bluuebunny/crossref_metadata_2025_split huggingface dataset:
Chloroform-Methanol Extraction Method for Determination of Fat in Foods: Collaborative Study
Authors: Daugherty Chester E , Lento Harry G ,   Collaborators:, Adams M L , Beckert E W , Bender M L , Berman S , Chow L , Davis C , Gedang D , Howe K , Murphy M J , Porcuna M , Sabolish G , Shen C-S J , Smith N M , Tessaro A 
Published: February 2020

Abstract
Achloroform-methanol extraction method (complete extraction of fat in 3 min) for determining fat in processed and prepared foods has been studied collaboratively. Fourteen collaborators reported single replicate fat results on 7 samples representative of various food types and 2 spiked samples by the proposed method. Each sample was accompanied by a blind duplicate. For statistical purposes, the blind duplicates were treated as paired observations, and there were 2 laboratory outliers. There was a 97.9% agreement among the results from the remaining 12 collaborators and the Associate Referee for the unfortified samples. Recoveries of 93.8 and 98.3% were obtained on fortified samples, based on results obtained from 11 collaborators. The statistical analysis of the results indicate (ranges for standard deviations were Sr = 0.083-0.528, Sb = 0.101-0.379, Sd = 8.130-0.631, for fat values ranging from 1.58 to 26.91%) that this method is adequate for quantitating the fat content in a wide variety of processed foods for nutritional labeling. The method has been adopted official first action.
Separation and Identification of Phencyclidine and Some of Its Analogs
Authors: Rao K Gurudath , Soni Shiv K 
Published: February 2020

Abstract
l-(l-Phenylcyclohexyl)piperidine (PCP) and 9 of its analogs have been separated and identified by using thin layer chromatography, high performance liquid chromatography (HPLC), gas chromatography-mass spectrometry (GC-MS), and infrared spectroscopy (IR). Spectral and chromatographic characteristics are discussed in terms of the structural variations observed in these compounds. Some compounds decomposed on the GC column; the HPLC procedure is a helpful substitute. A tentative scheme is proposed for the fragmentation of the major ions observed in the mass spectra. The effect of substitution on the IR spectra of the analogs was investigated.
Atomic Absorption Spectrophotometric Determination of Mercury in Mercury≃Containing Drugs: Collaborative Study
Authors: Holak Walter ,   Collaborators:, Baltz R , Elliott L , McGary E , McNerney E , Midwood R , Rupf J , Tepedino N 
Published: February 2020

Abstract
An atomic absorption spectrophotometric (AAS) method applicable to a wide variety of mercurycontaining drugs has been developed and subjected to a collaborative study. Samples were digested with a water-HCl-HN03 (4 + 3 + 1) mixture, and the mercury was determined in solution by AAS. High levels of mercury were measured with a conventional air-acetylene flame, whereas low levels were measured by the flameless technique. Each of 7 collaborators received duplicate synthetic samples of a tincture, an ophthalmic solution, and an antiseptic solution, and duplicate commercial samples of an ointment and an injectable. The overall mean value found by collaborators for mercury in these samples was 100.13%. The corresponding overall repeatability SD (CV, %) and reproducibility SD (CV, %) values were 2.18 (2.18) and 3.38 (3.38), respectively. The proposed AAS method has been adopted official first action.
Liquid Chromatographic Determination of Methyldopa and Methyldopa-Thiazide Combinations in Dosage Forms
Authors: Ting Susan 
Published: February 2020

Abstract
A liquid chromatographic (LC) method, using a reverse phase C18 column, an acetic acid-methanol-water mobile phase, and detection at 280 nm, was developed for the determination of methyldopa in tablets and oral suspensions and combinations of methyldopa with hydrochlorothiazide or chlorothiazide in tablets. A mixture of these 3 drugs was resolved in &lt;8 min. Detector responses were linear for the following amounts (mg/mL) of drug injected: methyldopa 0.031-0.393, chlorothiazide 0.019-0.114, and hydrochlorothiazide 0.004-0.083. Recoveries from commercial dosage forms ranged from 99.1 to 100.9% for methyldopa, 99.2-100.4% for chlorothiazide, and 100.0-101.2% for hydrochlorothiazide. Replicate injections of methyldopa, chlorothiazide, and hydrochlorothiazide standard preparations alone or in combination gave overall relative standard deviations of &lt;1.6% (n = 10). The results for methyldopa tablets by the proposed method were in agreement with those obtained by the USP XX method. The LC method detected as little as 0.6 μg 3-O-methylmethyldopa/mL and 0.5 μg 4-amino-6- chloro-l,3-benzenedisulfonamide/mL, which are sometimes found as contaminants of methyldopa and thiazides, respectively, and resolved methyldopa from its methyldopa glucose adduct, a substance found in methyldopa oral suspensions.
Pesticide, Metal, and Other Chemical Residues in Adult Total Diet Samples. (XIII). August 1976–September 1977
Authors: Johnson Roger D , Manske Dennis D , New Dallas H , Podrebarac David S 
Published: February 2020

Abstract
The Food and Drug Administration has conducted the Total Diet Study since 1964. The program originally focused on the average total diet of the young adult male but was eventually expanded to include the average total diets of infants and toddlers. This report is the fourth in the infant and toddler series and represents residues found in market basket samples, i.e., items comprising the average 2-week diet of infants and toddlers, collected in 10 different cities throughout 4 geographic areas of the United States from October 1977 through September 1978. The results are based on analyses of food composites representing 11 food classes into which all the food items were separated. Averages and ranges are reported for residues of pesticides, herbicides, fungicides, and selected metals and industrial chemicals. Recovery results are also included for various representative compounds added to a variety of food classes. The results for the adult market basket samples for the same reporting period are presented in a separate report.
Malt Beverages and Brewing Materials: Gas Chromatographic Determination of Ethanol in Beer
Authors: Cutaia Anthony J 
Published: February 2020

Abstract
The American Society of Brewing Chemists collaboratively tested a gas chromatographic method for determination of ethanol in beer. Ten laboratories collaborated in a comparison of the ASBC reference method for alcohol by distillation with the GC method. The latter was shown to be at least as precise as the former, it is more rapid, and it can be used for in-line or process monitoring. The method has been adopted official first action.
Liquid Chromatographic Determination of Ascorbic Acid in Foods
Authors: Ashoor Samy H , Monte Woodrow C , Welty Jim 
Published: February 2020

Abstract
Ascorbic acid has been determined quantitatively in a variety of fresh and frozen fruits and vegetables, fresh and fortified canned juices, and powdered drinks by liquid chromatography (LC). The method consists of blending the sample in a solution of 0.05% EDTA in 0.2N H2S04, centrifuging or filtering the mixture, then injecting a portion into the LC system. An Aminex HPX-87 LC column was used with 0.009N H2S04 as solvent with a flow rate of 0.5 mL/min. Detection was at 245 nm. The method is simple and sensitive, and yields a high recovery. It compares favorably with the AOAC method, and has the advantage of being more accurate for samples with interfering pigments.
Liquid Chromatographic Determination of Methocarbamol in Injection and Tablet Dosage Forms: Collaborative Study
Authors: Everett Richard L ,   Collaborators:, Allgire L , Ballbach R J , Booth J , Johnson D , Lookabaugh M , Tyson B C 
Published: February 2020

Abstract
A reverse phase liquid chromatographic method was developed for determining methocarbamol in injection and tablet dosage forms. The injections require dilution only; the tablets require a nitration step before introduction into the chromatograph. Response for methocarbamol was linear over the range 0-18 μg, using an ultraviolet detector at 274 nm. Recoveries by the author ranged from 96.1 to 101.9% for authentic injection formulations and 98.0 to 101.0% for authentic tablet formulations. A collaborative study of the method by 6 laboratories resulted in standard deviations of 1.70 and 2.22 for injection and tablet dosage forms, respectively. The method has been adopted official first action.
Multiresidue Gas Chromatographic Method for Determining Organochlorine Pesticides in Poultry Fat: Collaborative Study
Authors: Ault James A , Spurgeon Tim E ,   Collaborators:, Anderson M M , Bowers R , Brunton E , Gillard D F , Johnson F , Johnson R W , McDaniel C A , Meyer K A , Miller B W , Mitchell J , Osheim D J , Patel V , Richardson H , Roof J , Stogsdill C 
Published: February 2020

Abstract
A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for a-BHC, lindane, cis- and frans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.
Liquid Chromatographic Determination of Methiocarb in Technical and Formulated Products: Collaborative Study
Authors: Slahck Stephen C ,   Collaborators:, Carlstrom A A , Chenery L T , Ellis N D , Folsom B D , Forrette J E , Gentry G M , Jensen T , Jurgens D , Korger P D , Laster W G , Mummah L , Pearson P M L , Stroh S , Wong D L 
Published: February 2020

Abstract
An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. The method has been adopted official first action.
High Performance Thin Layer Chromatographic Identification of Synthetic Food Dyes in Alcoholic Products
Authors: Steele John A 
Published: February 2020

Abstract
High performance thin layer chromatography systems using 2 multicomponent solvent systems are described for the separation and identification of FD&C permitted dyes Yellow No. 5, Yellow No. 6, Red No. 40, Red No. 3, Blue No. 1, Blue No. 2, Green No. 3; FD&C delisted dyes for foods: Amaranth, formerly certified as FD&C Red No. 2, Red No. 1, Red No. 4 (delisted for foods, permitted for external drugs and cosmetics); D&C dyes Yellow No. 10, Green No. 5, and Red No. 4. The method is suitable for the rapid monitoring of synthetic food dyes in alcoholic beverage products. Also, the method offers the means of qualitative and quantitative spectrodensitometry of synthetic food dyes found in alcoholic beverage products.
Confirmation of Pesticide Residue Identity. XI. Organophosphorus Pesticides
Authors: Lee Hing-Biu , Weng Li-Da , Chau Alfred S Y 
Published: February 2020

Abstract
Modification of a method previously published by us generates a wider scope and more rugged procedure for the confirmation of 9 organophosphorus pesticides (OPs). This method involves the hydrolysis of OPs to the corresponding phenols which are then derivatized to their pentafluorobenzyl (PFB) ethers. The ethers are subsequently cleaned up and fractionated on a 5 % deactivated silica gel column and analyzed by electron capture gas chromatography. This procedure enables the confirmation of levels of 10–0.01 ppb OPs from 1 L of water.
Gas Chromatographic Determination of Metribuzin in Formulations: Collaborative Study
Authors: Betker William R ,   Collaborators:, Anderson D , Bajovich J M , Bennett O O , Carlstrom A A , Chenery L T , Chiang T C H , Doherty P J , Forrette J E , Grypa R , Hageman L , Hodgins E , Karr J J , Koenig D K , Korger P D , Launer J E , McDaniel S , Meinen V J , Minyard J P , Owen M E , Polli R L , Sabbann M , Teubert W E , Torma L , Victoria V C 
Published: February 2020

Abstract
A collaborative study was conducted on a gas chromatographic method for determining metribuzin. Two 75% dry flow able and two 42% liquid flowable formulations were analyzed by 18 laboratories. Formulations were extracted by shaking or ultrasonic mixing for 1-5 min with methylene chloride which contained di-n-butyl phthalate as an internal standard. The extracts were injected into a gas chromatograph equipped with an OV-225 column. Peak area ratios and peak height ratios showed no significant difference. The reproducibility coefficient of variation was 0.75% for the 75% formulation and 1.41% for the 42% formulation. This GC method has been adopted official first action.
Liquid Chromatographic Determination of Lactose Purity: Collaborative Study
Authors: Saucerman Janice R , Winstead Charles E ,   Collaborators:, Casaletto P J , DeAngelis N J , Foglia T A , Greene G W , Helbig T , Hugunin A G , Mills R S , Nupson H , West L G , West L G , Zimmermann A F 
Published: February 2020

Abstract
Results from 8 laboratories are presented for the collaborative study of a proposed method for quantitative liquid chromatographic (LC) determination of lactose purity. Each laboratory was provided with 10 blind duplicate, edible-grade lactose samples plus a lactose reference standard and a fructose internal standard. Testing required the comparison of aqueous 2% lactose sample solution against a reference standard of equal concentration and quantitation by using a fructose internal standard. The LC system specified an isocratic acetonitrilewater (80 + 20) mobile phase, flow rate 2.0 mL/min, and chromatographic separation on a carbohydrate column. Compounds were detected by using refractive index. Statistical analysis for all study data indicates excellent between-laboratory precision with a coefficient of variation (CV) range of 0.53-1.37% and an overall average of 0.977%. Statistical analysis after excluding outliers showed equally good repeatability and reproducibility of less than 1 % and 1.5% CV, respectively. The method has been adopted official first action.
Comparison of Helium Leak Test and Vacuum Leak Test Using Canned Foods: Collaborative Study
Authors: Rhea Ulysses S , Gilchrist James E , Peeler James T , Shah Dhirendra B ,   Collaborators:, Allen B , Hoffman D , Landry W , Radle C D , Shields S , Tepidino A , Varney G 
Published: February 2020

Abstract
Two can leak tests were compared by 7 collaborators. In the helium leak test, pressurized helium is applied to the outside of the container, and a headspace gas sample from the can is then analyzed for the presence of helium. The vacuum test is described in the Bacteriological Analytical Manual. Ninety No. 303 cans of creamed-style corn, green beans, carrots, fruit cocktail, and whole-kernel corn were shipped in 3 groups. Two groups of 30 cans had 10 dented flat cans, 5 flat controls (nondented), 10 dented swollen cans, and 5 swollen control cans (nondented). The third group had 10 dented swollen cans and 5 swollen control cans. Of 600 cans analyzed, 37 (6.2%) were deleted from the analysis because results were not available for both tests. One laboratory was constrained by scheduling to analyze 15 of 45 swollen cans. The helium leak test found 12 (13%) positives of 92 nondented swollen cans. One pressurization test yielded 7 of those 12 positives. Of the 400 dented cans sent as possible leakers, the helium test found 267 positives, and the vacuum test found 181. Five of the 7 analysts had significantly (α = 0.05) higher percent positive helium results. One analyst found more leakers by the vacuum leak test. Both tests found fewer positives in the swollen dented cans than in the flat dented cans. After exposure to pressurized helium, all cans with greater than 8 psi headspace pressure were positive helium leakers. The method was adopted official first action.
Development of an Overnight Rapid Bovine Identification Test (ORBIT) for Field Use
Authors: Mageau Richard P , Cutrufelli Mark E , Schwab Bernard , Johnston Ralph W 
Published: February 2020

Abstract
An Overnight Rapid Bovine Identification Test (ORBIT) has been developed as a serological screen test for species verification of raw, whole tissue, bovine meat products. The test, an agar-gel immunodiffusion technique, uses stabilized reagent paper discs and prepared agar plates that have a printed template for correct placement of test components. This test is reliable, practical, economical, and easily performed in the field, such as at a meat import inspection station. The only nonbovine species found to react in the test are the bovine-related species of American bison (buffalo) and water buffalo (from Australia); however, these rare-occurring species do not present a problem for the intended application of the test. Stability of all test components, when stored in a refrigerator, is excellent for at least 1 year. The nature and stability of the test make it suitable for commercial development into test kits which should be highly practical and economical for wide availability and application of this procedure to meat inspection programs concerned with species verification.
Inter- and Intra-laboratory Variability in Rat Growth Assays for Estimating Protein Quality of Foods
Authors: Sarwar Ghulam , Blair Robert , Friedman Mendel , Gumbmann Michael R , Hackler L Ross , Pellett Peter L , Smith Trevor K 
Published: February 2020

Abstract
Protein efficiency ratio (PER), relative PER (RPER), net protein ratio (NPR), relative NPR (RNPR), and nitrogen utilization (NU) methods were investigated in an interlaboratory rat growth study. Six collaborating laboratories studied 7 protein sources (ANRC casein; minced beef; soya assay protein, SAP; pea flour; whole wheat flour, WW; rapeseed protein concentrate, RPC; and egg white solids, EW), and their 10 supplementary or complementary mixtures (casein + Met, SAP + Met, pea flour + Met, WW + Lys, WW + casein, WW + beef, WW + SAP, WW + pea flour, WW + RPC, WW + EW). Test protein(s) were added at the 8% level (N × 6.25). Casein + Met was used as the reference protein. Interlaboratory variation (estimated as between-laboratories coefficients of variation) of PER (up to 17.2%) was greater than that of RPER (up to 14.9%), NU (up to 9.5%), NPR (up to 7.0%), and RNPR, which had the lowest variability (up to 4.7%). In most cases, intralaboratory variation (estimated as within-Laboratories coefficients of variation) for all the methods was less than 5%.
Spectrophotometric Determination of Pentaerythritol Tetranitrate in Tablets
Authors: Shingbal Dattatray M , Agni Ramesh M 
Published: February 2020

Abstract
A sensitive spectrophotometric method is reported for the quantitative determination of pentaerythritol tetranitrate in tablets. The method is based on reduction of pentaerythritol tetranitrate with zinc and calcium chloride, and reaction of the nitroso compound thus formed with 1-naphthylamine in acidic medium. The reaction gives a purple product having an absorbance maximum at 545 nm. Beer's law is obeyed in the concentration range of 1-10 μg/mL of reaction mixture. The presence of meprobamate in tablets does not interfere with the proposed analytical determination.
Instrumental Color Classification of Honey: Collaborative Study
Authors: White Jonathan W ,   Collaborators:, Beaty M R , Eaton W G , Hart B , Huser W , Killion E , Lamssies R R , Lee T , Moen W E , Nelson S L , O'Neal R , Probst J , Shepard G H , Stevenson W V , Teas J 
Published: February 2020

Abstract
A collaborative study was carried out to test the use of the Lovibond 2000 honey color comparator. Fourteen collaborators classified 6 honeys in the test. Results were generally favorable and the method has been adopted official first action.
The Luke et al. Method for Determining Multipesticide Residues in Fruits and Vegetables: Collaborative Study
Authors: Sawyer Leon D 
Published: February 2020

Abstract
Ten laboratories analyzed unfortified and fortified samples of lettuce, tomatoes, and strawberries for organochlorine and organophosphorus pesticides by applicable portions of the comprehensive multipesticide method of Luke et al. The 3 crops were fortified with 6 pesticides, a-BHC, dieldrin, chlorpyrifos, acephate, omethoate, and monocrotophos, each at 3 levels per crop. Included in the 54 fortifications were 16 pairs of blind duplicates: same pesticide, crop, and level. Recoveries were calculated by area comparisons with known reference materials, using the responses obtained from 2 separate element-specific gas chromatographic (GC) systems. The organochlorine pesticides were chromatographed on a methyl silicone column and detected with a Hall 700A electrolytic conductivity detector, and the organophosphorus pesticides were determined with a flame photometric detector after being chromatographed on a specified DEGS column material. Chlorpyrifos was quantitated on both GC systems. Mean recoveries ranged from 82.6% for acephate fortified at 0.5000 ppm in strawberries to 118.1% for 0.0636 ppm fortification of chlorpyrifos in lettuce. Interlaboratory coefficients of variation ranged from 4.0% for 0.6360 ppm fortification of chlorpyrifos in tomatoes to 17.8% for the 0.0636 ppm chlorpyrifos level in lettuce. The procedure features essentially no cleanup before GC and proved comparable to existing multiresidue methods for pesticides of the class types studied, as evidenced by the intra- and interlaboratory measurements of precision and recoveries obtained. The method with the 2 GC systems has been adopted official first action.
Determination of Ethanol in Wine by Titrimetric and Spectrophotometric Dichromate Methods: Collaborative Study
Authors: Pilone Gordon J 
Published: February 2020

Abstract
A dichromate-spectrophotometric method for the determination of ethanol in wine was compared in a collaborative, matched pair study with the AOAC dichromate-titrimetric method, 11.008-11.011. Both methods require distillation of the sample into dichromate. The titrimetric method measures ethanol by titrating the excess dichromate with ferrous ammonium sulfate after conversion of ethanol to acetic acid; the spectrophotometric method directly measures the reduced dichromate formed after oxidation. In addition to comparing the 2 methods, the collaborative study also compared the use of 2 types of assemblies for obtaining the ethanol distillate: the Scott-type, which is used in 11.008-11.011, and the electric Kirk-type. Results of the collaborative study indicated that the repeatability and reproducibility of the official titrimetric method were generally far superior to those of the spectrophotometric method; therefore, adoption of the spectrophotometric method is not recommended. Comparison of titrimetric method results obtained using the 2 types of stills indicated that repeatability and reproducibility were somewhat better when Scott apparatus was used, but measurements using Kirk-type compared well in the range of ethanol concentrations found in table and fortified wines. The Kirk-type distillation apparatus has been adopted official first action as an alternative to Scott apparatus in the dichromate oxidation method for ethanol in wine, 11.008-11.011.