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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 To establish a method for the determination of triazolam in blood by hollow fiber membrane liquid phase microextraction-gas chromatography-mass spectrometry. Methods 2 mL of whole blood was diluted to 10 mL with pH 9 buffer to prepare a sample solution. Liquid micro-extraction was performed on the hollow fiber membrane. The organic solvent in the hollow fiber cavity was directly extracted for GC / MS analysis. Investigate and select the optimal extraction conditions, including the length of hollow fiber, extractant, extraction temperature, stirring rate, extraction time, and methodological evaluation. Results The optimal extraction conditions were as follows: 5cm long hollow fiber, extractant was octanol, extraction temperature was 30 ℃, stirring rate was 600r / min, extraction time was 30min. The methodological evaluation showed that the linear range was 0.1 ~ 10.0μg / mL (r = 0.999 0), the relative standard deviation was 0.8% ~ 2.5%, the detection limit was 72.8ng / mL, the recovery was 74% and the enrichment factor was 165. Conclusion The method of this method is completed in one step of extraction and concentration, which is simple, rapid, less consumption of organic solvents, good reproducibility, and can be used in the blood triazolam drug testing.