固相萃取-LC-MS/MS法同时测定污水中苯丙胺和甲基苯丙胺

Simultaneous determination of amphetamine and methamphetamine in wastewater by solid-phase extraction-liquid chromatography-tandem mass spectrometry

目的:建立一种采用固相萃取-液相色谱-串联质谱法同时检测污水中苯丙胺和甲基苯丙胺的定性定量方法。方法:采用固相萃取法对污水前处理,以Agilent ZORBAX Eclipse C18为液相色谱柱,乙腈-0.1%甲酸水溶液为流动相,1.0mL·min^-1流速进行梯度洗脱;以电喷雾电离(ESI+),多反应监测模式(MRM)采集信号,内标-校准曲线法定量。结果:苯丙胺和甲基苯丙胺均在2.5ng·L^-1~500 ng·L^-1浓度范围内呈良好的线性关系,相关系数均大于0.99,日内精密度和日间精密度均在4%以下,回收率在88.4%~104.5%。结论:该方法简单快速,回收率高、重现性好,适用于污水中苯丙胺和甲基苯丙胺的检测,为客观地、实时地监测毒品滥用情况提供重要技术支持。

Objective:A method was established to simultaneous determination of amphetamine and methamphetamine in wastewater by solid-phase extraction-liquid chromatography-tandem mass spectrometry(SPE-LC-MS/MS).Methods:Solid-phase extraction was used to deal with wastewater samples.The analytes were separated on Agilent ZORBAX Eclipse C18 by a gradient elution with acetonitrile-0.1%methanoic acid aqueous solution as mobile phase at a flow rate of 1.0 mL/min.A mass spectrometry was equipped with electrospray ionization(ESI)source in the positive ion mode.Signal was collected in multiple reaction monitoring mode(MRM).The quantitative analysis was on the basis of internal standard-calibration curve.Results:The linear range was 2.5 ng/L-500 ng/L for the analysis of amphetamine and methamphetamine(r>0.99).In addition,the intra and inter-day relative standard deviations were lower than 4%.The recovery rate was 88.4%-104.5%.Conclusion:The established method is simple and rapid,and has high recovery rate and a good reproducibility,which is fit for analysis of amphetamine and methamphetamine in wastewater and can provide important technical supports for objective and real-time monitoring of drug abuse.