DPX-GC/MS法分析尿液中新精神活性物质二苯基乙基哌啶

Analysis of diphenidine in urine by disposable pipette extraction combined with gas chromatography mass spectrometry

目的建立一种枪头式分散固相微萃取-气相色谱质谱法,分析尿液中的二苯基乙基哌啶。方法对影响萃取效果的吸附树脂种类、淋洗液种类、洗脱液种类和洗脱液用量进行优化考察。结果在最佳实验条件下,尿液中二苯基乙基哌啶的线性范围为0.02~1.0 mg/L,相关系数r^(2)>0.99,检出限为0.005mg/L,回收率在76.7%~85.5%之间,相对标准偏差(RSD)为1.8%~2.8%之间(n=6)。结论该方法萃取效果好,操作步骤少,简便快速,线性范围良好,回收率和精密度均能满足检验需求。

Objective To establish a method for the determination of diphenidine in urine by dispersive pipette extraction(DPX)technology combined with gas chromatography mass spectrometry(GC-MS).Methods Experimental parameters affecting the extraction efficiency such as the variety of sorbent resin,the variety of washing solvent and eluting solvent,and the volume of eluting solvent were investigated.Results Under the optimal conditions,the linear range was from 0.02 mg/L to 1.0 mg/L,and r^(2) greater than 0.99,the limit of detection was 0.005 mg/L.The recovery ranged from 76.7%to 85.5%and the relative standard deviations were in the range from 1.8%to 2.8%(n=6).Conclusion This method has perfect linearity,precision and recovery,which can be applied to the analysis of diphenidine in urine due to its simplicity,accuracy and practicality.