CLC number: S859
On-line Access: 2011-06-07
Received: 2010-08-14
Revision Accepted: 2010-12-09
Crosschecked: 2011-05-10
Cited: 4
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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.
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