海洛因滥用者唾液中毒品代谢物的SPE-GC/MS-SIM分析  

Analysis of opiates in human saliva by solid-phase extraction and gas chromatography/mass spectrometry detection

作　　者：王燕燕[1] 孟品佳[1] 王彦吉[1] 王川[1] 李燕京[1] 

机构地区：[1]中国人民公安大学刑事科学技术系,北京100038

出　　处：《化学研究与应用》2010年第4期415-419,共5页Chemical Research and Application

基　　金：北京教育委员会共建项目建设计划(SYS1004100436)资助

摘　　要：本文首先考查了不同类型不同厂家的固相萃取柱的萃取效果,采用提取效果较好的50 mg/mL的Clean-screen CSDAUL01混合型强阳离子固相萃取柱,对唾液中的吗啡、可待因、6-单乙酰吗啡等3种鸦片类毒品进行提取后,将提取液吹干;再经MBTFA衍生化后,进行GC/MS-SIM检测。以乙基吗啡为内标,3种毒品的线性相关系数均大于0.99,线性范围为10～1000 ng/mL,相对回收率分别为85%～110%、94%～107%和75%～92%;相对标准偏差小于10%。3种毒品的检测限分别为2 ng/mL、1 ng/mL和2 ng/mL。该方法灵敏度高、重现性好、操作简便,可用于鸦片类毒品滥用者及中毒者唾液中的毒品及其代谢物的检测。In this paper, some solid-phase extraction columns in different types and from different manufacturers were tested, the better one among them with mixed strong cation exchange column（50 mg/mL of Cleanscreen CSDAUL01 ） was chosen to extract morphine ,codeine and 6-acetyl morphine which spiked in saliva. Using ethyl morphine as an internal standard ,and the 3 opiates spiked in blank saliva were extraeted using a solid-phase cartridge, followed by being derivatized with MBTFA, and analyzed directly by GC/MS in selected ion mode. The method was validated in the range 10 - 1000 ng/mL with the drug-spiked saliva,the reactor responded linearly over the studied range（ R^2 〉 0. 99 for the 3 drugs） ;The relative standard deviations（RSD） were less than 15% , the relative extraction recoveries were varying from 75% to 110% , and LODs were less than 2 ng/mL, which promised the perspective application of the method in detecting trace amount of opium in human saliva.

关 键 词：海洛因 唾液 SPE提取 GC/SIM—MS检测 

分 类 号：O657.7[理学—分析化学]