Cone E J, Hillsgrove M, Darwin W D
Addiction Research Center, National Institute on Drug Abuse, Baltimore, MD 21224.
Clin Chem. 1994 Jul;40(7 Pt 1):1299-305.
We developed a sensitive and specific assay for the simultaneous measurement of cocaine, cocaethylene, six of their metabolites, and anhydroecgonine methyl ester, a pyrolysis product, in biological fluids. The assay involves solid-phase extraction columns containing a copolymeric bonded phase for isolation of cocaine analytes, derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide and 10 g/L trimethylchlorosilane, and measurement with gas chromatography-mass spectrometry operating in the selected-ion monitoring mode. Detector responses for analytes were linear over a concentration range of 3.1-1000 micrograms/L. The limits of detection were approximately 1 microgram/L for cocaine, ecgonine methyl ester, and benzoylecgonine and 3-6 micrograms/L for the remaining analytes. Hydrolysis of cocaine and artifact formation of anhydroecogonine methyl ester during extraction and assay was < 1%. Cocaine and its derivatives appear in different proportions in plasma, saliva, and urine according to the biological fluid and time of measurement. Each biological fluid provides unique information on the disposition of cocaine in human subjects.
我们开发了一种灵敏且特异的检测方法，用于同时测定生物体液中的可卡因、可口卡因、它们的六种代谢物以及一种热解产物——脱水芽子碱甲酯。该检测方法包括使用含有共聚键合相的固相萃取柱来分离可卡因分析物，用N,O-双(三甲基硅基)三氟乙酰胺和10 g/L三甲基氯硅烷进行衍生化，以及采用在选择离子监测模式下运行的气相色谱-质谱联用仪进行测定。分析物的检测器响应在3.1 - 1000微克/升的浓度范围内呈线性。可卡因、芽子碱甲酯和苯甲酰芽子碱的检测限约为1微克/升，其余分析物的检测限为3 - 6微克/升。在提取和检测过程中，可卡因的水解以及脱水芽子碱甲酯的假象形成率<1%。根据生物体液和测量时间的不同，可卡因及其衍生物在血浆、唾液和尿液中的比例各异。每种生物体液都提供了关于可卡因在人体中处置情况的独特信息。
