唾液中鸦片类毒品的衍生化GC/MS-SIM分析研究  

GC/MS-SIM study of opiates in saliva after derivatization

作　　者：王燕燕[1] 孟品佳[1] 王川[1] 王彦吉[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：《药物分析杂志》2010年第9期1658-1663,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：北京教育委员会共建项目建设计划;项目编号SYS1004100436

摘　　要：目的:建立灵敏度高、重复性好、操作简便的唾液中鸦片类毒品的硅烷化和酰化GC/MS-SIM检测方法。方法:以乙基吗啡为内标,用混合溶剂氯仿-异丙醇-正庚烷(50∶33∶17)对添加吗啡、可待因和6-单乙酰吗啡的唾液进行提取后,经MB-TFA或MSTFA衍生化,采用气相色谱/质谱-选择离子法(GC/MS-SIM)检测。结果:添加吗啡、可待因和6-单乙酰吗啡的唾液药物浓度在10～1000ng·mL-1范围内均获得了良好的线性(r>0.99),3种成分日内精密度试验的RSD均在16%以内,提取回收率均在80%～120%之间,最小定量限均为10ng·mL-1,最小检测限MSTFA衍生化吗啡和可待因为1ng·mL-1、6-单乙酰吗啡为0.5ng·mL-1,MBTFA衍生化吗啡为0.5ng·mL-1、可待因和6-单乙酰吗啡为2ng·mL-1;采用该方法对服用治疗剂量的甘草片(内含无水吗啡成分)者的唾液检材进行检测,检测出吗啡。结论:该方法操作简单,灵敏度高,稳定可靠,可用于对吸毒者唾液中鸦片类毒品的检测和分析。Objective：To establish a simple and reliable method in which use gas chromatography/mass spectrometry-selected ion monitoring（GC/MS-SIM） after silylation and acetylation for identifying and quantifying opiates including morphine,6-acetylmorphine and codeine in human saliva. Methods：Using ethyl morphine as an internal standard,morphine,6-acetylmorphine and codeine spiked in blank saliva were extracted with a mixed solvent of chloroform-isopropyl alcohol-n-heptane（50：33：17）. The extracts were evaporated to dryness followed by being derivatized with MSTFA or MBTFA,and then it was analyzed directly by GC/MS in selected ion mode. Results：The method was validated in the range 10-1000 ng·mL-1 with the drug-spiked saliva,the reactor responded linearly over the studied range（r0.99 for the 3 drugs）; RSDs of intra-day precision test were less than 16%,the extraction recoveries were varying from 80% to 120%;the LODs were 1 ng·mL-1 for morphine and codeine,and 0.5 ng·mL-1 for 6-acetylmorphine,respectively after MSTFA derivatization;While for MBTFA derivatization,the LODs were 2 ng·mL-1 for both codeine and 6-acetylmorphine,and 0.5 ng·mL-1 for morphine,respectively.Saliva after administering a therapy dose of cough drop was collected from a healthy male volunteer and analyzed with the established method,in it morphine was detected.Conclusion：It is showing that the method can be applied in detecting trace amount of opiates in human saliva.

关 键 词：唾液 鸦片类毒品 衍生化 GC/MS-SIM 

分 类 号：R917[医药卫生—药物分析学]