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 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.

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.

Simultaneous determination of furan and its derivatives in food by headspace gas chromatography-mass spectrometry (HS-GC-MS)

2021 ◽  
Vol 4 (3) ◽  
pp. 13-23
Author(s):  
Ha Binh Nguyen Thi ◽  
Cao Tien Bui ◽  
Ngoc Anh Mai Thi ◽  
Hoai Pham Thi ◽  
Hong Hao Le Thi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Internal Standard ◽  
Food Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Powdered Milk ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A method for the simultaneous determination of furans, 2-methylfuran and 3-methylfuran in some food by gas chromatography-mass spectrometry (GC-MS) has successfully developed. Analysed samples were treated by a headspace technique using furan-d4 as an internal standard. The detection limit of the method is 0.3 µg/kg, the quantitative limit of the method is 1.0 µg/kg. The recovery of the method is in the range of 72 to 110%. The relative standard deviation ranges from 3.3 to 13%. The method was applied to analyze 100 food samples, including: coffees, canned meats, baby foods, powdered milk. The results showed that furans, 2-methylfuran, 3-methylfuran were detected in 30 samples out of 100 collected samples. In particular, furans were found in a ranges of 5.7 to 2803 µg/kg in all of coffee samples, including instant coffee and roasted coffee. In addition, furans were detected in one baby food sample contains, furans and 2-methylfuran in four canned meat samples, and no furans milk were detected in powder sample among 25 analysed samples.

scholarly journals Determination of 1,3-Dichloropropanol in Soy Sauce and Related Products by Headspace Gas Chromatography with Mass Spectrometric Detection: Interlaboratory Study

2005 ◽  
Vol 88 (5) ◽  
pp. 1404-1412 ◽  
Author(s):  
Sarah Hasnip ◽  
Colin Crews ◽  
Nicholas Potter ◽  
Paul Brereton ◽  
Henri Diserens ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Soy Sauce ◽  
Headspace Gas Chromatography ◽  
Relative Standard ◽  
Headspace Gas

Abstract An interlaboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96–130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9–23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9–35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

Determination of Pyrantel in Swine Liver by Flame Ionization Gas Chromatography and Confirmation by Gas Chromatography /Mass Spectrometry

1990 ◽  
Vol 73 (6) ◽  
pp. 883-886
Author(s):  
Susan S.C Tai ◽  
Nancy Cargile ◽  
Charlie J Barnes ◽  
Philip Kijak
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Tissue Samples ◽  
Flame Ionization ◽  
Chromatography Mass Spectrometry ◽  
Ionization Method ◽  
Swine Liver

Abstract During an evaluation of the gas chromatography/mass spectrometry (GC/MS) confirmatory procedure of Lynch and Bartoluccl for pyrantel residues in swine tissues, we developed a GC flame Ionization method for quantltatlng pyrantel residues In extracts of swine liver. The method was subjected to trial principally In the laboratories of Biospherics, Inc., using control liver, fortified control liver, and Incurred liver tissue samples. Although the method does not meet all of the current Food and Drug Administration criteria, it compares favorably to the official determinative method. Portions of the same extract can be used for quantitation and for GC/MS confirmation, true recoveries appear to be slightly higher, and an internal standard Is not required. The precision of this method equals or exceeds that of the official determinative method.

scholarly journals Determination of Se4+ in Drinkable Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry

2000 ◽  
Vol 83 (5) ◽  
pp. 1082-1086 ◽  
Author(s):  
Maurizio Guidotti
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Tap Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Drinkable Water

Abstract A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1′-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)–SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 μg/L concentration, the relative standard deviation was 10.1% for HS–SPME and 9.1% for direct SPME. For HS–SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water 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.

scholarly journals Determination of Hexabromocyclododecane in Expanded Polystyrene and Extruded Polystyrene Foam by Gas Chromatography-Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7143
Author(s):  
Tianao Mao ◽  
Haoyang Wang ◽  
Zheng Peng ◽  
Taotao Ni ◽  
Tianqi Jia ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase ◽  
Expanded Polystyrene ◽  
Gas Chromatography Mass Spectrometry ◽  
Polystyrene Foam ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Extruded Polystyrene Foam

A gas chromatography-mass spectrometry (GC/MS) method for the determination of hexabromocyclododecane (HBCD) in expanded polystyrene and extruded polystyrene foam (EPS/XPS) was developed. The EPS/XPS samples were ultrasonically extracted with acetone and the extracts were purified by filtration through a microporous membrane (0.22 μm) and solid-phase extraction. The samples were analyzed using a GC/MS using the selected ion monitoring mode. The ions 157, 319 and 401 were selected as the qualitative ions, while ion 239 was chosen as the quantitative ion. An HBCD standard working solution with a concentration range of 1.0–50.0 mg/L showed good linearity. The detection limit of HBCD was 0.5 mg/kg, meeting the LPC limit (<100 or 1000 mg/kg). Six laboratories were selected to verify the accuracy of the method, and 10 samples were tested. The interlaboratory relative standard deviation range was 3.68–9.80%. This method could play an important role in controlling HBCD contamination in EPS/XPS.

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