分散液液微萃取-气质联用法分析尿液中的曲马多

Determination of Tramadol in Urine by Dispersive Liquid–liquid Micro-extraction Combined with GC/MS

目的建立了分散液液微萃取-气相色谱质谱联用法(GC/MS)测定尿液中曲马多的方法。方法通过对分散液液微萃取过程中需要使用的萃取剂和分散剂的种类、体积、萃取时间、pH值等实验条件进行优化,建立尿液中曲马多的GC/MS分析方法。GC/MS方法通过程序升温对曲马多进行分离,质谱选择电子轰击离子源和特征碎片离子进行分析。结果在优化的实验条件下,尿液中曲马多的回收率超过80%,检出限为0.97μg/L,定量限为3.22μg/L,在10-1 000μg/L范围内线性关系良好。结论该方法操作简便、快捷、绿色环保,已经成功应用于尿液中曲马多及其代谢物的检测。

Objective A simple and rapid dispersive liquid-liquid micro-extraction technique （DLLME） combined with gas chromatography-mass spectrometry （GC/MS） was developed for the analysis of tramadol in urine sample. Method Parameters affecting the extraction rate such as the type and volume of extraction solvent, type and volume of dispersant, and extraction time, pH value were optimized. Results Under optimized conditions, the relative recovery of tramadol was more than 80 %, the limit of detection and the limit of quantification were 0.97 μg/L and 3.22 μg/L, respectively. The linear relationship was quite good in the range from 10 μg/L to 1000 μg/L. Conclusion DLLME combined with GC/MS is a fast and rapid method for the determination of tramadol and its metabolites in urine. This method has been applied in some cases.