| Articles |
|
|
|
|
| Analysis of 19-nortestosterone residue in animal tissues by ion-trap gas chromatography-tandem mass spectrometry |
| 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 |
| 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 |
|
|
|
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.
|
|
Received: 14 August 2010
Published: 07 June 2011
|
|
|
|
Cite this article:
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. Journal of Zhejiang University-SCIENCE B (Biomedicine & Biotechnology), 2011, 12(6): 460-467.
URL:
http://www.zjujournals.com/xueshu/zjus-b/10.1631/jzus.B1000301 OR http://www.zjujournals.com/xueshu/zjus-b/Y2011/V12/I6/460
|
|
Viewed |
|
|
|
Full text
|
|
|
|
|
Abstract
|
|
|
|
|
Cited |
|
|
|
|
| |
Shared |
|
|
|
|
| |
Discussed |
|
|
|
|
