Gas Chromatographic-Mass Spectiometric Determination of Adipate-Based Polymeric Plasticizers in Foods

1988 ◽  
Vol 71 (2) ◽  
pp. 394-396 ◽  
Author(s):  
Laurence Castle ◽  
Angela J Mercer ◽  
John Gilbert
Keyword(s):  
Internal Standard ◽  
Size Exclusion ◽  
Gas Chromatography Mass Spectrometry ◽  
Stable Isotope Dilution ◽  
Relative Standard ◽  
Exclusion Chromatography ◽  
Deuterated Internal Standard ◽  
Polymeric Plasticizer ◽  
Chromatographic Mass

Abstract A method for the quantitative determination of adipate-based polymeric plasticizers in foods is described. The procedure involves extraction from the food and transmethylation of the polymeric plasticizer to form dimethyladipate (DMA). The derivative is cleaned up by size-exclusion chromatography and determined by capillary gas chromatography-mass spectrometry with selected on monitoring. The use of a deuterated internal standard at the extraction stage enables quantitation by stable isotope dilution. A detection limit of 0.1 mg/kg of the polymeric plasticizer in foods and a relative standard deviation of 4% have been achieved routinely. The method has been applied successfully to the analysis of cheese, sandwiches, meat, biscuits, and cake that have been in contact with polymeric plasticized polyvinyl chloride) films.

Gas chromatographic mass spectrometric determination of myo-inositol in humans utilizing a deuterated internal standard

1982 ◽  
Vol 9 (4) ◽  
pp. 135-140 ◽  
Author(s):  
Jan Rud Andersen ◽  
Elfinn Larsen ◽  
Helge Harbo ◽  
Boye Bertelsen ◽  
J. E. Just Christensen ◽  
...  
Keyword(s):  
Internal Standard ◽  
Mass Spectrometric ◽  
Mass Spectrometric Determination ◽  
Deuterated Internal Standard ◽  
Chromatographic Mass

scholarly journals Size Exclusion Chromatographic Cleanup for GC/MS Determination of Organophosphorus Pesticide Residues in Household and Vehicle Dust

2002 ◽  
Vol 85 (1) ◽  
pp. 36-43 ◽  
Author(s):  
Thomas F Moate ◽  
Matthew Furia ◽  
Cynthia Curl ◽  
Juan F Muniz ◽  
Jianbo Yu ◽  
...  
Keyword(s):  
Organophosphorus Pesticides ◽  
Organophosphorus Pesticide ◽  
Fruit Production ◽  
Size Exclusion ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Size Exclusion Chromatographic ◽  
Tree Fruit ◽  
Exclusion Chromatography

Abstract Size exclusion chromatography (SEC) was used as a cleanup method for the analysis of organophosphorus pesticides in household and vehicle dusts. The pesticides investigated were diazinon, methyl parathion, chlorpyrifos, malathion, phosmet, and azinphosmethyl. These compounds are of interest due to their use in agricultural tree fruit production and/or urban pest control. Pesticides were determined via gas chromatography/mass spectrometry with selected-ion monitoring and cool on-column injection. The lower limit of method validation was 0.20 μg/g. Method limits of detection in dust ranged from 0.012–0.055 μg/g. Dust samples were collected with vacuums from the homes and vehicles of people living and working in a rural agricultural region in the central part of Washington State. The analytes were extracted from the dust by sonication in acetone. The extracts were solvent-exchanged to cyclohexane, frozen, thawed, and centrifuged prior to SEC injection. Following SEC, the eluent was split into 2 fractions, concentrated, and injected on-column into the gas chromatograph. This method represents the first complete publication describing the SEC cleanup of organophosphorus pesticides in dusts. Recoveries of pesticides in dusts ranged from 63.5–110.8 ± 4.9–19.6% over a fortification range of 0.20–10.00 μg/g. This optimized, automated, and reproducible SEC method does not require further treatment or cleanup for trace determination of these organophosphorus pesticides.

scholarly journals Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Lidong Cao ◽  
Hua Jiang ◽  
Jing Yang ◽  
Li Fan ◽  
Fengmin Li ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Internal Standard ◽  
Fused Silica ◽  
Gas Chromatography Mass Spectrometry ◽  
Equilibration Time ◽  
Emulsifiable Concentrate ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
Standard Additions

The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS) method using fluorobenzene as an internal standard (IS) for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC) was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m×0.20 mmi.d. and 0.25 μm film thickness) with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD) of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations.

Gas Chromatographic-Mass Spectrometric Determination of Epoxidized Soybean Oil Contamination of Foods by Migration from Plastic Packaging

1988 ◽  
Vol 71 (6) ◽  
pp. 1183-1186 ◽  
Author(s):  
Laurence Castle ◽  
Matthew Sharman ◽  
John Gilbert
Keyword(s):  
Fatty Acid ◽  
Soybean Oil ◽  
Lipid Extraction ◽  
Internal Standard ◽  
Epoxidized Soybean Oil ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Pvc Film ◽  
Relative Standard

Abstract A method for the quantitative determination of epoxidized soybean oil (ESBO) in foods is described. The procedure involves addition of a diepoxidized fatty acid ester internal standard, followed by lipid extraction from the food and transmethylation under basic conditions. Without further cleanup, the methylated fatty acid epoxides are derivatized to form 1,3-dioxolanes, which are then determined by capillary gas chromatography-mass spectrometry with selected ion monitoring. A detection limit of 2.0 mg/kg of epoxidized soybean oil in foods and a relative standard deviation of 7% have been achieved routinely. The method has been applied successfully to the analysis of cheeses, sandwiches, cakes, and microwave-cooked meals which have been contaminated with ESBO by migration from PVC film.

Gas Chromatographic Determinatiion of Monoethylene Glycol and Diethylene Glycol in Chocolate Packaged in Regenerated Cellulose Film

1988 ◽  
Vol 71 (3) ◽  
pp. 499-502
Author(s):  
Laurence Castle ◽  
Helen R Cloke ◽  
James R Startin ◽  
John Gilbert
Keyword(s):  
Gas Chromatography ◽  
Diethylene Glycol ◽  
Internal Standard ◽  
Hot Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Regenerated Cellulose ◽  
Regenerated Cellulose Film ◽  
Relative Standard ◽  
Monoethylene Glycol

Abstract A method for the quantitative determination of monoethylene glycol (MEG) and diethylene glycol (DEG) in chocolate is described. The procedure involves dissolving the chocolate in hot water, defatting with hexane, removing sugars by precipitation, and analyzing as trimethylsilyl (TMS) ether derivatives by capillary gas chromatography. The use of butan-l,4-dioI as an internal standard corrects for recovery, which is between 50 and 60%, to give a relative standard deviation of 10 -11 % for the determination of both glycols at the level of 50 mg/kg. The presence of MEG and DEG in chocolate is confirmed by full scanning gas chromatography/mass spectrometry of the TMS derivatives

scholarly journals Development and validation of a GC–MS method for the simultaneous determination of acetochlor, fluorochloridone, and pendimethalin in a herbicide emulsifiable concentrate formulation

2020 ◽  
Vol 32 (4) ◽  
pp. 238-241 ◽  
Author(s):  
Dandan Wang ◽  
Shengde Wu
Keyword(s):  
Internal Standard ◽  
Ternary Mixtures ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Limit Of Quantification ◽  
Emulsifiable Concentrate ◽  
Relative Standard ◽  
Replicate Measurements ◽  
Development And Validation

This paper describes a rapid method to simultaneously determine acetochlor, fluorochloridone and pendimethalin present in a herbicide emulsifiable concentrate (EC) formulation using gas chromatography–mass spectrometry (GC–MS). Selected ion monitoring mode was performed to increase the sensitivity, with dibutyl phthalate as an internal standard. The method was validated with respect to linearity, accuracy, precision, and stability. Chromatographic separation was carried out on a TG-5 MS column (30 m × 0.25 mm × 0.25 μm) with helium as the carrier gas at a flow rate of 1.0 mL/min. Calibration curves were linear over 2.0–20.0 μg/mL for each analyte, and the limit of quantification was below 20 ng/mL. Good performance in terms of recovery ranging from 94.5% to 102.5% at 3 concentration levels proved excellent accuracy. The intra- and inter-day relative standard deviations for 6 replicate measurements were always less than 5%. The developed method is simple and efficient for the routine determination of the ternary mixtures in a compound herbicide EC formulation product.

Oxybuprocaine and five metabolites simultaneously determined in urine by gas chromatography and gas chromatography-mass spectrometry after extraction with Extrelut.

1987 ◽  
Vol 33 (5) ◽  
pp. 697-700 ◽  
Author(s):  
F Kasuya ◽  
K Igarashi ◽  
M Fukui
Keyword(s):  
Gas Chromatography ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Aminobenzoic Acid ◽  
Acid Metabolite ◽  
Fragment Ions ◽  
Characteristic Fragment ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract We describe a gas-liquid chromatographic (GC) method for determination of oxybuprocaine, and a gas chromatographic-mass spectrometric (GC-MS) method for simultaneous determination of four of its nine metabolites in urine. We used an Extrelut column to simply and rapidly extract oxybuprocaine and its metabolites from urine. For the GC-MS analyses, we monitored the characteristic fragment ions at m/z 353, 395, 369, 411, and 235 for 3-butoxy-4-aminobenzoic acid (metabolite 2, M-2), 3-butoxy-4-acetylaminobenzoic acid (M-3), 3-hydroxy-4-aminobenzoic acid (M-4), 3-hydroxy-4-acetylaminobenzoic acid (M-5), and methaqualone (internal standard), respectively. We quantified the glucuronide of M-2 after enzymic treatment. The assay's selectivity and reproducibility (within-day and between-day CVs less than 8% for all metabolites) make it applicable to determine oxybuprocaine and its metabolites in human urine. Mean 9-h urinary excretion of oxybuprocaine and its five metabolites from four healthy volunteers was 89.2% after a 100-mg oral dose.

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