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本实验旨在建立豚鼠毛发中可卡因及其代谢物苯甲酰爱康宁的液相色谱-串联质谱分析方法,并考察单次给药后豚鼠毛发中可卡因和苯甲酰爱康宁的质量浓度。毛发洗涤、晾干后剪成1～2 mm小段,取20 mg,加入0.1mol.L-1HCl 1 mL和内标溶液(50 ng.mL-1d3-可卡因和d8-苯甲酰爱康宁)20μL,50℃水浴中酸水解过夜;调pH为中性,用二氯甲烷液液提取,移取有机相于60℃水浴下挥干,用甲醇100μL复溶,进样5μL。目标化合物用Allure PFP丙基柱分离,以甲醇-20 mmol.L-1乙酸铵(0.1%甲酸)(80∶20)为流动相。质谱采用电喷雾电离-正离子模式(ESI+),多反应监测模式(MRM)。动物实验:豚鼠8只分两组,分别以10和0.4 mg·kg-1的剂量腹腔注射盐酸可卡因水溶液一次,在给药后d 7和d 14分色剃取毛发进行检测。结果显示,毛发中可卡因和苯甲酰爱康宁的最低检出限均为1 pg.mg-1,在5～250 pg.mg-1线性良好(r2≥0.999 7)。在给药后d 7收集的豚鼠毛发中同时检测到可卡因和苯甲酰爱康宁;d 14收集的毛发中只检测到可卡因。所建LC-MS/MS法灵敏度高,特异性强,适用于豚鼠毛发中低质量浓度的可卡因和苯甲酰爱康宁的分析。
The purpose of this experiment was to establish a method for the determination of cocaine and its metabolite benzoylcodonquine in guinea pig hair by liquid chromatography-tandem mass spectrometry and investigate the mass concentration of cocaine and benzoyl icarin in guinea pig hair after a single dose. Hair wash, dry cut into small pieces of 1 to 2 mm, take 20 mg, add 0.1mol.L-1HCl 1mL and internal standard solution (50 ng.mL-1d3-cocaine and d8-benzoyl Ikaron) 20μL , Acid hydrolysis in water bath overnight at 50 ℃; pH was neutral, extracted with dichloromethane liquid, the organic phase was removed and evaporated to dryness under water bath at 60 ℃, reconstituted with 100μL methanol, into the sample 5μL. The target compound was isolated with Allure PFP propyl column using methanol-20 mmol.L-1 ammonium acetate (0.1% formic acid) (80:20) as the mobile phase. Mass spectrometry was electrospray ionization-positive ion mode (ESI +), multiple reaction monitoring mode (MRM). Animal experiments: 8 guinea pigs were divided into two groups. The mice were injected intraperitoneally with 10 and 0.4 mg · kg-1 of cocaine hydrochloride aqueous solution once a day, respectively. The guinea pigs were shaved and dyed at d 7 and d 14 after dosing. The results showed that the minimum detectable limit of cocaine and benzoyl icanine in hair was 1 pg.mg-1, and the linearity was good at 5 ~ 250 pg.mg-1 (r2≥0.9997). Cocaine and benzoyl icarine were detected simultaneously in guinea pig hair collected on day d7 after dosing; only cocaine was detected in d14 collected hair. The established LC-MS / MS method has the advantages of high sensitivity and specificity, and is suitable for the analysis of cocaine and benzoyl icanine in low-quality guinea pig hair.