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.

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 Diclazuril in Avian Feed and Premixes with Gas Chromatography/Mass Spectrometry

1994 ◽  
Vol 77 (5) ◽  
pp. 1061-1065 ◽  
Author(s):  
W John Blanchflower ◽  
Peter J Hughes ◽  
Andrew Cannavan ◽  
D Glenn Kennedy
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Internal Standard ◽  
Gas Chromatography Mass Spectrometry ◽  
Simple Liquid ◽  
Chromatography Mass Spectrometry ◽  
Coefficients Of Variation ◽  
Ethereal Diazomethane ◽  
Inclusion Rate

Abstract A method is presented for the determination of the relatively new anticoccidial drug diclazuril in avian feed and premixes. The drug was extracted from feed with acidified methanol-water, and the extracts were cleaned up by simple liquid-liquid extraction. These were then derivatized with ethereal diazomethane, and the methyl derivatives were analyzed by gas chromatography/mass spectrometry on a bench-top instrument An internal standard was used to enhance the reproducibility and ruggedness of the assay. The coefficients of variation for a finished feed and premix assayed 5 times each on 3 occasions were 6.6 and 6.0%, respectively. The detection limit of the assay is about 0.02 mg/kg, which is adequate for measuring the normal inclusion rate of 1 mg/kg in finished feed.

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 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.

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