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.

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.

Development and validation of a gas chromatography/mass spectrometry method for the determination of α- and ß-2, 7, 11-cembratriene-4, 6-diols in tobacco

2016 ◽  
Vol 13 (4) ◽  
pp. 341-347
Author(s):  
Wei Gao ◽  
Naiying Wu ◽  
Wenliang Sun
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Content Type ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Development And Validation

Purpose This paper aims to present a robust method for the determination of α- and ß-2, 7, 11-cembratriene-4, 6-diols (α, ß-CBT-diol) in tobacco samples which was developed and validated by using the self-made α, ß-CBT-diol with higher purity as the standard. Design/methodology/approach After the ultrasonic extraction and clean-up procedures, samples were analyzed by gas chromatography/mass spectrometry in selected ion monitoring mode and full scan mode at the same time. A 1-heptadecanol was used as an internal standard. The important parameters, such as extraction conditions and derivation conditions, were optimized. Findings Under the optimal conditions, good results in terms of linearity (R2 > 0.999) and recoveries (93.2-107 per cent) were achieved. The limits of detection were 0.120 and 0.180 μg/ml for α- and ß-CBT-diol, respectively. α, ß-CBT-diol level of analyzed tobacco was found in the range of 34.2-1.26 × 103 μg/g with relative standard deviations below 6 per cent. Originality/value Such a strategy opens a new door towards the development of a simple, robust and sensitive method for the determination of α, ß-CBT-diol in real samples.

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.

Determination of Clenbuterol in Cattle, Sheep, and Swine Tissues by Electron Ionization Gas Chromatography/Mass Spectrometry

1994 ◽  
Vol 77 (4) ◽  
pp. 917-924 ◽  
Author(s):  
Roger T Wilson ◽  
Joseph M Groneck ◽  
Kathleen P Holland ◽  
A Carolyn Henry
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Electron Ionization ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Method Performance ◽  
Chromatography Mass Spectrometry ◽  
Coefficients Of Variation

Abstract A gas chromatographic/mass spectrometric procedure is described for the quantitation and confirmation of clenbuterol residues from cattle, sheep, and swine tissues. After liquid–liquid extraction and derivatization with phosgene in an aqueous pH 10.1 buffer, the cyclic oxazolidone derivative is quantitated with a clenbuterol analogue as internal standard (NAB-760 CI). Confirmation is accomplished by comparison of ion ratios with those of a pure synthesized standard of clenbuterol oxazolidin-3-one obtained by selected ion monitoring, electron ionization gas chromatography/mass spectrometry on a benchtop instrument. Statistical information based on a series of standard curves for fortified tissues is included to describe method performance. Ion ratio variations were under 15%, and coefficients of variation for spiked tissue standard curves were above 0.997. Recoveries averaged 87.1 ± 6.6% for liver tissues across all 3 species and 67.1 ± 3.8% for muscle tissue across all 3 species.

Determination of Flunixin in Milk by Liquid Chromatography with Confirmation by Gas Chromatography/Mass Spectrometry and Selected Ion Monitoring

1995 ◽  
Vol 78 (4) ◽  
pp. 959-966 ◽  
Author(s):  
Heidi S Rupp ◽  
David C Holland ◽  
Robert K Munns ◽  
Sherri B Turnipseed ◽  
Austin R Long
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Enzyme Treatment ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Flunixin Meglumine ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A liquid chromatographic (LC) method was developed for the determination of flunixin (FNX) in raw bovine milk. The milk was acidified and mixed with silica gel, and the mixture was packed into a chromatographic column. The column was defatted with water-saturated dichloromethane–hexane (30 + 70, v/v), and the analyte was eluted with EtOAc. The EtOAc extract was washed with water at pH 3.5, the water was discarded, and the EtOAc layer was then extracted with 0.1 M NaOH. The aqueous layer was drained, passed through a primed C18 solid-phase extraction (SPE) column, and eluted with EtOAc. The EtOAc layer was dried under N2, taken up in a solution of MeOH–(5 mM tetrabutylammonium [TBA]–H2PO4 + 2 mM NaOH) (50 + 50), sonicated, and filtered. FNX was determined by LC using a C18 column (ODS Hypersil), a mobile phase mixture of 58% A (MeOH) and 42% B (5 mM TBA–H2PO4 + 2 mM NaOH), and a diode-array ultraviolet detector at 285 nm. FNX was determined in raw milk at 5 spiking levels (5,10,20,40, and 80 ng drug/mL milk). Absolute recoveries ranged from 69.6 to 74.4%, and relative standard deviations ranged from 1.1 to 6.9%. The limit of quantitation was 1.7 ng drug/mL milk. A lactating cow was dosed intravenously (2.2 mg/kg) with flunixin meglumine (Banamine) to generate incurred milk residues. FNX residues ranged from 7.34 ng/mL at 16 h postdose to 1.74 ng/mL at 24 h postdose. Both levels were obtained with additional β-glucuronidase treatment (almost no incurred drug was detected at these low levels without the enzyme treatment). The presence of FNX in incurred milk was confirmed by gas chromatography/mass spectrometry with selected ion monitoring.

Evaluation and interlaboratory validation of a GC-MS method for analysis of pesticide residues in teas

2007 ◽  
Vol 61 (1) ◽  
pp. 1-5 ◽  
Author(s):  
C. Peng ◽  
H. Kuang ◽  
X. Li ◽  
C. Xu
Keyword(s):  
Simultaneous Determination ◽  
Pesticide Residues ◽  
Graphitized Carbon Black ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
External Standard Method ◽  
Relative Standard ◽  
Interlaboratory Validation ◽  
Acetone Hexane

AbstractA method was described for simultaneous determination of nine organic heterocyclic pesticide residues by gas chromatography-mass spectrometry-selected ion monitoring. Atrazine, vinclozolin, procymidone, triflumizole, imazalil, buprofezin, propiconazole, fenarimol, and pyridaben were clearly separated from each other, extracted with acetone—hexane mixture, purified with graphitized carbon black cartridge and neutral Al2O3 cartridge, eluted with acetone—hexane mixture, simultaneously determined by GC-MS, and then quantified with an external standard method. Recoveries of pesticides ranged from 73 % to 116 % at the spiked level of 0.01–30 mg kg−1, while the relative standard deviation was between 3 % and 27 %. In addition, the limits of determination (0.01 mg kg−1 to 5.0 mg kg−1) and linearity (0.02–40 μg mL−1) revealed that simultaneous determination of multi-residues in Chinese teas (like Oolong tea, green tea, red tea, etc.) was possible. Furthermore, an interlaboratory study among 5 labs was conducted to further validate the method, and the results were satisfactory.

scholarly journals Direct Synthesis of ESBO Derivatives-18O Labelled with Dioxirane

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Stefano La Tegola ◽  
Cosimo Annese ◽  
Michele Suman ◽  
Immacolata Tommasi ◽  
Caterina Fusco ◽  
...  
Keyword(s):  
Soybean Oil ◽  
Analytical Methods ◽  
Direct Synthesis ◽  
Internal Standard ◽  
Epoxidized Soybean Oil ◽  
New Approach ◽  
Food Matrices

This work addresses a new approach developed in our laboratory, consisting in the application of isolated dimethyldioxirane (DDO,1a) labelled with18O for synthesis of epoxidized glyceryl linoleate (Gly-LLL,2). We expect that this work could contribute in improving analytical methods for the determination of epoxidized soybean oil (ESBO) in complex food matrices by adopting an18O-labelled-epoxidized triacylglycerol as an internal standard.

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 Determination of Pesticides in Composite Dietary Samples by Gas Chromatography/Mass Spectrometry in the Selected Ion Monitoring Mode by Using a Temperature-Programmable Large Volume Injector with Preseparation Column

2001 ◽  
Vol 84 (3) ◽  
pp. 891-900 ◽  
Author(s):  
Laura Rosenblum ◽  
Thomas Hieber ◽  
Jeffrey Morgan
Keyword(s):  
Mass Spectrometry ◽  
Sample Preparation ◽  
Diatomaceous Earth ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Residue Detection ◽  
Relative Standard ◽  
Wide Range ◽  
Mode Method

Abstract Use of a temperature-programmable preseparation column in the gas chromatographic (GC) injection port permits determination of a wide range of semi-volatile pesticides including organochlorines, organophosphates, triazines, and anilines in fatty composite dietary samples while reducing sample preparation time and solvent consumption. Dietary samples are mixed with diatomaceous earth and are Soxhlet-extracted with an azeotropic solution of hexane and acetone. Sample preparation uses liquid–liquid partitioning over diatomaceous earth followed by normal phase chromatography over partially deactivated alumina. The final cleanup step occurs in a preseparation column in the GC injector, which is able to perform splitless transfer of the analytes to the analytical column and purge 99% of the high molecular weight residue. Detection is performed by GC/mass spectrometry (MS) in the selected ion monitoring mode. Method detection limits were at or below 2 ng/g for 24 of 35 pesticides studied, with recovery between 70 and 125% for 27 pesticides in samples fortified at 10 ng/g. Recovery was not dependent on fat content when measured in laboratory fortified samples containing 1, 5, and 10% fat by weight. Precision over multiple injections was acceptable, with a relative standard deviation of 2.6–15% for 25 analytes.

scholarly journals Determination of acrylamide in foods by automatic accelerated solvent extraction and gas chromatography-mass spectrometry

2020 ◽  
Author(s):  
Cuicui Kang ◽  
Haijian Ma ◽  
Yuan Li ◽  
Chizhong Zhang ◽  
Yueqin Hong ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solvent Extraction ◽  
Internal Standard ◽  
Accelerated Solvent Extraction ◽  
Experimental Result ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

AbstractThe aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 μg/kg. The quantification limit of the method was 10 μg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.

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