Jindal S P, Lutz T, Vestergaard P
Biomed Mass Spectrom. 1978 Dec;5(12):658-63. doi: 10.1002/bms.1200051205.
A gas chromatographic mass spectrometric assay has been developed for the determination of cocaine and its pharmacologically active metabolite, norcocaine, in human urine. [2H3]Cocaine and [2H3]norcocaine were used as internal standards. The assay utilizes selective focusing to monitor in a gas chromatographic effluent the molecular ions of cocaine, [2H3]cocaine and the fragment ions of trifluoroacetylated norcocaine, [2H3]norcocaine generated by electron impact ionization. The assay can measure 2 ng ml-1 each of cocaine and norcocaine with about 5% precision. The curves, relating the amounts of cocaine and norcocaine added to control urine per 'fixed' amounts of their labeled analogs, versus the appropriate ion intensity ratios are straight lines with nearly zero intercepts and slopes of 0.98 +/- 0.01 and 0.98 +/- 0.02, respectively. The methodology is used for the analysis of urinary cocaine and norcocaine from three human subjects who received 100 mg cocaine-HCL intravenously.
已开发出一种气相色谱 - 质谱分析法,用于测定人尿液中的可卡因及其药理活性代谢物去甲可卡因。[2H3]可卡因和[2H3]去甲可卡因用作内标。该分析方法利用选择性聚焦,在气相色谱流出物中监测可卡因、[2H3]可卡因的分子离子以及电子轰击电离产生的三氟乙酰化去甲可卡因、[2H3]去甲可卡因的碎片离子。该分析方法可精确测定可卡因和去甲可卡因各2 ng ml-1,精密度约为5%。在对照尿液中,每‘固定’量的标记类似物所添加的可卡因和去甲可卡因量与相应离子强度比的曲线为直线,截距近零,斜率分别为0.98±0.01和0.98±0.02。该方法用于分析三名静脉注射100 mg盐酸可卡因的人体受试者尿液中的可卡因和去甲可卡因。