海洛因滥用者唾液中毒品代谢物的SPE-GC/MS-SIM分析

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。

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

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 extracted 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.