bluuebunny/crossref_metadata_2025_split huggingface dataset:
Determination of Zeranol/Zearalenone and Their Metabolites in Edible Animal Tissue by Liquid Chromatography with Electrochemical Detection and Confirmation by Gas Chromatography/Mass Spectrometry
Authors: Roybal Jose E , Munns Robert K , Morris William J , Hurlbut Jeffrey A , Shimoda Wilbert 
Published: February 2020

Abstract
A sensitive method is described for the determination and confirmation of zeranol and zearalenone, as well as their isomers and metabolites, in edible animal tissue. The analytes are extracted from tissue with methanol, hydrolyzed enzymatically, cleaned up by acidbase partitioning, determined by liquid chromatography (LC) with electrochemical (EC) detection, and confirmed by gas chromatography/ mass spectrometry (GC/MS). LC analysis is performed by isocratic elution with a buffered mobile phase using a Nova-Pak reverse-phase C,„ column with amperometric EC detection at +0.90 V. Capillary GC/MS analysis of the trimethylsilyl derivatives provides mass spectral confirmations.
Determination of Dextran in Raw Cane Sugar by Roberts Copper Method:
Collaborative Study
Authors: Clarke Margaret A , Godshall Mary An 
Published: February 2020

Abstract
A collaborative study was conducted using the Roberts copper method for the determination of dextran in raw cane sugars. Four samples were analyzed in duplicate, representing the range of dextran concentrations found in raw sugar. The overall repeatability and reproducibility coefficients of variation were 4.3 and 13.2%, respectively. The method has been adopted official first action.
Comparison of Four Thin-Layer Chromatographic Methods for the Determination of
Aflatoxins in Raisins
Authors: Boyacioglu Dilek , Gonul Meral 
Published: February 2020

Abstract
A study was conducted to determine the accuracy and precision of 3 AOAC methods, sees 26.026-26.031 (CB), sees 26.032-26.036 (BF), and sees 26.052-26.060 (cottonseed), and the Romer quantitative method for the thin-layer chromatographic (TLC) determination of aflatoxins B„ B2, G„ and G2 in raisins. The samples were spiked at a level of 10 Mg total aflatoxins/kg. The TLC development systems were: ether-methanol-water (94 + 4.5 + 1.5) and chloroform-acetone (9 + 1). The interaction between the 4 methods and the 2 development systems was also studied. The average recoveries were 88, 80, 75, and 93% with coefficients of variation of 14.0,10.4,14.0, and 9.6% for aflatoxin B, using the CB, BF, cottonseed, and Romer methods, respectively. Statistical analysis showed no difference in the results obtained using the 2 TLC development systems
Comparison of Stainless Steel Penicylinders Used in Disinfectant Testing
Authors: Cole Eugene C , Rutala William A , Alfano Edith M 
Published: February 2020

Abstract
Two brands of stainless steel penicylinders, S&L Metal Products and Fisher Scientific, were simultaneously tested to determine if they provide comparable results when used in the AOAC use-dilution method of disinfectant testing. Results showed consistently more positive tubes for the Fisher brand of penicylinders than for the S&L, regardless of the surface finish of the test cylinders.
Intercomparative Study on the Determination of Polynuclear Aromatic Hydrocarbons in Marine Shellfish Tissue
Authors: Uthe John F , Musial Charles J 
Published: February 2020

Abstract
Twenty-five laboratories were sent 2 materials, one an acetone powder of lobster digestive gland, the other, the oil which had been extracted during preparation of the powder. Each laboratory was requested to measure the levels of a suite of polycyclic aromatic hydrocarbons in both materials. The response was poor with only 10 laboratories submitting results. Both intra- and interlaboratory precisions were poor; the interlaboratory error was so great as to preclude statistical analysis of the error. Relative standard deviations for oil results determined by liquid chromatography ranged from 39 to 96%.
Determination of Inorganic Tin in Biological Samples by Hydride Generation-Atomic Absorption Spectrometry after Silica Gel Cleanup
Authors: Tsuda Taizo , Wada Minoru , Aoki Shigeru , Matsui Yoshihiro 
Published: February 2020

Abstract
A method is described for the determination of inorganic tin in biological samples by hydride generation-atomic absorption spectrometry (HG-AAS). A sample is extracted with ethyl acetate after addition of HC1 and NaCl. The concentrated extract is passed through a silica gel column. The column is washed with ethanol, water, and 0.2N HC1 successively, and then inorganic tin is eluted with 2N HC1 and measured by HG-AAS. Recoveries from fish muscle spiked with 0.1 ng/g Sn4+ are 78.9 ± 4.2% (average ± standard deviation, n = 5). The detection limit is 0.01 jug/g as Sn.
Detection of Poultry and Pork in Cooked and Canned Meat Foods by Enzyme-Linked
Immunosorbent Assays
Authors: Berger Ronald G , Mageau Richard P , Schwab Bernard , Johnston Ralph W 
Published: February 2020

Abstract
Enzyme-linked immunosorbent assays (ELISA) are described for the detection of poultry and pork in cooked and canned muat foods. These assays are based on species-specific, polyclonal antibodies raised against heat-resistant antigens. The heat-resistant antigens were isolated from raw skeletal muscle tissue of pork and chicken and were found to be immunoreactive even after heating to 120°C for 15 min. The poultry ELISA could detect chicken or turkey at the 126 ppm level, and the pork ELISA could detect pork at the 250 ppm level. Samples of frankfurters, bolognas, pressed meats, canned baby foods, and canned spreads were prepared by simple aqueous extractions
Ion Abundance Criteria for Gas Chromatographic/Mass Spectrometric
Environmental Analysis
Authors: Donnelly J R , Sovocool G W , Mitchum R K 
Published: February 2020

Abstract
Mass and intensity calibration of gas chromatograph/mass spectrometer (GC/MS) responses is an important quality assurance issue for chemical analysis. Ion abundance calibration with decafluorotriphenylphosphine (DFTPP) was applied in 1975 to standardize quadrupole spectra to resemble the ion abundances that were obtainable from magnetic sector mass spectrometers. Modern &lt;j uadrupole mass spectrometers provide significantly greater high-mass sensitivity than allowed under the 1975 study. Thus, those recommendations were reevaluated with 2 approaches. First, an interlaboratory study was conducted using 15 different gas chromatography/mass spectrometry (GC/MS) systems. Second, the U.S. Environmental I'rotection Agency Contract Laboratory Program (EPA-CLP) quality assurance data base was searched and over 6500 DFTPP tune results were plotted and evaluated. Based on these approaches, updated ion abundance criteria recommendations have been developed, which contemporary instruments can meet, and which meet data quality objectives regarding identification and quantitative analysis of analytes.
Liquid Chromatographic Determination of Cimetidine in Whole Blood and Plasma by Using
Short Polymeric Reverse Phase Column
Authors: Abu M Rustum , Hoffman Norman E 
Published: February 2020

Abstract
A rapid and simple reverse phase liquid chromatographic method for the separation and quantitation of the H2-receptor antagonist drug cimetidine in human whole blood and plasma is described. The method involves a single step organic extraction of the drug from alkalinized biological samples followed by a salting-out of the organic solvent by an appropriate salt. A short column packed with polymeric reverse phase particles was used with an isocratic elution of 20mM potassium phosphate (pH = 9.5) and acetonitrile (87.5 + 12.5). The cimetidine was monitored at 210 nm and 0.10-0.005 absorbance unit full scale (AUFS). The relative standard deviation I %) for analysis was reproducible within 1 day and that for day-to-day analysis was 5 (n = 8) or lower
Combined Extraction-Cleanup Column Chromatographic Procedure for Determination of
Dicofol in Avian Eggs
Authors: Krynitsky Alexander J , Stafford Charles J , Wiemeyer Stanley N 
Published: February 2020

Abstract
Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl etherhexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/ mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues
Characterization of Benzyl Isothiocyanate and Phenyl Acetonitrile from Papayas by
Mass Spectrometry
Authors: Cairns Thomas , Siegmund Emil G , Stamp John J , Jacobs Richard M 
Published: February 2020

Abstract
Two unidentified analytical responses in a papaya extract were structurally determined by mass spectrometry to be benzyl isothiocyanate and phenyl acetonitrile. Both these compounds have previously been shown to result from degradation of benzylglucosinokte that occurs naturally in the seeds of the fruit. Characterization by mass spectrometry has now provided a convenient mechanism to detect both these degradation compounds in extracts resulting from routine pesticide residue analysis
Review of the Decontamination of Aflatoxins by Ammoniation: Current Status and Regulation
Authors: ParK Douglas L , Lee Louise S , Price Ralph L , Pohland Albert E 
Published: February 2020

Abstract
Ammoniation of corn, peanuts, cottonseed, and meals to alter the toxic and carcinogenic effects of aflatoxin contamination has been the subject of intense research effort by scientists in various government agencies and universities, both in the United States and abroad. Results of these studies have been well documented over the last 20 years. Engineers have devised workable systems of treatment of whole seeds, kernels, or meals; chemists have identified and characterized products formed from the reaction of aflatoxin B, with ammonia with and without a meal matrix; biochemists have studied the biological effects of these compounds in model systems; and nutritionists have studied animal responses to rations containing ammoniated or nonammoniated components. This review describes these studies. Results demonstrate overwhelming support for the efficacy and safety of ammoniation as a practical solution to aflatoxin detoxification in animal feeds.
Liquid Chromatographic Method for Determination of Citreoviridin in Corn and Rice
Authors: Stubblefield Robert D , Greer Judith I , Shotwell Odette L 
Published: February 2020

Abstract
Citreoviridin, a neurotoxic mycotoxin, has been found as a natural contaminant in corn left unharvested in the southeastern United States and in rice of several Asian countries, including Japan. A reliable analytical method for the quantitative determination of citreoviridin in corn and rice is described. Corn or rice is extracted with dichloromethane, and the extract is partially purified on silica and amino solid-phase extraction (SPE) columns. The extract is analyzed for citreoviridin by normal-phase liquid chromatography, using a mobile phase of ethyl acetate-hexane (75 + 25) at 1.5 mL/min and a fluorescence detector to measure the yellow fluorescence (388 nm excitation, 480 nm emission). With a 100 nL injection loop, the relationship between concentration and injection volume is linear for 20- 60 itL injections. Recoveries of citreoviridin added to yellow corn at 10-50 ng/g were 91.0-96.9%; recoveries from white corn (10-50 ng/g added) were 96.8-102.8%. Recoveries of 5000 ng/g added to white corn were 89.0%, indicating that heavily contaminated samples can be assayed by the method. Minimum detection limits were 10 ng for citreoviridin standard and 2 ng/g for citreoviridin added to corn. White rice fermented with Penicillium citreo-viride (1524 ppm) was mixed with and serially diluted with uncontaminated ground corn to obtain citreoviridin-contaminated corn (ca 25 ppb). When the samples were assayed by the method, a mean level of 24.4 ± 1.65 ppb (6.5% coefficient of variation) was obtained. Four fermented rice food samples and 3 commercial rice samples were investigated. Analyses of a fermented red rice and a fermented wild rice gave unsatisfactory results because impurities in partially purified extracts interfered with LC analysis. Extracts of most rice samples did not require cleanup by the SPE columns to remove interfering LC peaks.
β-Cyclodextrin Post-Column Fluorescence Enhancement of Aflatoxins for Reverse-Phase
Liquid Chromatographic Determination in Corn
Authors: Francis Octave J , Kirschenheuter Gary P , Ware George M , Carman Allen S , Kuan Shia S 
Published: February 2020

Abstract
β-Cyclodextrin enhances the fluorescence of aflatoxins B1 and G1 in aqueous systems. This effect was utilized in developing a unique reverse-phase liquid chromatographic (LC) method for determination of aflatoxins B1, B2, G1,and G2 (B1 detection limit 1 ppb), without preparing derivatives of B1 and G1. The aflatoxins are dissolved in methanol or the mobile phase for injection onto the LC system. Using a mobile phase of methanoI-β-cyclodextrin (1 + l), the aflatoxins are resolved on a C18 column. Fluorescence of the aflatoxins is enhanced by post-column introduction of an aqueous concentrated 0-cyclodextrin solution. All 4 aflatoxins elute within 10 min in the order G2, G1, B2, B1. Fluorescence responses for B1 and G1 standards were linear over the concentration range 0.5-10 ng, yielding correlation coefficients (r) of 0.9989 and 1.000, respectively. The average peak response ratio for G^B, for the mobile phase-enhancement solution described was 0.765 with a coefficient of variation (CV) of 0.98%. CVs were 6.2, 9.0, and 7.5% for multiple assays of aflatoxin B1 in 3 samples of naturally contaminated corn. For samples of corn spiked to a total B1 content of 8.3 ng/g, average B1 recovery was 90% (CV 11.7%)
Gas Chromatographic Determination of Formaldehyde in Maple Syrup as 2,4-Dinitrophenylhydrazone Derivative
Authors: Baraniak Zbigniew , Nagpal Daljit S , Neidert Eli 
Published: February 2020

Abstract
A procedure is presented for the quantitative extraction and determination of formaldehyde in maple sap and syrup. The method is based on the reaction between formaldehyde and 2,4-dinitrophenylhydrazine and determination of the derivative by gas chromatography. The procedure was used to evaluate formaldehyde in saps and syrups of paraformaldehyde implanted trees. Average recoveries were 101.5 ± 5.7%. The detection limit was 0.078 mg/kg
Normal-Phase Liquid Chromatographic Determination of Menadione in Animal Feeds
Authors: Laffi Roberto , Marchetti Silvia , Marchetti Mario 
Published: February 2020

Abstract
A simple method is presented for determination of menadione in vitamin premixes and feedstuffs by normal-phase liquid chromatography (LC). Vitamin K3 is extracted and converted to free menadione, which can be determined directly by LC analysis. Peak area or height is measured at 251 nm, and menadione is quantitated by comparison with the working standard. Menadione can be estimated with a detection limit of 2.5 ppm. Recoveries for premixes ranged from 97.3 to 98.3% and for feedstuffs from 93.7 to 96.8%. The method allows the assay of all commercial K3 compounds in pure or stabilized form and is applicable to a wide variety of feeds and premixes.
Comments on AOAC Dry Ash Method for Digestion of Mineral-Mix Feeds
Authors: Latimer George W , Ilger Wayne , Hinojosa Heron , Roth Marta 
Published: February 2020

Abstract
Phosphorus in feeds or mineral mixes containing monobasic calcium phosphate cannot be determined accurately if the sample is subjected to the dry ash procedure described in AOAC method 7.125-7.128. HCl-insoluble calcium metaphosphates are formed at the high temperature required for ashing.
Interference by Tin in AOAC Dry-Ash Voltammetric Method for Determination of Lead and
Cadmium in Canned Foods
Authors: Holak Walter , Specchio John J 
Published: February 2020

Abstract
When lead and cadmium were determined in samples of canned food by the AOAC anodic stripping voltammetric method, an interference was observed which was believed to be tin(IV). This interference could cause false positive results for lead and cadmium. The electroactivity of tin(IV) was suppressed by increasing the concentration of tartaric acid in the supporting electrolyte from 0.005M to 0.1M after mixing with an equal volume of sample solution.
Determination of Insoluble, Soluble, and Total Dietary Fiber in Foods and
Food Products: Interlaboratory Study
Authors: Prosky Leon , Asp Nils-Georg , Schweizer Thomas F , Devries Jonathan W , Furda Ivan 
Published: February 2020

Abstract
A collaborative study was conducted to determine the insoluble dietary fiber (IDF), soluble dietary fiber (SDF), and total dietary fiber (TDF) content of food and food products by using a combination of enzymatic and gravimetric procedures. The method was basically the same as that developed for TDF only, which was adopted official final action by AOAC, except for changing the concentration of buffer and base and substituting hydrochloric acid for phosphoric acid. These changes were made to improve the robustness of the method. Duplicate blind samples of soy isolate, white wheat flour, rye bread, potatoes, rice, corn bran, oats, Fabulous Fiber, wheat bran, and a high fiber cereal were analyzed by 13 collaborators. Dietary fiber values (IDF, SDF, and TDF) were calculated as the weight of residue minus the weight of protein and ash. The coefficients of variation (CVs) of both the independent TDF determination and the sum of IDF and SDF were better than 15 and 18%, respectively, with the exception of rice and soy isolate. These 2 foods, however, contained only about 1% TDF. The CVs of the IDF were equally good, except for Fabulous Fiber, for which filtration problems occurred. The CVs for the SDF were somewhat high, but these products had very low SDF content. There was excellent agreement between the TDF determined independently and the TDF determined by summing the IDF and SDF. The method for separate determination of IDF and SDF requires further study. The modifications (changes in concentration of buffer and base and the use of hydrochloric acid instead of phosphoric acid) to the official final action method for TDF have been adopted.
Selective Membrane Electrode Potentiometry and Spectrophotometry of a Photochemical
Reaction of Thioredazine Hydrochloride
Authors: Shoukry Adel F , Badawy Sayed S 
Published: February 2020

Abstract
A PVC membrane electrode of the coated wire type was prepared which is selective for thioredazine. It showed a Nernstian response over a thioredazine concentration range 6.3 x 10 «to 2.5 x 10_3M, at 25°C, and was selective, precise, and usable within the pH range 2.1-7.0. The standard electrode potentials, E°, were determined at different temperatures and used to calculate the isothermal temperature coefficient of the electrode. The photoreaction occurring in thioredazine solution exposed to daylight did not affect the electrode performance. This reaction was investigated kinetically to determine its rate constant and half-life at different temperatures.
Determination of Nitrogen Content in Milk by the Kjeldahl Method Using Copper Sulfate: Interlaboratory Study
Authors: Grappin R , Horwitz William 
Published: February 2020

Abstract
Copper sulfate was substituted for mercury as the catalyst in the International Dairy Federation (IDF) Standard 20A:1986 method for the determination of nitrogen content in milk. The substitution was supported by results obtained in an interlaboratory study by 24 laboratories in 12 countries. Each laboratory analyzed 12 test samples of milk as blind duplicates in a double split level design with high, medium, and low nitrogen concentrations. The method protocol requires the concurrent analyses of an ammonium salt solution and a tryptophan solution as internal quality control standards with a minimum nitrogen recovery between 99 and 100% for the former and at least 98% for the latter. The repeatability and reproducibility relative standard deviations are 0.5 and 1%, respectively, for the range 0.35-0.70 g N/100 g. The performance of the laboratories that did not meet the required quality control specifications was clearly poorer than that of those that did meet the specifications.
Determination of Sulfite in Foods by Headspace Liquid Chromatography
Authors: Lawrence James F , Chadha Rajinder K 
Published: February 2020

Abstract
Sulfite was determined in a variety of foods by liquid chromatography (LC) after the samples were mixed with a solution containing mannitol, FeS04, and Na2HP04, adjusted to pH 11, and left to stand for 15 min at room temperature. An aliquot of the mixture was placed in a headspace vial and mixed with 50% H3P04. After 15 min, a portion of the headspace was removed with a syringe containing LC mobile phase without acetonitrile. The syringe was shaken and an aliquot of the solution was analyzed on an anion exchange column with a mobile phase of 0.03M methane sulfonate (pH 10.8) containing 5% acetonitrile. Sulfite was detected amperometrically (glassy carbon electrode) at +0.7 V. The method was successfully compared to the FDA-modified Monier-Williams procedure for a variety of foods. Minimum detectable levels were about 1 ng/g, based on a 15 g sample
Fluorometric Determination of Benzylideneacetone in Fragrance Products by Liquid Chromatography with Post-Column Derivatization
Authors: Yates Ronald L , Wenninger John A 
Published: February 2020

Abstract
A method is described for the liquid chromatographic (LC)-fluorometric determination of benzylideneacetone in fragrance products. Benzylideneacetone is first separated from other fragrance ingredients by LC and then reacted post-column with a methanolic solution of isonicotinic acid hydrazide and aluminum nitrate. The reactants are maintained at 65°C for about 1.5 min to quantitatively form the fluorescent isonicotinoyl hydrazone derivative of benzylideneacetone. The aluminum ion forms a complex with the hydrazone to enhance the fluorescence of the derivative. The amount of benzylideneacetone is determined by measuring the intensity of the fluorescence emitted by the hydrazone derivative and comparing that value with those obtained for derivatized standards. Recovery studies were conducted by spiking commercial fragrances with benzylideneacetone at concentrations of 0.01,0.05, and 0.1% (w/v). Recoveries ranged from 98 to 104% with a mean recovery of 100.2% and a standard deviation of 2.4%.
Visual Immunoassay for Detection of Salmonella in Foods: Collaborative Study
Authors: Flowers Russell S , Klatt Mary Joan , Keelan Susan L 
Published: February 2020

Abstract
A collaborative study was performed in 13 laboratories to validate a visual enzyme immunoassay (EIA) procedure, TECRA®, for rapid detection of Salmonella in foods. The EIA method was compared with the standard culture procedure for detection of Salmonella in 6 food types: ground black pepper, soy flour, dried whole eggs, milk chocolate, nonfat dry milk, and raw deboned turkey. Uninoculated and inoculated samples were included in each food group analyzed. There was no significant difference in the productivity of the EIA and culture procedures at the 5% level for any of the 6 foods. The enzyme immunoassay screening method has been approved interim official first action.