【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。更多还原

【Abstract】 A liquid chromatography-mass spectrometric(LC-ESI-MS/MS)method for the determination of multi-residues of 22 anabolic 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 C18 solid-phase extraction(SPE)cartridges.The elution was evaporated 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.更多还原