固相萃取-气相色谱-质谱联用法测定人尿中11种蛋白同化激素  

GC-MS Determination of 11 Anabolic Steroids in Human Urine with Solid-Phase Extraction

作　　者：张卓旻[1,2] 上官良敏[1,2] 刘薇[3] 张兰[1,3] 

机构地区：[1]食品安全分析与检测教育部重点实验室(福州大学),福州350002 [2]福州大学化学化工学院,福州350002 [3]福州大学测试中心,福州350002

出　　处：《理化检验（化学分册）》2008年第9期810-814,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：福建省自然科学基金资助项目(B0510006);福州大学人才基金资助项目(0041826260;0041826486);"高校新世纪优秀人才支持计划"资助项目。

摘　　要：建立了固相萃取(SPE)-气相色谱-质谱联用(GC-MS)同时测定尿样中11种蛋白同化激素的分析方法,并将该方法用于美雄酮(MADE)阳性尿的分析。尿样前处理采用含500mg填料的C_(18) SPE柱净化浓缩,然后进行酶解,最后由液-液萃取获得待测样品。为了提高灵敏度,待测样品采用硅烷化衍生后进行GC-MS分析。在选择离子监测(SIM)模式下,采用甲睾酮(MT)为内标进行定量分析,方法检出限为0.1～2.0μg·L^(-1);分析加标实际样品,回收率在70.5%～121%,相对标准偏差为1.1%～13.9%。Hyphenated GC-MS was applied to the simultaneous determination of 11 anabolic steroids in human urine. Urine sample was treated with C18 solid phase extraction （SPE） column to purify and concentrate the analytes. The eluate from the SPE column was evaporated to dryness and enzymehydrolyzed in PBS of ca. pH 7, extracted with tert. butyl methyl ether, and dried by blowing with nitrogen. To improve sensitivity of determination, prederivatization of the sample solution with silane was performed. GC-MS determination was carried out using methyl testosterone as internal standard and with the SIM mode. Detection limits （S/N= 3） obtained were in the range of 0. 1--2. 0 μg ·L^-1. Tests for recovery and precision were made on the base of substantial samples, and values of average recovery found were in the range of 70. 5%--121.0%, and values of RSD＇s （n=5） were in the range from 1.1 % to 13. 9 %.

关 键 词：气质联用 固相萃取 蛋白同化激素 人尿 

分 类 号：O657.37[理学—分析化学]