猪尿中26种性激素与13种β_2-激动剂的同时测定  

Determination of Sex Hormones and β_2-Agonists Multi-residue in Porcine Urine by Gas Chromatography-Mass Spectrometry Method

作　　者：湛嘉[1,2] 俞雪钧[1] 李佐卿[1] 谢东华[1] 黄绍棠[1] 樊苑牧[1] 陈树兵[1] 彭锦峰[1] 

机构地区：[1]宁波出入境检验检疫局,浙江宁波315012 [2]浙江大学理学院,浙江杭州310028

出　　处：《分析测试学报》2009年第10期1133-1137,共5页Journal of Instrumental Analysis

基　　金：宁波市科技资助项目(2004C100020)

摘　　要：采用GC-MS对猪尿中26种性激素和13种β2-激动剂进行检测。尿样经β-葡糖苷酸酶水解后,用正己烷、MCX小柱和NH2小柱提取和净化性激素,并由七氟丁酸酐进行衍生,β2-激动剂由同支MCX小柱提取和净化,并用BSTFA衍生。性激素和激动剂的检出限均为0.25-1.0μg/kg。性激素的3个添加水平的平均回收率为86%-108%,相对标准偏差为8.8%-20.6%;β2-激动剂的3个添加水平的平均回收率为86%-108%,相对标准偏差为9.6%-16.1%。方法实现了对极性差异大和酸碱性相反的两类禁用化合物的同时测定,且前处理简便高效。A highly sensitive, specific method for the simultaneous determination of 26 sex hormones and 13/32-agonists in urine of pig was developed by gas chromatography- mass spectrometry（ GC - MS）. Urine samples were deconjugated by Helix pomatia juice, then extracted and purified by hexane, MCX and NH2 solid phase extraction column, sequencely. The extracts were derivatized with heptafluorobutyric anhydride. And β2 -agonists were extracted and purified by the same MCX solid phase extraction column, then were derivatized with BSTFA. The detection limits for all analytes were in the range of 0.25 - 1.0 μg · kg^-1. The average recoveries of sex hormones and β2-agonists were both in the range of 86% - 108%. Their relative standard deviations（RSDs） were in the range of 8.8% -20.6% , and 9.6% - 16. 1% , respectively. The method could be applied in the determination of sex hormones and 13 β2-agonists with high efficiency and simple sample preparation.

关 键 词：性激素 β2-激动剂 气相色谱-质谱 猪尿 

分 类 号：O657.7[理学—分析化学] R977.12[理学—化学]