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

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.

1994 ◽  
Vol 77 (4) ◽  
pp. 917-924 ◽  
Author(s):  
Roger T Wilson ◽  
Joseph M Groneck ◽  
Kathleen P Holland ◽  
A Carolyn Henry

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.


Author(s):  
Cuicui Kang ◽  
Haijian Ma ◽  
Yuan Li ◽  
Chizhong Zhang ◽  
Yueqin Hong ◽  
...  

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.


2016 ◽  
Vol 13 (4) ◽  
pp. 341-347
Author(s):  
Wei Gao ◽  
Naiying Wu ◽  
Wenliang Sun

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.


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