色谱

色谱

• 研究论文 • 上一篇    下一篇

气相色谱-质谱法同时检测动物组织中多种激素类兽药的残留量

林维宣*, 董伟峰, 陈溪, 田苗, 于灵, 赵景红, 杨春光   

  1. Liaoning Entry-Exit Inspection and Quarantine Bureau, Dalian 116001, China
  • 收稿日期:2008-10-20 修回日期:2008-12-22 出版日期:2009-05-30 发布日期:1982-09-25
  • 通讯作者: 林维宣

Determination of hormone multi-residues in animal tissues by gas chromatography-mass spectrometry

LIN Weixuan*, DONG Weifeng, CHEN Xi, TIAN Miao, YU Ling, ZHAO Jinghong, YANG Chunguang   

  1. Liaoning Entry-Exit Inspection and Quarantine Bureau, Dalian 116001, China
  • Received:2008-10-20 Revised:2008-12-22 Online:2009-05-30 Published:1982-09-25
  • Contact: LIN Weixuan

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955

被引次数

111

摘要： 建立了不同动物基质(肌肉、肝脏、肾脏)中己烷雌酚、己烯雌酚、己二烯雌酚、还原尿睾酮、表睾酮、雌酮、雌二醇、炔雌醇和雌三醇激素残留量的气相色谱-质谱联用(GC-MS)检测方法。以乙腈为提取溶剂,固相萃取柱净化,微波辅助衍生化,用双(三甲基硅烷基)三氟乙酰胺(BSTFA)与甲基氯硅烷(TMCS)(体积比为99 :1)的硅烷化试剂在吡啶存在下进行衍生化反应。实验结果表明,9种激素的检出限为0.1～1 μg/kg。3种动物基质中9种激素的平均回收率为68.8%～93.1%,实验室内相对标准偏差(RSD)为4.1%～22.3%,实验室间RSD为3.1%～17.9%。方法的技术指标满足动物组织中激素类兽药残留分析的要求。

关键词: 动物组织 , 多残留检测, 固相萃取, 激素, 气相色谱-质谱法, 兽药, 微波辅助衍生

Abstract: A method of gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of nine sex hormone residues, such as hexestrol, diethylstilbestrol, dienestrol, etiocholan-3α-ol-17-one, epitestosterone, estrone, estradiol, ethinylestradiol and estriol, in animal tissues was developed. The sex hormones were extracted with acetonitrile, then cleaned-up with a C18 solid-phase extraction (SPE) column. The microwave-assisted derivatization of the target components with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and trimethylchlorosilane (TMCS) (99:1, v/v) using pyridine as solvent was performed, and then the derivatives were analyzed by GC-MS. The limits of detection were 0.1~1 μg/kg for all hormones, and the limits of quantification were 0.2~2 μg/kg. The average recoveries of sex hormones were 68.8%~93.1%. The relative standard deviations (RSDs) of inter- and intra-assay were 4.1%~22.3% and 3.1%~17.9%, respectively. The real sample tests showed this method can be used for the sensitive and accurate determination of multi-sex hormones residues in biological samples.

Key words: animal tissues , hormones, microwave-assisted derivatization, multi-residue determination, solid-phase extraction (SPE), veterinary drugs, gas chromatography-mass spectrometry (GC-MS)