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.

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.

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.

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.

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