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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 silanization and acylation GC / MS-SIM method for determination of opiate drugs in saliva with high sensitivity, good repeatability and easy operation. Methods: Ethyl morphine was used as an internal standard to extract the saliva of morphine, codeine and 6-monoacetylmorphine by chloroform-isopropanol-n-heptane (50:33:17) -TFA or MSTFA derivatized with gas chromatography / mass spectrometry-selective ionization (GC / MS-SIM). RESULTS: The saliva concentrations of morphine, codeine and 6-monoacetylmorphine were all good linearity (r> 0.99) in the range of 10-1000 ng · mL-1. The RSDs of intra-day precision test Within 16%, the recovery rates were between 80% and 120%, the minimum limit of quantification was 10 ng · mL-1, the minimum detectable limit of MSTFA derivatized morphine and codeine was 1 ng · mL-1, 6-monoacetyl Morphine was 0.5ng · mL-1, 0.5ng · mL-1 morphine was derivatized with MBTFA, 2ng · mL-1 codeine and 6-monoacetylmorphine. With this method, Anhydrous morphine component) were detected in saliva samples to detect morphine. Conclusion: The method is simple, sensitive, reliable and can be used to detect and analyze opiate drugs in saliva of drug addicts.