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Journal of Zhejiang University SCIENCE B 2011 Vol.12 No.6 P.460-467

http://doi.org/10.1631/jzus.B1000301


Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry


Author(s):  Jin-qing Jiang, Lei Zhang, Guang-ling Li, Hai-tang Zhang, Xue-feng Yang, Jun-wei Liu, Ren-feng Li, Zi-liang Wang, Jian-hua Wang

Affiliation(s):  College of Veterinary Medicine, Northwest A&F University, Yangling 712100, China, College of Animal Science, Henan Institute of Science and Technology, Xinxiang 453003, China, College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003, China

Corresponding email(s):   wangzl_2008@yahoo.com.cn, jhwang1948@sina.com

Key Words:  19-Nortestosterone (19-NT), Gas chromatography-tandem mass spectrometry (GC-MS), Animal tissues


Jin-qing Jiang, Lei Zhang, Guang-ling Li, Hai-tang Zhang, Xue-feng Yang, Jun-wei Liu, Ren-feng Li, Zi-liang Wang, Jian-hua Wang. Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry[J]. Journal of Zhejiang University Science B, 2011, 12(6): 460-467.

@article{title="Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry",
author="Jin-qing Jiang, Lei Zhang, Guang-ling Li, Hai-tang Zhang, Xue-feng Yang, Jun-wei Liu, Ren-feng Li, Zi-liang Wang, Jian-hua Wang",
journal="Journal of Zhejiang University Science B",
volume="12",
number="6",
pages="460-467",
year="2011",
publisher="Zhejiang University Press & Springer",
doi="10.1631/jzus.B1000301"
}

%0 Journal Article
%T Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry
%A Jin-qing Jiang
%A Lei Zhang
%A Guang-ling Li
%A Hai-tang Zhang
%A Xue-feng Yang
%A Jun-wei Liu
%A Ren-feng Li
%A Zi-liang Wang
%A Jian-hua Wang
%J Journal of Zhejiang University SCIENCE B
%V 12
%N 6
%P 460-467
%@ 1673-1581
%D 2011
%I Zhejiang University Press & Springer
%DOI 10.1631/jzus.B1000301

TY - JOUR
T1 - Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry
A1 - Jin-qing Jiang
A1 - Lei Zhang
A1 - Guang-ling Li
A1 - Hai-tang Zhang
A1 - Xue-feng Yang
A1 - Jun-wei Liu
A1 - Ren-feng Li
A1 - Zi-liang Wang
A1 - Jian-hua Wang
J0 - Journal of Zhejiang University Science B
VL - 12
IS - 6
SP - 460
EP - 467
%@ 1673-1581
Y1 - 2011
PB - Zhejiang University Press & Springer
ER -
DOI - 10.1631/jzus.B1000301


Abstract: 
A rapid sample treatment procedure for the gas chromatography-tandem mass spectrometry (GC-MS) determination of 19-Nortestosterone (19-NT) in animal tissues has been developed. In our optimized procedures, enzymatic hydrolysis with β-glucuronidase from Escherichia coli was performed in an acetate buffer (pH 5.2, 0.2 mol/L). Next, the homogenate was mixed with methanol and heated at 60 °C for 15 min, then placed in an ice-bath at −18 °C for 2 h. After liquid-liquid extraction with n-hexane, the analytes were subjected to a normal-phase solid phase extraction (SPE) C18 cartridge for clean-up. The dried organic extracts were derivatized with heptafluorobutyric anhydride (HFBA), and then the products were injected into GC-MS. Using electron impact mass spectrometry (EI-MS) with positive chemical ionization (PCI), four diagnostic ions (m/z 666, 453, 318, and 306) were determined. A standard calibration curve over the concentration range of 1–20 ng/g was reached, with Y=467084X−68354 (R2=0.9997) for 19-NT, and the detection limit was 0.3 ng. When applied to spiked samples collected from bovine and ovine, the recoveries ranged from 63% to 101% with relative standard deviation (RSD) between 2.7% and 8.9%. The procedure is a highly efficient, sensitive, and more economical method which offers considerable potential to resolve cases of suspected nandrolone doping in husbandry animals.

Darkslateblue:Affiliate; Royal Blue:Author; Turquoise:Article

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