Gas Chromatographic-Mass Spectrometric Detection and Quantitation of Lincomycin in Animal Feedingstuffs

1984 ◽  
Vol 67 (3) ◽  
pp. 582-588
Author(s):  
Cecil H McMurray ◽  
W John Blanchflower ◽  
Desmond A Rice
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Coefficient Of Variation ◽  
Chemical Ionization ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Ionization Mode ◽  
Main Fragment ◽  
Chromatographic Mass

Abstract A substantially Improved assay was developed for lincomycin A in animal feedingstuffs. The assay allows unambiguous quantitation of at least 0.1 ppm in feed. Lincomycin B did not interfere because of differences in both retention time and mass of the main fragment ion in electron impact (EI) spectra. The assay using single ion monitoring with EI detection would not discriminate between lincomycin A and clindamycin. The presence of the latter was easily confirmed by using gas chromatography-mass spectrometry in the chemical ionization mode. The assay for lincomycin A was linear in the range 0–40 ng applied to the gas chromatographic column. The recovery was 93.4 ± 4.2% at 1 and 5 ppm and 86.2 ± 5.5% at 0.1 ppm in feed. The coefficient of variation of the assay was 4.8% at both 1 and 5 ppm, and was 6.43% at 0.1 ppm.

Gas chromatographic-mass spectrometric assay for 6-hydroxymelatonin sulfate and 6-hydroxymelatonin glucuronide in urine.

1987 ◽  
Vol 33 (4) ◽  
pp. 453-457 ◽  
Author(s):  
P L Francis ◽  
A M Leone ◽  
I M Young ◽  
P Stovell ◽  
R E Silman
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Original Sample ◽  
Chromatography Mass Spectrometry ◽  
Chromatographic Mass

Abstract Circulating melatonin is hydroxylated to 6-hydroxymelatonin and excreted in urine as the sulfate and glucuronide conjugates. We extracted these two compounds from urine by using octadecylsilane-bonded silica cartridges to eliminate most of the urea and electrolytes, and silica cartridges to separate the sulfate and glucuronide conjugates. After hydrolyzing the separated conjugates enzymically, we determined the free hydroxymelatonin by gas chromatography-mass spectrometry. Though recoveries were low and variable, we were able to quantify the analyte in the original sample by adding deuterated sulfate and glucuronide conjugates to the urines before extraction.

Gas Chromatographic/Mass Spectrometric Determination of Benzene in Nonstick Cookware and Microwave Susceptors and Its Migration into Foods on Cooking

1993 ◽  
Vol 76 (4) ◽  
pp. 760-764 ◽  
Author(s):  
Sue M Jickells ◽  
Mark R Philo ◽  
John Gilbert ◽  
Laurence Castle
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Polymer Coatings ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Static Headspace ◽  
Headspace Gc ◽  
Chromatographic Mass

Abstract Benzene in poly(tetrafluoroethylene) (PTFE) coatings of nonstick cookware was determined by heating a small amount of coating in a sealed vial. Gas chromatography/mass spectrometry (GC/MS) was used to analyze the vial headspace for benzene. A small survey (26 samples) of retail nonstick cookware detected benzene ranging from 2 to 50 μg/dm2 in 7 samples. Nonstick frying pans with various polymer coatings were obtained directly from 1 manufacturer. Benzene (6–30 μg/dm2) was detected in a number of these samples and was attributed to the use of a phenylmethyl silicone ingredient that contained benzene at 360 mg/kg. To determine the possible transfer of benzene from these coatings during normal use, several foods (puddings, cakes, and roast potatoes) were prepared in previously unused cookware. The foods were analyzed by using static headspace GC/MS. Benzene was not detected in any of these foods at a limit of detection of 2 μg/kg. In related studies, the determination of benzene release from microwave susceptors was performed by heating the materials in a sealed system at 190PC for 4 min. Benzene release above 1 μg/dm2 was not detected in 24 samples of susceptors. However, 1 specially supplied sample of nonmetallized susceptor released 10 μg/dm2 benzene when heated above normal anticipated temperatures of usage (to 220°C). Foods such as french fries and pizza when cooked according to the manufacturer’s instructions in susceptors contained no benzene with a limit of detection of 2 μg/kg. Even under abuse conditions of susceptors, the transfer of benzene to foods remained below this limit.

Versatile, efficient system for extracting drugs from urine for gas chromatographic/mass spectrometric analysis.

1989 ◽  
Vol 35 (10) ◽  
pp. 2100-2103 ◽  
Author(s):  
K E Brooks ◽  
N B Smith
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometric Analysis ◽  
Efficient System ◽  
Carboxylate Groups ◽  
Amino Amide ◽  
Alcoholic Hydroxyl ◽  
Chromatographic Mass

Abstract This is a method for efficiently extracting a wide variety of drugs from urine for toxicological analysis by gas chromatography/mass spectrometry. Before extraction, the urine sample is acetylated, diluted with an equal volume of water, and saturated with NaCl. This solution is then mixed with an equal volume of dichloromethane/acetone (2:1 by vol). The organic (top) phase is aspirated and evaporated, and the residue is redissolved in a suitable solvent for injection or further derivatization. This procedure is suitable for all drugs except carboxylate-containing drugs, which may be isolated by replacing the acetylation step with acidification of the urine to pH 2. Studies with 16 drugs containing amino, amide, alcoholic hydroxyl, phenolic hydroxyl, carboxylate groups, or combinations thereof, showed that all drugs except theophylline and benzoylecgonine were extracted with analytical recoveries ranging from 70% to 100%.

Detection of pentazocine and tripelennamine in urine.

1981 ◽  
Vol 27 (1) ◽  
pp. 10-13 ◽  
Author(s):  
R W Reid ◽  
C M Gerbeck
Keyword(s):  
Gas Chromatography ◽  
Drug Abuse ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Chemical Ionization ◽  
Mass Spectrometric ◽  
Routine Screening ◽  
Ionization Mode ◽  
Layer Chromatography ◽  
Chromatographic Mass

Abstract Pentazocine and tripelennamine can be identified in urine as a part of routine screening for drug abuse. Pentazocine, pentazocine hydrate, and tripelennamine can be detected by thin-layer chromatography of chloroform/isopropanol extracts of heat- and acid-hydrolyzed urine. Gas chromatography is used for confirmation. Gas chromatographic/mass spectrometric studies (chemical ionization mode) show that such extracts contain major molecular (M+) ions of m/e 256, 286, and 304, indicating the presence of tripelennamine, pentazocine, and pentazocine hydrate, respectively.

scholarly journals Extractives of Fungi. VI Gas Chromatographic-Mass Spectrometric Investigations of the Lipids of Trametes Lilacino-Gilva (Berk.) Lloyd

1981 ◽  
Vol 34 (1) ◽  
pp. 115 ◽  
Author(s):  
RK Christopher ◽  
AM Duffield ◽  
J Ralph ◽  
J JH Simes
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Chromatographic Mass

The lipid constituents of T. lilacino-gilva were examined by gas chromatography and gas chromatography?mass spectrometry.

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