中空纤维液相微萃取-气质联用检测血液中的三唑仑

Determination of triazolam in blood by hollow fiber liquid phase microextraction and GC/MS

目的建立中空纤维膜液相微萃取-气质联用测定血液中三唑仑的方法。方法取2mL全血用pH9缓冲溶液稀释至10mL制成样品溶液,采用中空纤维膜进行液相微萃取,直接抽取中空纤维内腔中的有机溶剂进行GC/MS分析。考察和选择最优萃取条件,包括中空纤维长度、萃取剂、萃取温度、搅拌速率、萃取时间,并进行方法学评价。结果最优萃取条件为：5cm长中空纤维,萃取剂为辛醇,萃取温度为30℃,搅拌速率为600r/min,萃取时间为30min。方法学评价表明线性范围为0.1~10.0μg/mL（r=0.999 0）,相对标准偏差在0.8%~2.5%,检测限为72.8ng/mL,回收率为74%,富集倍数为165。结论本文方法萃取和浓缩一步完成,简便、快速、消耗有机溶剂少,重现性好,可在血液三唑仑药物检测中选用。

Objective A method was developed to determine the triazolam in blood by GC/MS coupled with hollow fiber liquid phase microextraction. Methods The 10 mL sample solution can be gotten by diluting a 2mL whole blood with pH9 buffer solution. By adopting hollow fiber membrane liquid phase membrane microextraetion, the author can extract organic solvent directly from the hollow fiber lumen and inject it into GC/MS analysis. Optimal extraction conditions, including the length of hollow fiber, extracting solvent, extracting time and extracting temperature, should be selected. The evaluation of the methodology should be done as well. Results The optimal experimental conditions were as followings： 5cm long hollow fiber, octyl alcohol as extraction solvent, 30℃ extracting temperature, 600r/min stirring speed and 30 min extraction time. Methodology evaluation showed that the linear range of were from 0. 1 to 1.0 μ/mL （ r = 0. 999 0）, and RSD were between 0. 8% and 2. 5%. The limits of detection was 72. 8ng/mL. The extraction recovery was 74%, and the enrichment factor was 165. Conclusion ： The method of extraction and enrichment in this thesis was completed in one step. Because of its simple and rapid characteristics, as well as its low organic solvent consumption and good reproducibility, this method can be applied to the determination of triazolam in blood.