bluuebunny/crossref_metadata_2025_split huggingface dataset:
Determination of Gentian Violet, Its Demethylated Metabolites, and Leucogentian Violet in Chicken Tissue by Liquid Chromatography with Electrochemical Detection
Authors: Roybal Jose E , Munns Robert K , Hurlbut Jeffrey A , Shimoda Wilbert 
Published: February 2020

Abstract
A method Is presented for determination of residues of gentian violet (GV), Its demethylated metabolites (pentamethyl and tetramethyl), and leucogentian violet (LGV) In chicken tissue. The analytes are extracted from tissue with acetonitrlle/ buffer and partitioned Into methylene chloride. Polar lipids are removed on an alumina column followed by partitioning Into methylene chloride from a citrate buffer. The compounds of interest are isolated on a disposable carboxyl- Ic acid cation exchange column and then eluted with 0.02% HCI In methanol. GV, Its metabolites, and LGV are determined by liquid chromatography using Isocratlc elution with a buffered mobile phase from a cyano column and amperometrlc electrochemical detection at +1.000 V. Average recoveries of GV and LGV from commercially purchased chicken liver fortified with 20 ppb of each compound were 92% [standard deviation (SD) = 7, coefficient of variation (CV) = 7.6%] and 86% (SD = 7, CV = 8.1 %), respectively. Average recoveries of GV, LGV, the pentamethyl metabolite, and 1 of the tetramethyl metabolites from control chicken liver (provided by the Center for Veterinary Medicine) fortified with 20 ppb of each compound were 80% (SD = 7, CV = 8.8%), 76% (SD = 3, CV = 3.9%), 83% (SD = 6, CV = 7.2%), and 76% (SD = 8, CV = 10.5%), respectively. Mean results from 10 analyses of residue-Incurred chicken liver were 31 ppb GV (SD = 3, CV = 9.7%), 34 ppb pentamethyl metabolite (SD = 3, CV = 8.8%), and 40 ppb tetramethyl metabollte(s) (SD = 2, CV = 5.0%), for an average value of 105 ppb total residues (SD = 6, CV = 5.7%); no LGV was found. Data are also presented to show applicability of the method to muscle tissue.
Liquid Chromatographic Determination Of Three Sulfonamides In Animal Tissue And Egg
Authors: Horii Shozo , Momma Chie , Miyahara Kayoko , Maruyama Tsutomu , Matsumoto Masao 
Published: February 2020

Abstract
Sulfonamides are widely used as a feed additive in animal production In Japan. The present paper is a determination of 3 sulfonamides: sulfamethazine (SMZ), sulfamonomethoxlne [SMX, 4-amino-/V-(3-methoxypyrazlnyl)-benzenesulfonamlde], and suifadimethoxine (SDX) in animal tissue and egg by liquid chromatography (LC). Tissues were extracted with acetonltrlle and fat was removed by liquid/liquid partition. The sulfonamides were purified by an ODS cartridge column; then each compound was separated by an ODS LC column and detected at 268 nm. Quantification levels were 0.02 ppm for SMZ and SMX, and 0.04 ppm for SDX; detection limits were 0.01 ppm for SMZ and SMX, and 0.02 ppm for SDX. Calibration curves were linear between 2 and 40 ng for SMZ and SMX, and between 4 and 80 ng for SDX. Recoveries from muscle and egg samples spiked with 1-2 /μg/10 g were 8 1 - 98%.
A Single Cell Protein as Standard Reference Material for Determination of Amino Acids, Fatty Acids, and Elements in Foods
Authors: Aziz Abdul , Abu-Dagga Faisal 
Published: February 2020

Abstract
A commercially available single-cell protein (Pruteen) was analyzed for amino acids, fatty acids, and major, minor, and trace-element composition after storage at room temperature and at 4°C over a period of 5 years. The purpose was to assess its suitability as an organic-nutrient standard reference material for food analysis. The material showed longterm stability and is, therefore, recommended for interlaboratory certification studies.
Multiresidue Assay for Benzimidazole Anthelmintics by Liquid Chromatography and Confirmation by Gas Chromatography/Selected-Ion Monitoring Electron Impact Mass Spectrometry
Authors: Wilson Roger T , Groneck Joseph M , Henry Carolyn A , Rowe Loyd D 
Published: February 2020

Abstract
A multiresidue method utilizing all-disposable labware has been developed for 8 benzimidazole anthelmintics from ovine, bovine, and swine muscle and liver tissues. After an Initial extraction with ethyl acetate and subsequent evaporation, a 3-component extraction using hexane, ethanol, and 0.2N HCI was used for final cleanup. Clean extracts were produced for separation and determination by reverse-phase liquid chromatography at 298 nm, using methanol and aqueous buffer as mobile phase. A synthesized internal standard, 2-(n-butylmercapto)benzlmldazole, was used for quantitation of all drugs. Results are Included along with statistical information verifying the performance of the method. Spiked control tissues and Incurred drug tissues were used for an Intralaboratory study with a concentration range of 50-1470 ppb. A series of standard curves at 0, 50, 100, and 200 ppb were analyzed. Overall recovery at the 100 ppb level averaged 92% (CV 8%) In liver tissues, across all 3 species and 88% (CV 5%) in muscle tissues across all 3 species. Results were confirmed by gas chromatography/mass spectrometry with acid hydrolysis of the remaining extract In 2N HCI followed by re-extractlon of the amine and derivatlzation to the ferf-butyldimethylsilyl derivative. The anthelmintics were Identified by gas chromatography/selected ion monitoring electron-Impact mass spectrometry. Ion ratio measurements were taken and compared to standard material. CVs averaged 10% or less for all drugs tested.
Gas Chromatographic Determination and Pattern Recognition Analysis of Methanol and Fusel Oil Concentrations in Whiskeys
Authors: Wilson Linda A , Ding Jia H , Woods A Edwin 
Published: February 2020

Abstract
A more efficient determination of methanol and fusel oil in 4 types of whiskeys was accomplished using gas chromatography and temperature programming. Carbopack C with 0.2% Carbowax 1500 (Supelco, Inc., Bellefonte, PA) produced baseline separation of 13 aliphatic alcohols containing 5 carbons or less. A comparison of methanol and fusel oil concentrations between various types of whiskeys Indicates that bourbon and sour mash whiskeys contain considerably more fusel oil (275 ± 1 2 and 265 ± 5 mg/100 mL, respectively) than blended and scotch whiskeys (47 ± 5 and 114 ± 7 mg/100 mL, respectively). All concentrations were corrected to 100 proof. A statistical pattern recognition analysis of the data showed that fusel oil components (1-propanol, 2- methyl-1-propanol, 2-methyl-1-butanol, and 3-methyl-1-butanol) and methanol could be used to distinguish between bourbon-sour mash, blended, and scotch whiskeys. Bourbon and sour mash whiskeys were indistinguishable by fusel ollmethanol analysis. A significant increase in methanol content occurred In bourbon and sour mash whiskeys after bottles were opened and reseaied for up to 58 months; fusel oil content remained essentially unchanged.
Moisture Analysis in Forage by Near-Infrared Reflectance Spectroscopy: Collaborative Study of Calibration Methodology
Authors: Windham William R , Barton Franklin E 
Published: February 2020

Abstract
Fifteen collaborating laboratories analyzed 16 forage samples including 3 blind duplicate pairs for moisture by air-oven (AO) method 7.007 (14th Ed.; 930.15, 15th Ed.) and nearinfrared reflectance spectroscopy (NIRS). Laboratories performed method 7.007 on 50 calibration samples and applied the NIRS calibration method Independently. NIRS moisture equations were used to predict the 16 test samples, and the values were compared to those for method 7.007. Moisture concentration of the test samples ranged from approximately 6 to 16%. Within-laboratory repeatability (sr) ranged from 0.10 to 0.18% and 0.16 to 0.39% for NIRS and method 7.007, respectively. Between-laboratory reproducibility (sR) ranged from 0.22 to 0.57 and 0.29 to 0.57 for NIRS and method 7.007, respectively. Repeatability relative standard deviations (RSDr) for the NIRS and AO methods ranged from 1.18 to 1.50% and 1.84 to 3.68%, respectively. The range in the average reproducibility relative standard deviations (RSDR) for the NIRS and AO methods were 1.29-7.49% and 3.64-6.66%, respectively. The NIRS method demonstrated consistently lower wlthln-laboratory RSDr agreement and between-laboratory variabilities equal to method 7.007. Thereby, we demonstrated that NIRS can be used as a standard method for the determination of 6-16% moisture In forages. The method has been adopted official first action by A0AC.
Determination of Benzene in Polypropylene Food-Packaging Materials and Food-Contact Paraffin Waxes
Authors: Varner Sandra L , Hollifield Henry C , Andrzejewski Denis 
Published: February 2020

Abstract
An analytical procedure was developed for determination of benzene in polypropylene food packaging and was adapted for determination of benzene in commercial paraffin waxes Intended for food-contact use. The polymer was dissolved in hexadecane at 150°C. The wax was melted in an 80°C oven. A simple helium-sparging apparatus was used to remove the volatile chemical from the polymer or wax. The contaminant was collected In methanol, distilled water was added, and the resulting solution was analyzed by headspace gas chromatography. The Instrument was equipped with a 30 m fused silica open tubular capillary column and a photoionization detector. Average recoveries of benzene from polymer and paraffin wax at low parts-per-billion concentrations were 63 and 70%, respectively. Limits of detection and quantitation for analysis of polypropylene were 8 and 17 ppb, respectively; the limit of quantitation for analysis of paraffin wax was 2 ppb. in several commercial polypropylene products examined, benzene levels ranged from none detected to 426 ppb. In 3 commercial waxes examined, concentrations of 16-73 ppb benzene were determined. The presence of benzene was confirmed by gas chromatography/mass spectrometry
Gas Chromatographic Method for Determination of Dimethylamine, Trimethylamine, and Trimethylamine Oxide in Fish-Meat Frankfurters
Authors: Fiddler Walter , Doerr Robert C , Gates Robert A 
Published: February 2020

Abstract
A method Is described for analysis of minced fish-meat and surlmi-meat frankfurters for dimethylamine (DMA), trimethyiamine (TMA), and trimethyiamine oxide (TMAO) using a headspace-gas chromatographic technique. After simple acid extraction and addition of NaOH, the headspace was directly Injected Into a gas chromatograph by a gas-tight syringe. DMA and TMA were separated on a Chromosorb 103 column and detected by a flame Ionization detector. TMAO was measured as TMA after Zn reduction. Repeatability of the method for DMA, TMA, and TMAO was 6.6,1.0, and 18.8 ppm, respectively. The method was applicable to Alaska pollock-meat and Atlantic menhaden-meat frankfurters, unwashed, and washed mince and surlml.
Liquid Chromatographic Method for Selegiline Hydrochloride and Related Compounds in Raw Materials and Tablets
Authors: Beaulieu Normand , Cyr Terry D , Graham Susan J , Lovering Edward G 
Published: February 2020

Abstract
A liquid chromatographic method has been developed for determination of selegiline hydrochloride and related substances in drug raw material and tablet formulations. The method resolves 3 known related compounds from the drug with a limit of quantitation of less than 0.05%. Drug raw material and tablet samples contained ca 0.2 and 0.6% impurities, respectively. These included some related compounds, the identities of which were confirmed by gas chromatography with a Fourier transform Infrared detector.
Turbidimetric Assay for Tetracyclines in Feeds Using a Microtiter Plate System
Authors: Brady Marietta Sue , Katz Stanley E 
Published: February 2020

Abstract
The microtiter plate system for turbidimetric assay of chlortetracycline (CTC) and oxytetracycline (OTC) levels in feeds uses a 96 well microtiter plate, a multichannel pipette, and an ELISA reader to measure turbidity. Feeds are extracted for both tetracyclines using AOAC extraction systems. For CTC, the range of the standard curve is 0.001-0.005 μg CTC/ mL; for OTC, the range is 0.004-0.016 μg OTC/mL. Repeatability of CTC assays, as shown by the coefficient of variation (CV), ranged from 0.54 to 5.65% for same-day assays and from 2.01 to 9.39% for assays on different days. For OTC, CVs ranged from 2.69 to 10.01% for same-day assays and 3.24 to 9.08 % for different-day assays. Average recoveries for CTC were 108.7% for same-day assays and 106.8% for different-day assays; for OTC, average recoveries were 112.4% and 106.5% for same-day and different-day assays, respectively.
Defined Substrate Technology Method for Rapid and Specific Simultaneous Enumerationof Total Coliforms and Escherichia coli from Water: Collaborative Study
Authors: Edberg Stephen C , Allen Martin J , Smith Darrell B 
Published: February 2020

Abstract
The defined substrate technology (DST) method Is a reagent system designed to enumerate specific target microbes(s) from a mixture of bacteria. The system simultaneously enumerates total coliforms and Escherichia coll directly from a water sample. The reagent contains o-nitrophenyl-β-D-galactopyranoside (ONPG), which is hydrolyzed by total conforms to produce a yellow chromogen, and 4-methylumbelllferyl-β-D-glucuronide (MUG), which is hydrolyzed and fluoresces when E. coll organisms grow. Noncoliform bacteria are suppressed and cannot metabolize the indicator nutrients. Nine laboratories participated in a field evaluation of the method, which covered a wide range of surface and subsurface water sources and water-processing modalities, including the examination of natural samples. The DST system was compared to multiple-tube fermentation (MTF) (quantitative) and presence-absence (P-A) (qualitative) Standard Methods formats. Comparison of water samples from natural sources by using the most probable number (MPN) procedure showed that the DST test was equivalent to the currently used MTF test. Results from the DST and the qualitative P-A procedure showed that these tests agreed with each other in 94% of the water samples analyzed. Specificity of the DST method was established by subculturing a species consistent with a total conform or E. coll from each positive tube. Eight laboratories participated in a collaborative study of the method. Each laboratory received 3 concentrations of E. coll (organisms/100 mL): 10 (low); 60 (medium); and 120 (high). The DST test was inoculated from a split sample of each bacterial density In parallel with Standard Methods brilliant green lactose broth. Statistical analyses for repeatability and reproducibility showed the DST system to be equivalent to currently used standard methods. The DST method has been adopted official first action by AOAC for detection and enumeration of total coliforms and E. coll in water.
Evidence of an Unusual Pattern of Polychlorinated Biphenyls in the Serum of Some Residents and Canines in Paoli, Pennsylvania
Authors: Burse Virlyn W , Groce Donald F , Korver Margaret P , Caudill Samuel P , McClure Patricia C , Lapeza Chester R , Head Susan L , Schilling Rebecca J , Farrar Jeffrey A , Ostrowski Stephanie R , Mortensen B Kim , Maher John P , Russell Harold L , Sievila Sara 
Published: February 2020

Abstract
The present study uses gas liquid chromatography (GLC) electron capture detection with packed and capillary columns to detect polychlorinated biphenyls (PCBs) in serum samples from people living near the electric car repair and maintenance facility of the Southeastern Pennsylvania Transit Authority in Paoli, Pennsylvania. Most of the cohort surveyed had serum patterns similar to patterns for Aroclor 1260 (AR 1260); a small portion (3/69) had patterns Indicative of an AR with higher chlorlnation (e.g., AR 1268). In addition to analyzing serum samples from humans, we also analyzed serum samples from canines (pets of some of the subjects). In general, the serum pattern for canines was less descriptive for AR 1260 than the pattern for humans; however, the pattern for several canines (9/16) was that of the higher chlorinated PCBs (e.g., AR 1268). By using mass spectrometry and capillary column GLC, we confirmed the presence of high molecular weight polychlorinated congeners in both human and animal samples. We were not able to show a statistically significant relationship between serum patterns of PCBs In canines and their owners or between canines and certain behavioral traits (e.g., runs free, retrieves, hours outside, hours Inside). However, the correlation between PCBs quantified as AR 1268 and canines' residence time was statistically significant.
Liquid Chromatographic Determination of Tolnaftate in Commercial Products
Authors: Thompson Richard D , Carlson Marvin 
Published: February 2020

Abstract
A liquid chromatographic (LC) method for the determination of the antifungal agent tolnaftate was developed. Isolation of the analyte was achieved by direct extraction or dilution with acetonltrlle-water (80 + 20) followed by reverse-phase liquid chromatography using a C18 column. The mobile phase was acetonltrlle-water (80 + 20) acidified with phosphoric acid. Detection was by UV absorption at a wavelength of 257 nm. The proposed procedure was applied to 20 consumer products comprising 6 formulation types, including solutions, powders, liquid and powder aerosols, creams, and gels. The precision (RSD) for the products ranged from 0.23 to 1.16% (n = 5), and recoveries via fortification ranged from 98.1 to 103.0%. Six different brands of C18 columns were evaluated for use with the method. The overall simplicity and versatility of the method suggest possible adaptations to both regulatory and quality-control situations.
A Rapid 13C/12C Test for Determination of Corn Syrups in Honey
Authors: Brookes Steven T , Barrie Andrew , Davies Jonathan E 
Published: February 2020

Abstract
The AOAC official method for detection of corn syrup products in honey measures the 13C/12C ratio (δ13C) (978.17). In the official method, a suspect honey is combusted off-line to C02 gas for analysis on a dual-inlet isotope ratio mass spectrometer (IRMS). The procedure is manual, requires liquid N2, and takes 20-50 min/sample. In the present study, we examine a recently developed alternative, automated 15N 13C analysis mass spectrometry (ANCA-MS). This procedure combusts and analyzes 66 samples in a batch and takes only 5 min/sample. We used both ANCA-MS and IRMS with offline combustion to analyze 6 honeys containing from 0 to 100% high fructose corn syrup (HFCS). δ13C values by both methods agreed within 0.2%o and gave an excellent straight line fit (slope = 0.991; R = 1). As an alternative to IRMS, ANCA-MS is automated and provides a 5-fold increase in sample throughput.
Multiresidue Matrix Solid Phase Dispersion (MSPD) Extraction and Gas Chromatographic Screening of Nine Chlorinated Pesticides in Catfish (Ictalurus punctatus) Muscle Tissue
Authors: Long Austin R , Crouch Michael D , Barker Steven A 
Published: February 2020

Abstract
A multiresidue technique for extraction and gas chromatographic screening of 9 insecticide (lindane, heptachlor, aldrin, heptachlor epoxide, p,p-DDE, dieldrin, endrin, p,p- TDE, and p,p'-DDT) residues In catfish {Ictalurus punctatus) muscle tissue is presented. The 9 Insecticides, plus dibutyl chlorendate internal standard, were fortified into catfish muscle tissue (0.5 g) and blended with 2 g C18 (octadecylsilyl derlvatized silica reverse-phase material). The C18/muscle tissue matrix blend was fashioned into a column by adding the blend to a 10 mL syringe barrel containing 2 g activated Florisil. The insecticides were then eluted from the column with acetonitrlle (8 mL), and a portion (2 μL) of the acetonitrile eluate was then directly analyzed by gas chromatography with electron capture detection. Unfortified blank controls were treated similarly. The resultant extracts contained pesticide analytes (31.25-500 ng/g) free of interfering compounds when analyzed. Correlation coefficients for the 9 extracted pesticide standard curves (linear regression analysis, n = 5) ranged from 0.9967 (± 0.0018) to 0.9999 (± 0.0001). Average percentage recoveries (82 ± 4.8% to 97 ± 3.6%, n = 25 for each Insecticide), Interassay (5.0 ± 2.7% to 16.9 ± 6.5%, n = 25 for each insecticide) and intraassay (1.8 to 4.7%, n = 5 for each Insecticide) variabilities were Indicative of an acceptable methodology for the analysis and screening of these residues in catfish muscle tissue.
Rapid Pentachlorophenol Evaluation in Solid Matrixes by Second Derivative UV Spectroscopy for Application to Wood and Leather Samples
Authors: Secchieri Monica , Benassi Carlo A , Pastore Saveria , Semenzato Alessandra , Bettero Antonio , Levorato Marco , Guerrato Alfredo 
Published: February 2020

Abstract
A method for the quali-quantltatlve evaluation of pentachlorophenol (PCP) in solid matrixes has been developed. The procedure Is based on solid-liquid extraction of solid samples (leather or wood), followed by purification on a cyanopropyl column and determination of the preservative by second derivative UV spectroscopy considering the PCP A peakthrough value (304-297 nm). The method allows rapid PCP determination In the concentration range 1-40 μg/mL; any matrix interference is avoided by the purification step and recoveries of the preservative were 99.12% (RSD% 0.13) for the leather matrix and 98.03 (RSD% 0.17) for the wood matrix.
Crude Oil Content of Selected Oilseeds and Flours: A Comparison of Solvents
Authors: Granata Gary , Lane Ralph H 
Published: February 2020

Abstract
A variety of wheat flours and ground oilseeds was subjected to continuous extraction for 6 h with each of 4 solvents (anhydrous diethyl ether, hexane, pentane, and petroleum ether). Hexane and diethyl ether were equally superior (P &lt; 0.05) to the other 2 solvents In extracting crude oil from all-purpose flour and from ground peanuts, soybeans, cottonseeds, and canola seeds. Hexane yielded higher crude oil values (P &lt; 0.05) than the other solvents in the case of ground safflower and sunflower seeds. Diethyl ether produced higher values (P &lt; 0.05) from ground corn germ and bread flour. No differences (P &lt; 0.05) were found among solvents when extracting whole wheat flour.
Performance Characteristics of Methods of Analysis Used for Regulatory Purposes.Part II. Pesticide Formulations
Authors: Horwttz William , Albert Richard 
Published: February 2020

Abstract
The precision parameters of the method-performance (collaborative) studies published In the AOAC Journal from 1915 through 1990 for pesticide formulations have been recalculated on a uniform basis by the International Union of Pure and Applied Chemistry 1987 protocol. About 93% of the 953 accepted assays, which are predominantly gravimetric (G), volumetric (V), and gas (GC) and liquid (LC) chromatographic methods, exhibit relative standard deviations among laboratories (RSDR) that are generally less than 2 times the values predicted from the Horwitz equation: RSDR (%) = 2 exp (1 - 0.5 log C), where C is the concentration expressed as a decimal fraction. UV, VIS, and IR spectrophotometrlc (S) methods are somewhat poorer, with about 80% of the reported RSDR values less than twice the predicted RSDR value. The precision parameters of pesticide formulations analyzed by the older methods (G, V, GC) are equivalent to those previously found for drug preparations in the same concentration range; the precision parameters of pesticide formulations analyzed by LC and S are somewhat poorer. Overall, however, the precision parameters of pesticide formulations are generally independent of analyte, method, and matrix, and are primarily a function of concentration. The method-acceptability decisions of the AOAC for pesticide formulations during the past 75 years can be approximated retrospectively by using a criterion for RSDR that is less than 2 times the RSDR calculated from the Horwitz equation.