液相色谱-串联质谱同时测定动物组织中22种同化激素  

Multi-residue Method for Detrmination of 22 Anabolic Hormones in Animal Tissues by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：陈慧华[1] 应永飞[1] 吴平谷[2] 韦敏珏[1] 朱聪英[1] 屈健[1] 陈熳茜 

机构地区：[1]浙江省畜产品质量安全检测中心,杭州310020 [2]浙江省疾病预防控制中心,杭州310051

出　　处：《分析化学》2009年第2期181-186,共6页Chinese Journal of Analytical Chemistry

基　　金：浙江省重大科技攻关项目(No.2006C12025);浙江省重点科技攻关项目(No.2005C22029)资助

摘　　要：采用高效液相色谱-电喷雾串联质谱仪(LC-ESI-MS-MS),在多反应监测(MRM)模式下建立了动物组织中甾体类和1,2-二苯乙烯类22种同化激素(睾酮、甲基睾酮、丙酸睾酮、苯丙酸诺龙、勃地龙、康力龙、群勃龙、醋酸群勃龙、丙酸诺龙、大力补、醋酸甲羟孕酮、诺龙、孕酮、甲炔诺酮、甲羟孕酮、雌酮、雌二醇、雌三醇、炔雌醇、己烷雌酚、己烯雌酚、双烯雌酚)的快速确认测定方法。试样中的药物经叔丁基甲醚提取后,过C18固相萃取柱净化,氮吹至干,用1mL乙腈/水(1∶1,V/V)定容后测定。采用正离子扫描和负离子扫描的方式进行仪器方法学研究,确定丰度比最高的2对离子作为监测离子,进行MRM模式定性定量分析。该方法的检出限(LOD)为0.2～0.5μg/kg,定量限(LOQ)为0.5～1.0μg/kg;在2.0～200.0μg/L的线性范围,相关系数r均大于0.998。在1.0μg/kg的添加水平上,上述22种激素的平均回收率为56.2%～112.3%,相对标准偏差为2.6%～13.2%。本法操作简单,灵敏度高,可用于动物组织中22种同化激素的残留测定。A liquid chromatography-mass spectrometric （LC-ESI-MS/MS）method for the determination of multi-residues of 22 anabolie steroids （17β-TS, MTS, PTS, PNT, BOL, STA, TRE, TRA, PN, DIA, MPA, 17β-NT, PG, NOG, MED, 17β-ES, EST, ESN, EES） and 1, 2-stilbenes （HES, DES, DIS） in animal tissues was reported. The drugs were extracted with methyl tertiary butyl ether （MTBE） from analyte, then extraction was evaporated at 50℃ by nitrogen blow. After the residue was dissolved in methanol/water （20：80）, it was purified by passing through C 18 solid-phase extraction （SPE）cartridges. The elution was evap- orated by nitrogen blow , dissolved in acetonitrile/water （1 ： 1） and then assayed by LC-MS/MS. The limits of detection（LOD） were 0.2 -0.5 μg/kg, and the limits of quantitation（LOQ） were 0.5 - 1.0 μg/kg. The calibration curves were linear between 2. 0 to 200.0 μg/L for these drugs. Recoveries were 56. 2% - 112.3%, and the inter-relative standard deviation （ n = 5 ） was 2. 6% - 13. 2%, at spiked levels of 1.0 μg/kg. The method has merits of simplicity, sensitivity and rapidity and hence can be used for simultaneous determination of anabolic hormones in animal tissues.

关 键 词：液相色谱-串联质谱法 同化激素 甾体类激素 1 2-二苯乙烯类 动物组织 

分 类 号：Q954.6-3[生物学—动物学]