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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
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
