中空纤维膜液相微萃取-气相色谱-质谱法测定血中3种苯二氮卓类药物
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摘要
采用中空纤维膜液相微萃取-气相色谱-质谱法测定血中艾司唑仑、阿普唑仑和三唑仑等3种苯二氮卓类药物的含量。优化的试验条件如下:(1)聚偏氟乙烯中空纤维膜的孔径为0.1μm;(2)萃取溶剂为二甲苯;(3)萃取搅拌速率为500r·min~(-1);(4)萃取温度为30℃;(5)萃取时间为25min;(6)样品溶液的pH为9.0。在气相色谱分离中采用HP-5MS石英毛细管色谱柱,在质谱分析中采用选择离子监测模式。采用互为内标法进行定量。3种苯二氮卓类药物的线性范围均为0.03～5.00mg·L~(-1),方法的检出限(3S/N)为0.006～0.010mg·L~(-1)。以空白样品为基体进行加标回收试验,所得回收率为95.0%～104%,测定值的相对标准偏差(n=6)为0.52%～6.3%。
LPME-GC-MS was applied to the determination of 3 benzodiazepine drugs,i.e.eurodin,alprazolam and triazolam in blood with hollow fiber membranes.The optimized conditions found were as follows:(1)aperture of hollow fiber membrane of polyvinylidene fluoride was 0.1μm;(2) extraction solvent was xylene;(3)stirring rate of extraction was 500 r·min-1;(4)extraction temperature was 30℃;(5)extraction time was 25 min;(6) pH of the sample solution was 9.0.The HP-5 MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Crossing internal standard method was used for quantitative.Linearity ranges of the 3 benzodiazepine drugs were all between 0.03 mg·L~(-1) and5.00 mg·L~(-1) with detection limits(3 S/N)in the range of 0.006-0.010 mg·L~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 95.0%-104%,with RSDs(n=6)in the range of 0.52%-6.3%.
LPME-GC-MS was applied to the determination of 3 benzodiazepine drugs,i.e.eurodin,alprazolam and triazolam in blood with hollow fiber membranes.The optimized conditions found were as follows:(1)aperture of hollow fiber membrane of polyvinylidene fluoride was 0.1μm;(2) extraction solvent was xylene;(3)stirring rate of extraction was 500 r·min-1;(4)extraction temperature was 30℃;(5)extraction time was 25 min;(6) pH of the sample solution was 9.0.The HP-5 MS quartz capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination.Crossing internal standard method was used for quantitative.Linearity ranges of the 3 benzodiazepine drugs were all between 0.03 mg·L~(-1) and5.00 mg·L~(-1) with detection limits(3 S/N)in the range of 0.006-0.010 mg·L~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 95.0%-104%,with RSDs(n=6)in the range of 0.52%-6.3%.
引文
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[5]张建丽,王占良,张亦农.液相色谱-串联质谱法测定尿样中11种苯二氮卓类药物及其代谢产物[J].分析试验室,2014,33(4):479-482.
[6] MARIEKE D B,SOPHIE M,WIM D,et al.Development and validation of a fast ionic liquid-based dispersive liquid-liquid microextraction procedure combined with LC-MS/MS analysis for the quantification of benzodiazepines and benzodiazepine-like hypnotics in whole blood[J].Forensic Science International,2017,274:44-54.