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目的:建立快速、准确的尿液中甲基苯丙胺(MA)、苯丙胺(AM)、3,4-亚甲基二氧基甲基苯丙胺(MDMA)、3,4-亚甲基二氧基苯丙胺(MDA)、3-甲氧基-4,5-亚甲基二氧基苯丙胺(MMDA)残留的分子印迹固相萃取(MISPE)高效液相色谱测定方法。方法:尿液经与醋酸铵缓冲液(pH 8.0)混合后通过离心分离(8000 rpm),上清液采用预先活化的分子印迹固相萃取小柱净化,以1.0%醋酸/乙腈(1/99,v/v)溶液进行洗脱,在XBridge RP18色谱柱上,以甲醇-乙腈-100 mmol/L醋酸铵水溶液为流动相进行梯度洗脱,采用215 nm波长进行检测。结果:MA、AM、MDMA、MDA、MMDA的加标回收率在88.0%~98.8%范围,其相对标准偏差均小于5.0%,5种待测物在0.05 mg/L~15.0 mg/L范围均呈现良好的线性,其回归系数大于0.999,最低定量检出限(LOQs)在0.017 mg/L~0.03 mg/L范围。结论:本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可满足临床吸毒病人尿液中MA、AM、MDMA、MDA和MMDA的残留检测要求。
OBJECTIVE: To establish a rapid and accurate method for the determination of methamphetamine (MA), amphetamine (AM), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA) and 3-methoxy-4, 5-methylenedioxypropylamine (MMDA) residues by high performance liquid chromatography (HPLC). METHODS: Urine was mixed with ammonium acetate buffer (pH 8.0) and centrifuged (8000 rpm). The supernatant was purified using a pre-activated molecularly imprinted solid-phase extraction cartridge and eluted with 1.0% acetic acid in acetonitrile , v / v). The elution was carried out on a XBridge RP18 column with gradient elution with methanol-acetonitrile-100 mmol / L ammonium acetate aqueous solution as the mobile phase. The detection wavelength was at 215 nm. Results The recoveries of MA, AM, MDMA, MDA and MMDA were all in the range of 88.0% ~ 98.8% with relative standard deviations (RSDs) less than 5.0%, and the five analytes were in the range of 0.05 mg / L ~ 15.0 mg / L Showed a good linearity, the regression coefficient was greater than 0.999, the lowest limit of detection (LOQs) in the range of 0.017 mg / L ~ 0.03 mg / L. Conclusion: The method has high recovery rate, significant purification effect, good stability and less impurity interference, which can meet the requirements of residue detection of MA, AM, MDMA, MDA and MMDA in urine of clinical drug users.