摘要
采用液相色谱-电喷雾串联质谱仪（LC-ESIMS/MS）,在多反应监测（MRM）模式下建立了动物尿液中15种甾类同化激素（睾酮、孕酮、诺龙、甲基睾酮、丙酸睾酮、丙酸诺龙、苯丙酸诺龙、大力补、勃地龙、群勃龙、康力龙、醋酸群勃龙、甲炔诺酮、甲羟孕酮、醋酸甲羟孕酮）的快速确证测定方法。试样经酶解处理后,过C18固相萃取柱净化,氮吹至干,残余物用0.50 mL乙腈-水（体积比1∶1）溶解后测定。采用正离子扫描方式进行仪器方法学研究,确定监测离子对,进行MRM模式定性定量分析。该方法的检出限（LOD）为0.2～0.5μg/L,定量下限（LOQ）为0.5～1.0μg/L;在2.0～200.0μg/L范围内线性关系良好,相关系数均大于0.998。在1.0、5.0μg/L的添加水平上,上述15种激素的平均回收率为59%～118%,相对标准偏差为1.0%～11.2%。该法操作简单,灵敏度高,可用于动物尿液中15种甾类同化激素的测定。
A liquid chromatography - mass spectrometry （ LC - MS/MS ） method for determination of 15 anabolic steroids （17β-TS, PG, 17β-NT, MTS, FFS, PN, PNT, DIA, BOL, TRE, STA, TRA, MED, NOG, MPA） in animal urines was established. After the treatment of enzyme hydrolysis, the sample was cleaned up by C18 solid-phase extraction（SPE）cartridges. The elution was evaporated under nitrogen and redissolved by acetontrile -water（1 ： 1, by volume）. The target analytes were determined by LC -MS/MS in multiple reaction monitoring（MRM） mode. The limits of detection （LODs） were range of 0.2 -0.5 μg/L, and the limits of quantitation（LOQs） were 0.5 -1.0 μg/L. The regression equations were linear between 2.0 and 200.0 μg/L for these drugs with correlation coefficient of more than 0. 998. The recoveries from the spiked sample at level of 1.0, 5.0 μg/L ranged from 59% to 118% with RSD（n = 5） of 1.0% - 11.2% . The method was simple, sensitive and rapid, and could be used for simultaneous determination of 15 anabolic steroids in animal urines.
出处
《分析测试学报》
CAS
CSCD
北大核心
2008年第12期1308-1312,共5页
Journal of Instrumental Analysis
基金
浙江重大科技攻关项目资助(2006C12025)
浙江重点科技攻关项目资助(2005C22029)
