生物检材中苯丙胺类兴奋剂和氯胺酮的LC-MS/MS分析

目的建立生物检材中苯丙胺类兴奋剂和氯胺酮的液相色谱-串联质谱(LC-MS/MS)分析方法。方法生物检材包括血液、尿液和毛发,采用稀释法和液液提取的前处理方法,应用两个不同的液相柱,优化LC-MS/MS分析方法,并考察了血液和尿液基质的离子抑制作用。结果同时分析苯丙胺和MDA,液相1在3m in内完成,液相2可用于确认分析或复杂基质分离。尿液稀释法检材用量少,前处理简便快速。毛发中苯丙胺类兴奋剂和氯胺酮的最低检测限(LOD)为0.005~0.05ng/mg。对送检案例检材产妇头发和胎毛进行苯丙胺类兴奋剂和氯胺酮的分析。结论本方法可用于生物检材中苯丙胺类兴奋剂和氯胺酮的同时分析,血、尿等生物检材的离子抑制作用是影响本方法灵敏度的主要原因。

Determination of amphetamines and ketamine in biological specimens by liquid chromatography-tandem mass spectrometry

Objective To develop a method for simultaneous determination of amphetamines and ketamine in biological specimens by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The parent drugs and their metabolites were isolated simultaneously from human plasma,urine and hair by dilution and LLE.The parameters of LC-MS/MS including two columns were optimized.Ion suppression effects of matrixes were reviewed.ResultsAmphetamine and MDA were detected simultaneously with Liquid phase 1 ran within 3 min.The compounds were isolated from matrix and confirmed with Liquid phase 2.The amount of sample was less required by urine dilution method that was prepared simply and rapidly.Limits of detection ranged from 0.005 ng/mg to 0.05ng/mg.We also analyzed the hair segments from a postpartum woman and her infant.ConclusionThe method developed may be applied for simultaneous determination of amphetamines and ketamine in biological specimens with small quantities of samples.The matrix effect of plasma and urine is the primary factor influencing the sensitivity.