Kintz P, Cirimele V, Sengler C, Mangin P
Institut de Médecine Légale, Strasbourg, France.
J Anal Toxicol. 1995 Oct;19(6):479-82. doi: 10.1093/jat/19.6.479.
A method using gas chromatography coupled to mass spectrometry for the determination of the cocaine (COC) pyrolysis product, anhydroecgonine methyl ester (AEME), in urine and hair is described. The same procedure allows the simultaneous determination of COC, benzoylecgonine (BZE), ecgonine methyl ester, and cocaethylene. The assay involves acid hydrolysis for hair, deuterated internal standards, a three-step liquid-liquid extraction, and derivatization with N,O-bis(trimethylsilyl) trifluoroacetamide plus 1% trimethylchlorosilane. Detector responses for analytes were linear over the concentration ranges of 0.2-50 ng/mg and 10-2000 ng/mL for hair and urine, respectively. Artifact formation of AEME during the injection was less than 1%. AEME was tested in 65 and 81 cases for hair and urine, respectively, where COC or BZE or both tested positive. Concentrations of AEME ranged from 0.2 to 2.4 ng/mg (n = 7) and from 4 to 226 ng/mL (n = 12) in hair and urine, respectively. Its presence was observed in few cases, clearly indicating that COC smoking is not frequent in France.
描述了一种使用气相色谱-质谱联用技术测定尿液和毛发中可卡因(COC)热解产物脱水芽子碱甲酯(AEME)的方法。相同的程序可同时测定COC、苯甲酰芽子碱(BZE)、芽子碱甲酯和古柯乙烯。该分析方法包括对毛发进行酸水解、使用氘代内标、三步液-液萃取以及用N,O-双(三甲基硅基)三氟乙酰胺加1%三甲基氯硅烷进行衍生化。毛发和尿液中分析物的检测器响应在浓度范围分别为0.2 - 50 ng/mg和10 - 2000 ng/mL时呈线性。进样过程中AEME的假象形成小于1%。分别在65例毛发和81例尿液样本中对AEME进行了检测,这些样本中COC或BZE或两者检测均呈阳性。毛发和尿液中AEME的浓度分别为0.2至2.4 ng/mg(n = 7)和4至226 ng/mL(n = 12)。在少数案例中观察到其存在,这清楚表明在法国吸食COC的情况并不常见。