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  

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

作　　者：林维宣[1] 董伟峰[1] 陈溪[1] 田苗[1] 于灵[1] 赵景红[1] 杨春光[1] 

机构地区：[1]辽宁出入境检验检疫局,辽宁大连116001

出　　处：《色谱》2009年第3期294-298,共5页Chinese Journal of Chromatography

基　　金：国家质量监督检验检疫总局立项课题(课题编号:2002IK042)

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0.1～1μg/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。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.

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

分 类 号：O658[理学—分析化学]