Liquid Chromatographic Determination of Moxidectin Residues in Cattle Tissues and Confirmation in Cattle Fat by Liquid Chromatography/Mass Spectrometry

1993 ◽  
Vol 76 (6) ◽  
pp. 1230-1235 ◽  
Author(s):  
Alisa Khunachak ◽  
Adrian R Dacunha ◽  
Steven J Stout
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Parent Compound ◽  
Chromatographic Determination ◽  
Liquid Chromatography Mass Spectrometry ◽  
Liver And Kidney ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Moxidectin, a potent new endo- and ectoparasitic agent, is determined in cattle tissues by liquid chromatography (LC) with fluorescence detection. Moxidectin residues in cattle fat are confirmed with thermospray LC/mass spectrometry (MS). Moxidectin is extracted from the tissue with acetonitrile; the extract is partitioned with hexane, concentrated, and reacted with acetic anhydride, 1-methylimidazole, and dimethylformamide to produce a fluorescent product. The validated sensitivity of the LC/fluorescence method was 10 ppb, with a limit of detection typically between 1 and 2 ppb. Average recoveries from cattle fat, muscle, liver, and kidney were 99,95,89, and 92%, respectively. LC/MS confirmatory method determined the underivatized parent compound following the acetonitrilehexane partitioning step, with an average recovery of 108% at the 250 ppb level in cattle fat.

Gas-Liquid Chromatographic Determination of Ethylenediaminetetraacetic Acid in Pickled Vegetables

1974 ◽  
Vol 57 (6) ◽  
pp. 1383-1385
Author(s):  
David T Williams
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Ethylenediaminetetraacetic Acid ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatography Mass Spectrometry ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Pickled Vegetables

Abstract A method has been developed for the determination of ethylenediaminetetraacetic acid in pickled vegetables after conversion to its tetramethyl ester. The ester is identified by gas-liquid chromatography and confirmed by gas-liquid chromatography-mass spectrometry. Recoveries from pickled beet samples spiked at 20-250 ppm were 87-74%.

Simultaneous Liquid Chromatographic Determination of Thiabendazole, o-Phenylphenol, and Diphenyl Residues in Citrus Fruits, Without Prior Cleanup

1982 ◽  
Vol 65 (6) ◽  
pp. 1302-1304
Author(s):  
Yoshimi Kitada ◽  
Michiko Sasaki ◽  
Kaoru Tanigawa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Citrus Fruits ◽  
Ultraviolet Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, rapid, efficient method has been developed for determining thiabendazole, o-phenylphenol, and diphenyl in citrus fruits by using high performance liquid chromatography, with fluorescence or ultraviolet detection. The compounds are extracted with ethyl acetate and separated from soluble fruit components on a LiChrosorb RP-8 column. Recovery of these compounds added to citrus fruits at 5 or 50 ppm levels was >93%; the limit of detection for the compounds is 1 ppm.

Gas-Liquid Chromatographic Determination of Congeners in Alcoholic Products with Confirmation by Gas Chromatography/Mass Spectrometry

1981 ◽  
Vol 64 (1) ◽  
pp. 186-190
Author(s):  
Glenn E Martin ◽  
James M Burggraff ◽  
Randolph H Dyer ◽  
Peter C Buscemi
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Acetic Acid ◽  
Liquid Chromatography ◽  
Chromatographic Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A procedure is described for the separation and determination of the following compounds which are found as congeners in alcoholic products: acetaldehyde, ethyl acetate, methanol, ethanol, n-propanol, isobutanol, n-butanol, acetic acid, and the amyl alcohols (2-methyl-l-butanol and 3-methyl-l-butanol). These compounds were separated by gas-liquid chromatography (GLC) using 5% Carbowax 20M on Carbopack B as the column packing. The results obtained by using this method were compared with those obtained using the present AOAC methods for these compounds. GLC chromatograms show better resolution by the method presented.

Mass Spectral Identification and Gas-Liquid Chromatographic Determination of Methyl 4-Chloroindolyl-3-Acetate in Canned and Frozen Peas

1980 ◽  
Vol 63 (6) ◽  
pp. 1224-1225
Author(s):  
David L Heikes
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Mass Spectral ◽  
Spectral Identification ◽  
Naturally Occurring ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Methyl 4-chloroindolyl-3-acetate (MCIA), a naturally occurring auxin, has been identified in canned and frozen peas by gas-liquid chromatography (GLC)/mass spectrometry. Eight samples were analyzed for MCIA using slightly modified official AOAC multiple pesticide residue procedures employing GLC with microcoulometric detection. Levels of MCIA averaged 0.20 ppm for canned peas and 0.16 ppm for frozen peas. Recovery of MCIA from a fortified sample was 40%.

High-Speed Liquid Chromatographic Determination of o-Phenylphenol Residues in Citrus Products

1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder
Keyword(s):  
Liquid Chromatography ◽  
Quantitative Analysis ◽  
High Speed ◽  
Steam Distillation ◽  
Chromatographic Determination ◽  
Analysis Time ◽  
Hexane Extraction ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.

Gas-Liquid Chromatographic Determination of Sodium Fluoroacetate (Compound 1080)

1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker
Keyword(s):  
Liquid Chromatography ◽  
Tissue Sample ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Tissue Samples ◽  
Fluoroacetic Acid ◽  
Pentafluorobenzyl Bromide ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.

Gas-Liquid Chromatographic Determination of Maleic Hydrazide in Tobacco and Tobacco Smoke

1979 ◽  
Vol 62 (1) ◽  
pp. 171-175 ◽  
Author(s):  
Alfred F Haeberer ◽  
Orestes T Chortyk
Keyword(s):  
Liquid Chromatography ◽  
Tobacco Smoke ◽  
Plant Growth Regulator ◽  
Maleic Hydrazide ◽  
Chromatographic Determination ◽  
Gas Liquid Chromatography ◽  
Trimethylsilyl Derivative ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is presented for the determination of the plant growth regulator maleic hydrazide (MH; l,2-dihydro-3,6-pyridazinedione) in tobacco and tobacco smoke. Residues are converted to the bis(trimethylsilyl) derivative before analysis by gas-liquid chromatography. The method has been applied to cigarettes and condensed smoke and has been used to determine the per cent transfer of MH into cigarette smoke. Free MH residues could be determined directly on the tobacco samples, whereas total MH values were obtainable only after acid hydrolysis. In spite of large MH residues in tobacco, only 0.2% of the MH was transferred into smoke.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

Gas-Liquid Chromatographic Determination of T-2 Toxin in Plasma

1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Aqueous Sodium Hydroxide ◽  
Chromatographic Determination ◽  
Florisil Column ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.

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