bluuebunny/crossref_metadata_2025_split huggingface dataset:
Identification of O,O-Dialkyl-S-MethyIpnosphorodithioate Residues in Fish
Authors: Yurawecz Martin P , Puma Bart J 
Published: February 2020

Abstract
O,O-Dialkyl-S-methylphosphorodithioates were found in Mississippi River buffalo fish caught near several chemical plants and oil refineries in Hartford and Wood River, IL. These chemicals, which have not been previously recognized as environmental or food contaminants, were identified and quantitated by a procedure similar to the AOAC multiresidue method for organochlorine and organophosphorus pesticides, using gas chromatography (GC) with flame photometric detection (FPD). The key to their identification was a GC/FPD retention time pattern that was virtually the same as that for the diazomethane reaction products of a commercial zinc dialkyl dithiophosphate motor oil additive. GC/mass spectrometry (MS) showed that the compound producing the largest GC/FPD peak contained butoxy groups. The identification of this compound as O,O-di(2-methyIpropyl)-S-methyIphosphorodithioate (Compound C) was confirmed by GC/MS analysis by comparison with the authentic material. The buffalo fish contained 0.15 ppm Compound C and 0.5 ppm total O,O-dialkyl-S-methyIphosphorodithioates. Subsequent analyses of fish from other areas showed that these contaminants were not limited to the Hartford-Wood River area. Lower residue levels of Compound C, ranging from 0.01 to 0.05 ppm, were found in fish from the Mississippi River at Sauget, IL, and from the Delaware River and Newark Bay in NJ.
Harmonization of Collaborative Study Protocols
Authors: Horwitz William 
Published: February 2020

Abstract
The 2 major protocols for the design, conduct, and interpretation of collaborative analytical studies—those from AOAC and the International Organization for Standardization—are already fairly well harmonized. The statistical models are identical and the outlier tests are essentially the same. The major differences are in symbols and terminology and in the specification of the minimum number of laboratories and replicates.
View of the International Dairy Federation on Interlaboratory Analytical Studies
Authors: Grappin R 
Published: February 2020

Abstract
The International Dairy Federation develops and studies methods for the analysis of milk and milk products. A first draft of an IDF protocol for conducting interlaboratory studies is presented. Major features of the protocol are type and number of participating laboratories; nature, duplication, and number of sample materials; final design (numbers of samples and laboratories); statistical analysis of the data; report of the final results.
Design and Conduct of Collaborative Studies: CIPAC Collaborative Experience in Pesticide Formulations
Authors: Henriet J , Martijn A 
Published: February 2020

Abstract
CIPAC has set up procedures for carrying out interlaboratory studies on analysis of technical pesticide materials and formulations. CIPAC studies comprise several steps: allocation of leadership; method survey and selection; pre-collaborative trial; full collaborative study; evaluation of results and final decision on acceptance.
Liquid Chromatographic Determination of Monensin in Chicken Tissues with Fluorometric Detection and Confirmation by Gas Chromatography-Mass Spectrometry
Authors: Takatsuki Keigo , Suzuki Shigeru , Ushizawa Isamu 
Published: February 2020

Abstract
An accurate, sensitive method is described for the determination of monensin residue in chicken tissues by liquid chromatography (LC), in which monensin is derivatized with a fluorescent labeling reagent, 9-anthryldiazomethane (ADAM), to enable fluorometric detection. Samples are extracted with methanol-water (8 + 2), the extract is partitioned between CHCl3 and water, and the CHC13 layer is cleaned up by silica gel column chromatography. Free monensin, obtained by treatment with phosphate buffer solution (pH 3) at 0°C, is derivatized with ADAM and passed through a disposable silica cartridge. Monensin-ADAM is identified and quantitated by normal phase LC using fluorometric detection. The detection limit is 1 ppb in chicken tissues. Recoveries were 77.6 ± 1.8% at 1 ppm, 56.7 ± 7.1% at 100 ppb, and 46.5 ± 3.7% at 10 ppb fortification levels in chicken. Gas chromatography-mass spectrometry is capable of confirming monensin methyl ester tris trimethylsilyl ether in samples containing residues &gt;5 ppm.
Determination of Glyphosate Herbicide and (Aminomethyl)phosphonic Acid in Natural Waters by Liquid Chromatography Using Pre-Column Fluorogenic Labeling with 9-Fluorenylmethyl Chloroformate
Authors: Miles Carl J , Wallace Louis R , Moye H Anson 
Published: February 2020

Abstract
An analytical method has been developed for determination of glyphosate herbicide and its major metabolite, (aminomethyl)phosphonic acid (AMFA), in natural waters. Sample pretreatment consisted of filtration, addition of phosphate buffer, concentration by rotary evaporation, and a final filtration before derivatization with 9-fluorenylmethyl chloroformate. The derivatives were separated by anion exchange liquid chromatography and measured with a fluorescence detector. Standard curves were linear over 3 orders of magnitude and minimal detectable quantities were 10 ng/mL for glyphosate and 5 ng/mL for AMPA. The 20-fold concentration factor realized in sample preparation corresponds to ppb method detection limits for glyphosate and AMPA in natural waters. Recovery and storage studies were performed and are discussed.
Determination of Halogenated Phenols in Raw and Potable Water by Selected Ion Gas Chromatography-Mass Spectrometry
Authors: Sithole Bishop B , Williams David T , Lastoria Chester , Robertson John L 
Published: February 2020

Abstract
Pentafluorobenzylation and in situ acetylation are compared in the determination of phenol and halogenated phenols in water samples. The latter technique is considered superior to the former for determining phenols at the ng/L level because of less background interference and better recoveries (80% or better except for pentachlorophenol and trichloroguaiacol which had recoveries of about 60%). Further evaluation of the in situ technique by electron capture gas chromatography and gas chromatography-mass spectrometry shows that the latter, in the selected ion monitoring mode, is more suitable because, unlike GCECD, it can confirm and quantitate all phenols. In particular, GCECD could not detect even high levels of phenol and the monohalogenated phenols. Phenols at 5-473 ng/L were detected in some Canadian drinking water supplies by the in situ acetylation technique combined with GC-MS.
Liquid Chromatographic Determination of Leuco Base in FD&C Blue No. 1
Authors: Scher Alan L , Murray H Dean 
Published: February 2020

Abstract
Methods are described for the determination of leuco base in FD&C Blue No. 1 by reverse phase liquid chromatography and for the preparation and standardization of leuco base stock solution. The stock solution is prepared by reductive titration of the color with TiCl3. Solutions of the color and of leuco base are chromatographed by isocratic elution, which is followed by a wash and equilibration that can be omitted for screening. Peak area and height calibrations were linear. At the specification level, the 99% prediction limits were 5.00 ± 0.14% (area) and 5.00 ± 0.37% (height). Limits of determination were 0.29% (area) and 0.73% (height) at the 99.5% confidence level. Recoveries were 97-101% for leuco base added to FD&C Blue No. 1 at levels of 1-6%.
Development of Poultry Rapid Overnight Field Identification Test (PROFIT)
Authors: Cutrufelli Mark E , Mageau Richard P , Schwab Bernard , Johnston Ralph W 
Published: February 2020

Abstract
A poultry rapid overnight field identification test (PROFIT) has been developed as a screening test which is practical, economical, and easy to perform and interpret for use in field environments to determine the presence of poultry tissue (chicken and turkey) in raw whole tissue or ground/formulated meat products. The basis of the test is an agar-gel immunodiffusion technique used with a printed template pattern and stabilized reagent paper discs. The test shows adequate sensitivity and specificity for its intended purpose. Key components are stable for at least 1 year if they are stored at refrigerator conditions. The design of the test is such that it can be made commercially available as a complete, stable, test kit suitable for use by any type of inspection program concerned with verification of poultry species in meat and/or poultry products that are subject to regulatory or quality controls
Liquid Chromatographic Method for Determination of Oxythioquinox in Technical and Formulated Products: Collaborative Study
Authors: Slahck Stephen C ,   Collaborators:, Aaron L B , Bennett O O , Elliott R M , FontaniUa A O , Jurgens D , Korger P D , Laster W G , Launer J E , Law M W , Lim B M , Muniz J , Polli R L , Schulz R P , Skelly N E , Stroh S , Tengler H 
Published: February 2020

Abstract
A liquid chromatographic method for determination of oxythioquinox (Morestan®) in oxythioquinox technical and formulated products has been developed and collaboratively studied in 14 laboratories. Samples are dissolved in chloroform containing n-valerophenone as an internal standard, diluted with acetonitrile, and analyzed by reverse phase chromatography. Collaborators analyzed blind duplicate samples of oxythioquinox technical and 25 WP. Coefficients of variation were 1.06 and 1.72% for the technical and 25 WP samples, respectively. The method has been adopted official first action.
Gas Chromatographic-Thermal Energy Analysis Method for iV-Nitrosodibutylamine in Latex Infant Pacifiers: Collaborative Study
Authors: Thompson Harold C , Billedeau Stanley M , Miller Barbara J ,   Collaborators:, Clarkson S , Feit M , Hotchkiss J , Miller B , Yu W 
Published: February 2020

Abstract
Each of 5 collaborating laboratories determined volatile N-nitrosamines in 3 blind quadruplicate sets of latex rubber infant pacifier samples, using a gas chromatographic-thermal energy analysis (GCTEA) method. Volatile N-nitrosamines are extracted from cut-up pacifier nipples with CH2C12. The extract is concentrated and subjected to high temperature purge and trap, and the nitrosamines are eluted from the trap and determined by GC-TEA. N-Nitrosodibutylamine (NDBA) was the only nitrosamine found in sufficient concentration to allow analysis. NDBA concentrations of the 3 sets of samples were 82.6,21.0, and 7.12 ng/g rubber. The repeatability relative standard deviations ranged from 7.46 to 24.0% and the reproducibility relative standard deviations from 7.46 to 29.2%. The minimum detectable level of NDBA by this method is 3.6 ng/g rubber. The method has been adopted official first action.
Enumeration of Total Bacteria and Coliforms in Milk by Dry Rehydratable Film Methods: Collaborative Study
Authors: Ginn Roy E , Packard Vernal S , Fox Terrance L ,   Collaborators:, Arnold E , Barnett J , Bulthaus M , Bushman P , Case R , Crevey N , Fenelon M , Fuqua R , Gilman C , Hawkinson J , Heady J , Hendrickson H , Koenig E , Messer J , Mullen R , Phillips M , Santorello J , Slamp R , Wehr M , Zimmerman A 
Published: February 2020

Abstract
Eleven laboratories participated in a collaborative study to compare the dry rehydratable film (Petrifilm® SM and Petrifilm® VRB) methods, respectively, to the standard plate count (SPC) and violet red bile agar (VRBA) standard methods for estimation of total bacteria and coliform counts in raw and homogenized pasteurized milk. Each laboratory analyzed 16 samples (8 different samples in blind duplicate) for total count by both the SPC and Petrifilm SM methods. A second set of 16 samples was analyzed by the VRBA and Petrifilm VRB methods. The repeatability standard deviations (the square root of the between-replicates variance) of the SPC, Petrifilm SM, VRBA, and Petrifilm VRB methods were 0.0S104, 0.0444, 0.14606, and 0.13806, respectively; the reproducibility standard deviations were 0.7197, C.06380, 0.15326, and 0.13806, respectively. The difference between the mean Iog10 SPC and the mean logio Petrifilm SM results was 0.027. For the VRBA and Petrifilm VRB methods, the mean log10 difference was 0.013. These results generally indicate the suitability of the dry rehydratable film methods as alternatives to the SPC and VRBA methods for milk samples. The methods have been adopted official first action.
DNA Colony Hybridization Method Using Synthetic Oligonucleotides to Detect Enterotoxigenic Escherichia coli: Collaborative Study
Authors: Hill Walter E , Wentz Barry A , Payne William L , Jagow James A , Zon Gerald ,   Collaborators:, Boutin B K , Codor J , Crouch R J , Forney E D , Gemski P , Jagow J A , Kaper J B , Madzo S C , Meyer R , Moseley S L , Murray B E , Noah C W , Rhea U S , Rubin F A , Ruby R M , Singleton E , Tardio J L , Varney G W , Weagant S D , Wohlhieter J A , Womble D D , Wong P , Zink D L 
Published: February 2020

Abstract
The genes that encode several of the enterotoxins produced by Escherichia coli have been cloned by recombinant DNA techniques. When the nucleotide sequence of these genes is determined, defined sequence oligonucleotides that include a part of these genes may be synthesized. A 22-base DNA hybridization probe was produced for each of 2 heatstable E. coli enterotoxin (ST) genes: STH, from strains originally isolated from humans; and STP, from strains first found in pigs. For this study, 32P end-labeled DNA probes, sonicated calf thymus DNA, and 3 known and 20 unknown (10 ST-positive and 10 ST-negative) strains were sent to each of 23 collaborators. Cultures were spotted onto an agar-based medium and grown into colonies, which were transferred by blotting to cellulose filters, lysed by alkali and steam, and used for DNA colony hybridization with the ST DNA probes. Strains containing an ST gene were recognized as dark spots on an autoradiogram. Of the 460 samples analyzed, 440 (95.7%) were correctly classified by the collaborators. The method has been adopted official first action.
Determination of Sulfite in Food by Flow Injection Analysis
Authors: Sullivan John J , Hollingworth Thomas A , Wekell Marleen M , Newton Richard T , Larose Jack E 
Published: February 2020

Abstract
A method is described for the determination of sulfite levels in food products by flow injection analysis (FIA). The method is based on the decolorization of malachite green by S02, which is isolated from the flowing sample stream by means of a gas diffusion cell. The FIA method has a detection limit in food sample extracts of 0.1 ppm S02 (3 times peak height of blank), which corresponds to 1-10 ppm S02 in a food product, depending on the extraction procedure used. At the 5 ppm SO2 level in a food extract, the precision of replicate injections is ± 1-2%. The method was tested on a variety of both sulfite-treaied and untreated food products and the results compared favorably with those obtained by the Monier-Williams, colorimetric (pararosaniline), and enzymatic (sulfite oxidase) methods. The average differences from the FIA results were 19, 11, and 12%, respectively, for those samples (n = 12) above SO ppm S02. At lower levels the results were somewhat more erratic due to inaccuracies of the various methods at low concentrations.
Analysis of Eleven Triazines in Natural Waters
Authors: Lee Hing-Biu , Stokker Yvonne D 
Published: February 2020

Abstract
A gas chromatographic method was developed for the analysis of 11 triazine herbicides in natural waters. Triazine residues were extracted from water by methylene chloride and cleaned up on a 10% deactivated Florisil column, using 3% methanol in benzene as eluant. Extracts were quantitated, in 2 separate runs, on an Ultrabond 20M and a 3% OV-1 column connected to a nitrogen-phosphorus detector. These extracts could also be analyzed on a 30 m DB-1 capillary column in a single run. This method has been validated at 10, 1, and 0.1 u.g/L by using fortified distilled water and Lake Ontario water, and was also validated at 1.0 μg/L with 2 other natural water samples. Recoveries of the 11 triazines at all levels of fortification were between 87 and 108%, except simetone and simetryne were about 80% recovered in a few cases. Detection limit for all 11 triazines in this method is 0.025 μg/L.
Determination of Residues of Alachlor and Its Metabolite in Corn, Soybeans, and Potatoes as Heptafluorobutyryl-2,6-Diethylaniline
Authors: Newsome W Harvey , Collins Peter , Lewis David 
Published: February 2020

Abstract
Alachlor [2-chloro-2'6'-diethyl-N-(methoxymethyl)acetanilide] was determined by hydrolysis to 2,6-diethylaniline with 6N HC1 and quantitation of the heptafluorobutyryl derivative by gas chromatography with electron capture detection. 2,6-Diethylaniline was isolated from the hydrolysate by steam distillation, derivatized with heptafluorobutyric anhydride, and the derivative was purified by chromatography on silicic acid with 60% toluene in hexane as eluant. Recoveries from potatoes, soybeans, and corn spiked at levels from 3 to 26 ppb averaged 81,90, and 96% respectively.
Determination of the Composition of Gentamicin Sulfates by 1H and 13C Nuclear Magnetic Spectroscopy
Authors: Busson Roger , Claes Paul J , Vanderhaeghe Hubert 
Published: February 2020

Abstract
The British Pharmacopoeia test controlling the composition of gentamicin sulfate is based on CW 60 MHz magnetic resonance spectroscopy. Application of this method to FT 90 MHz spectra was evaluated. Results clearly show the limitations of this technique and point out the need for more reliable assay methods. Thus a 13C nuclear magnetic resonance (NMR) procedure for quantitative analysis of gentamicin sulfate was developed. Ratios of 4 gentamicin components (C1, C2, C1., and C2.) were obtained from peak height measurements of selected resonance signals in spectra recorded under steady-state conditions. Relative response factors were determined from spectra of a reference mixture or, alternatively, from spectra of the individual pure components. Results obtained by the 13C NMR method were in agreement with those obtained by liquid chromatography using pre-column derivatization.
Liquid Chromatographic Determination of Coumarin Anticoagulants in Tablets
Authors: Moore Ella , Lau-Cam Cesar 
Published: February 2020

Abstract
A simple and rapid liquid chromatographic method is described for the qualitative and quantitative determination of 5 coumarin anticoagulants in tablet composites and individual tablets. Analyses are carried out on a C18 reverse phase column using tetrahydrofuran-methanol-water-acetic acid (35 + 10 + 65 + 0.1) as mobile phase and photometric detection at 311 nm. The coefficients of variation for 10 consecutive injections of a mixed standards solution ranged from 0.28% for ethyl biscoumacetate to 0.78% for acenocoumarol. Standard recoveries were as follows: acenocoumarol, 99.3%; dicumarol, 99.6%; phenprocoumon, 101.6%; and warfarin sodium, 99.0%. The method was linear between 2 and 8 μg of drug injected. Assay results agreed favorably with those of the USP XX methods for dicumarol, phenprocoumon, and warfarin, and the NF XIV method for acenocoumarol. In addition, close correspondence was found with the results previously reported for the same drugs by a semiautomated spectrophotometric method. The content uniformity testing of individual 50 mg dicumarol tablets and 5 mg warfarin sodium tablets by the proposed method gave average (SD) values of 100.32% (0.64) and 101.00% (0.14), respectively, whereas these values were 101.60% (1.81) and 101.80% (0.18), respectively, by the method of USP XX.
Liquid Chromatographic Determination of Spiramycin Residues in Chicken Tissues
Authors: Nagata Tomoko , Saeki Masanobu 
Published: February 2020

Abstract
A liquid chromatographic (LC) method is described for determination of spiramycin residues in chicken muscles. The drug is extracted from muscles with acetonitrile, the extract is concentrated to 3-4 mL and rinsed with n-hexane followed by ethyl ether, and the drug is extracted with chloroform. LC analysis is carried out on a Zorbax BP-C8 column, and spiramycin is detected spectrophotometrically at 231 nm. Recoveries of spiramycin added to chicken muscles at 0.2 and 0.1 ppm were 93.9 and 89.0%, respectively. The detection limit was 5 ng for spiramycin standard, and 0.05 ppm in chicken muscles.
Determination of Morantel-Related Residues in Bovine Milk by Electron Capture Gas Chromatography
Authors: Lynch Martin J , Burnett Donald M , Mosher Franklyn R , Dimmock Mary E , Bartolucci S Richard 
Published: February 2020

Abstract
A gas chromatographic assay was developed to determine major residues of morantel in bovine milk over a range that is suitable for monitoring residues of the drug. The method is based on hydrolysis of the N-methyl-tetrahy dropyrimidine portion of morantel and its metabolites to N-mefhyl-1,3-propanediamine, and converting the diamine to an N,N-bis-(2-nitro-4-trifluoromethylphenyl) derivative. The addition of an internal standard, the N-desmethyl-N-ethyl homolog of pyrantel, to the milk sample circumvents any potential problem that could arise from variable reaction yields, and eliminates the true recovery as a factor affecting the accuracy and precision of the procedure. The concentrations of the derivatives are determined by pulsed electron capture gas chromatography over a linear dynamic range that is equivalent to 12.5-50 ppb morantel. The method was evaluated at the 0, 12.5,25, and 50 ppb levels in fortified bovine milk, and in a withdrawal sample containing physiologically incurred morantel residues. Mean values of 14 ± 1.7,24 ± 3.7, and 47 ± 6.9 were found for the fortified samples, approximately 3 ppb for control milk, and 16 ± 1.7 ppb for the withdrawal sample.
Anion-Exchange Method for Determination of Phytate in Foods: Collaborative Study
Authors: Harland Barbara F , Oberleas Donald ,   Collaborators:, Ellis R , Gelroth J , Gordon D , Phillips K , Ranhotra G , Shah B G , Stoecker B , Trick K D , Zymonas J 
Published: February 2020

Abstract
Phytate, a naturally occurring organic compound found in plant seeds, roots, and tubers, was determined in a collaborative study using a modified anion-exchange method. Seven samples (peanut flour, oats, rice, isolated soybean protein, a vegetarian diet composite, wheat bran, and whole wheat bread), supplied as blind duplicate samples, were analyzed in triplicate by 7 collaborators. Phytate concentrations in the samples ranged from 2.38 to 46.70 mg/g. Relative standard deviations (RSD = CV) for repeatability ranged from 2.5 to 10.1%, and for reproducibility, from 4.5 to 11.0%. The method has been adopted official first action.
Effects of Superglue, Other Fingerprint Developing Agents, and Luminol on Bloodstain Analysis
Authors: Duncan George T , Seiden Howard , Vallee Laura , Ferraro Donna 
Published: February 2020

Abstract
The stability of bloodstains exposed to various fingerprint developing agents (superglue, ninhydrin, and black powder) and luminol, which indicate the presence of blood via luminescence, was examined. Parameters used to characterize the stability were those common to forensic serology, and included any anomolies in ABO grouping, enzyme electrophoresis, species origin tests, and crystal and peroxidase examinations for the presence of hemoglobin in blood. Blood samples were collected from laboratory personnel and placed on absorbent and nonabsorbent substrates. These samples were then exposed to the developing agents and were characterized by using serological methods. Superglue, luminol, and black powder did not interfere with catalytic (peroxidase) examinations, crystal testing for hemoglobin, species origin testing, or ABO blood grouping. It was noted, however, that ninhydrin may adversely affect species origin, hemoglobin tests, and typing of “O” blood groups. All materials except black powder destroyed or weakened various enzymes of forensic interest. These results strongly suggest that before any fingerprint development, blood samples should be collected for serological examination by qualified personnel except when the black powder fingerprint method is used.