in fluid milk for gas chromatographic (GC-ECD) analysis. Extraction and cleanup are performed in the same glassware, an ordinary separatory funnel. The only chemicals needed are H2SO4 and petroleum ether. Size of milk samples is versatile provided proportions of the chemicals are adjusted accordingly. Recoveries greater than 80% are obtained for 18 common organochlorines added to the milk which correspond well with recoveries with official methods for determining incurred residues. The proposed procedure shows a low lipid carryover (about 1%), and extraneous interferences are minimal. Its inherent simplicity makes the method suitable for standardization, and the small number of operations permit semi- or full automation.
Vacuum Desiccation Methods for Determination of Free Water in Fertilizers: Interlaboratory Comparison
Authors: Duncan Russell D ,   Collaborators:, McBride C H , Hube E J , Kane P , Kemp S T , Rund R C , Sheffield L J 
Published: February 2020

Abstract
A vacuum desiccation method for determining free water in fertilizer, proposed by the International Organization for Standardization (ISO), was compared to the official AOAC vacuum desiccation method (2.013). The combined results of 4 U.S. laboratories showed, on the basis of 5 samples, that precision was better by the ISO method, but results were lower for 4 of the 5 samples. The AOAC method gave a slightly lower result for one sample.
Potentiometric Titration Methods for the Determination of Sodium Chloride in Certifiable Water-Soluble Colors: Collaborative Study
Authors: Brammell Wallace S ,   Collaborators:, Clark F R , Downey R H , Goldberg A , Gorman T , Hensley D , Kiernan H , King J H , Marcus S A , Mogg R , Moore M M , Sulek A M , Tait G , Trcka R , Westwell A 
Published: February 2020

Abstract
In a collaborative study, 7 laboratories successfully analyzed 8 different samples, in duplicate, by a manual potentiometric titration method. These same samples were used by 7 different laboratories in a concurrent collaborative study of the automated potentiometric titration method. The samples are dissolved in water and acidified, and soluble chloride is determined by titration with silver nitrate to the potentiometric end point. The methods are applicable to all water-soluble certifiable colors except D&C Red No. 19, at levels &gt;0.03% sodium chloride, although there is a positive error at very low levels for the automated titration. In halogenated fluoresceins, any iodide or bromide is determined as sodium chloride, but the maximum amount normally present is equivalent to &lt;0.2% sodium chloride. The sodium chloride content of the collaborative samples ranged from 0.04 to 18.2% for the manual method, and from 0.11 to 18.1% for the automated method. In general, except at very low sodium chloride levels, the precision of the automated method was good, although not as high as that for the manual method; single determination coefficients of variation ranged from 1.5 to 13.5% for the former, and from 1.2 to 2.7% for the latter. Recovery of 0.45% added sodium chloride ranged from 62 to 96%, and for 4.5% added sodium chloride it varied from 94 to 99% by the automated method. Recoveries ranged from 96 to 104% for 0,45% added sodium chloride and from 98 to 102% for 4.5% added sodium chloride by the manual method. The coefficient of correlation of the sample means for the manual and the automated methods was 0.9999%. The methods have been adopted as official first action.
Determination of Total Fat in Meat and Meat Products by a Rapid, Dry Column Method
Authors: Maxwell Robert J , Marmer William N , Zubillaga Marta P , Dalickas Gail A 
Published: February 2020

Abstract
A rapid, dry column method is proposed for determining fat in meat and meat products. Unlike AOAC procedures 24.005 and 24.006, this procedure measures total rather than crude fat. A 5 g sample is blended with anhydrous sodium sulfate in a mortar and is then reduced to a fine powder with Celite 545. The fat is eluted on a glass column, using dichloromethane-methanol (9+1). Solvent is removed from the eluate, and the resulting residue is weighed to calculate total fat of the sample. A determination takes 2.5 hr or less. Fat levels ranged from 7 to 90% in 15 meat samples. Quadruplicate determinations by this method and duplicate determinations by 24.005 (a) yielded overall means of 29.9 and 29.3% fat, respectively. Repeatability was 0.3% fat. The 0.6% mean difference is significant (P = 0.05) and represents a more complete extraction of polar lipids by the proposed method. Results of determinations by this method are compared with results by an accepted but laborious chloroform/methanol procedure for total fat recovery. Overall means and standard deviations of replicate determinations on 4 meats containing 4–30% fat were 12.8±0.1 with this method and 12.7±0.1 with the reference method.
Aflatoxigenic Potential for Aspergilli on Sucrose Substrates
Authors: Llewellyn Gerald C , Jones Hudson C , Gates James E , Eadie Thomas 
Published: February 2020

Abstract
Sucrose concentrations of 3, 10, 20, and 30% in Czapek Dox broth served as the carbon source for growth, aflatoxin production, and sporulation for Aspergillus parasiticus NRRL 2999 and A flavus NRRL 3557, 5862, and 5013. All cultures produced mycelial growth and sporulated in all sucrose concentrations during the 12-day growth period. The area of mycelial mat coverage per hour increased directly with increased sugar concentrations. The 20 and 30% sucrose concentrations inhibited mycelial growth for 5862. The 30% sucrose cultures of 3557 and 5862 failed to produce detectable levels of aflatoxins. All other isolates produced B1 and G1 in an approximately 4:1 ratio in all sucrose concentrations. Only 2999 was a substantial producer of aflatoxin in all 4 sucrose cultures, ranging from 72 to 96 μg/mL medium. A. flavus 5013 produced the most toxin, 144 and 126 μg/mL medium in the 10 and 20% sucrose cultures, respectively. The 10 and 20% sucrose cultures were most conducive to aflatoxin production. Since these sucrose levels correspond closely to the levels in many food and drink products, especially home-made products, care and attention should be taken to keep them free of aflatoxigenic spores. Extensive mycelial growth and sporulation, even in aflatoxigenic strains, do not necessarily result in comparably high aflatoxin levels. Routine extraction and quantitation procedures for aflatoxin were applicable and provided satisfactory results.
Extraction, Cleanup, and Quantitative Determination of Aflatoxins in Corn
Authors: Thean James E , Lorenz David R , Wilson David M , Rodgers Kathleen , Gueldner Richard C 
Published: February 2020

Abstract
A method is proposed for extraction and cleanup of corn samples for the quantitation of 4 aflatoxins by high pressure liquid chromatography (HPLC). After aqueous methanol extraction, ammonium sulfate treatment, and partition of aflatoxins into chloroform, sample extracts are partially purified on Sep-Pak cartridges or small columns packed with HPLC grade silica; cleanup requires only 13 mL solvent/sample. Aflatoxins B1, B2, G1, and G2 in the purified extract are resolved in ca 10 min by normal phase HPLC on a microparticulate (5 μm) silica gel column with a 50% water-saturated chloroform-cyclohexaneacetonitrile- ethanol solvent, and are measured by ultraviolet fluorescence in a silica gel-packed flowcell. Recoveries of added aflatoxins B1, B2, G1, and G2 were 84–118 % at levels of 1.5–125 μg/kg