Gas-Liquid Chromatographic Headspace Method for Vinyl Chloride in Vinegars and Alcoholic Beverages

1976 ◽  
Vol 59 (1) ◽  
pp. 30-31
Author(s):  
David T Williams
Keyword(s):  
Mass Spectrometry ◽  
Vinyl Chloride ◽  
Limit Of Detection ◽  
Direct Injection ◽  
Headspace Analysis ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Injection Methods ◽  
Liquid Chromatographic

Abstract Vinyl chloride (VC) is determined in vinegars and alcoholic beverages by gas-liquid chromatographic headspace analysis. The lower limit of detection is 10 ppb and confirmation by gas chromatography-mass spectrometry, single ion monitoring at m/e 62, is possible at this level. Comparison of the headspace and the direct injection methods for the determination of VC in vinegars and alcoholic beverages showed that the results obtained by the 2 methods were not significantly different (P>0.05).

Gas-Liquid Chromatographic Determination of Vinyl Chloride in Alcoholic Beverages, Vegetable Oils, and Vinegars

1975 ◽  
Vol 58 (2) ◽  
pp. 272-275 ◽  
Author(s):  
David T Williams ◽  
Walter F Miles
Keyword(s):  
Vinyl Chloride ◽  
Vegetable Oils ◽  
Limit Of Detection ◽  
Direct Injection ◽  
Headspace Analysis ◽  
Chromatographic Determination ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Vinyl chloride in foods is determined by gasliquid chromatography either by direct injection of vinegars and alcoholic beverages or by headspace analysis of vegetable oils. The lower limit of detection is 10–15 ng/ml for direct injection and 5–10 ppb for headspace analysis. Confirmation by gas chromatography-mass spectrometry, single ion monitoring at m/e 62, is possible at 50 ppb for either method. The levels of vinyl chloride found in foods packaged in polyvinyl chloride bottles were 0.0–1.6 μg/ml for alcoholic beverages, 0.0–8.4 μg/ml for vinegars, and 0.3–3.3 ppm for peanut oil.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

Determination of Phytosterols in Butter Samples by Using Capillary Column Gas Chromatography

1987 ◽  
Vol 70 (5) ◽  
pp. 912-915 ◽  
Author(s):  
Randall L Smith ◽  
Darryl M Sullivan ◽  
Earl F Richter
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Packed Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Positive Bias ◽  
Capillary Column Gas Chromatography

Abstract A positive bias in the gas chromatographic (GC) analysis of butter for β-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from β-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate β-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%

Gas Chromatographic/Mass Spectrometric Determination of α-Methylstyrene in Styrene-Based Polymers and Food Simulants

1991 ◽  
Vol 74 (5) ◽  
pp. 815-818
Author(s):  
Shigeru Tan ◽  
Takashi Tatsuno ◽  
Taro Okada
Keyword(s):  
Mass Spectrometry ◽  
Direct Injection ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Monitoring Method ◽  
Food Simulants ◽  
Multiple Ion Monitoring ◽  
Chromatographic Mass

Abstract A selected ion monitoring method is described for the analysis of styrene (St)-based polymers for a-methylstyrene (α- MSt) and for determining the level of α-MSt migration from St-based sheets Into 4 food simulants. The polymers are dissolved in dlchloromethane; α-MSt Is determined by direct Injection of the polymer solutions. α-MSt migration from St-based sheet to water, 4% acetic acid, 20% ethanol, and n-heptane was measured by gas chromatography/mass spectrometry, using multiple ion monitoring of Ions at mix 118,78, and 91. α-MSt can be quantltated at levels as low as 10 μ/g in the polymer and 0.01 μ/g In the food simulants. Recoveries were 83-113% from St-based sheets and 90-99% from food simulants, respectively.

Determination of ketamine and norketamine in hair and evaluation of polydrug use in ketamine abusers using hair analysis in Korea

2020 ◽  
Author(s):  
Jongsook Rhee ◽  
Jihyun Kim ◽  
Moonhee Jang ◽  
Ilchung Shi ◽  
Sangki Lee
Keyword(s):  
Mass Spectrometry ◽  
Matrix Effects ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Controlled Drugs ◽  
Hair Samples ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Forensic Service

Abstract This study evaluated hair samples from 28 subjects who had measurable ketamine levels among the samples requested from 2016 to 2017 into Seoul Institute National Forensic Service in Korea. Ketamine in the hair was extracted by using a solution of 1% hydrochloric acid in methanol for 16 h. Extracts were analyzed using gas chromatography mass spectrometry (GC-MS) or liquid chromatography tandem mass spectrometry (LC-MS-MS). LC-MS-MS method was validated by determining the limit of detection (LOD), limit of quantitation (LOQ), linearity, intra- and inter-accuracy, precision, and matrix effects. In 59 ketamine-positive hair or hair segments from 28 ketamine abusers, the ketamine concentration was found to be in the range of 0.011-335.8 ng/mg (mean, 13.6; median, 1.8), and the norketamine concentration was found to be in the range of 0.001-35.7 ng/mg (mean, 7.5; median, 0.44). The ratio of norketamine to ketamine concentration in hair was in the range of 0.01-1.46 (mean, 0.34; median, 0.26). The distribution of ketamine concentration in hair samples was as follows: 0.01-0.1 ng/mg in 11 samples (18.6%), 0.1-5 ng/mg in 33 samples (55.9%), 5-10 ng/mg in 4 samples (6.8%), 10-15 ng/mg in 2 samples (3.4%), 15-20 ng/mg in 4 samples (6.8%), 40-45 ng/mg in 2 samples (3.4%), 45-50 ng/mg in 1 samples 1.7%) and >100 ng/mg in only 2 samples (3.4%). In the hair of ketamine-abusers, 26 of 28 subjects had simultaneously ketamine with detectable levels of other controlled drugs, including MDMA (n=9), MA (n=3), MDMA/MA (n=3), MDMA/PMA (n=3), MDMA/PMA/MA (n=2), cocaine (n=1), and other drugs (n=5, propofol, zolpidem or benzodiazepines). In most of the hair samples were detected ketamine with other controlled drugs: MDMA (60.7%), MA (28.6%), PMA(17.9%), zolpidem (17.9%), and propofol (14.3%) in the frequency of abuse. In conclusion, most of the ketamine-abusers (92.9%) would be polydrug abusers, who were concomitantly abusing other controlled substances.

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 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.

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