LPME-GC-MS Determination of 3 Benzodiazepine Drugs in Blood with Hollow Fiber Membranes
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0.1 μm;② 萃取溶剂为二甲苯;③ 萃取搅拌速率为500 r·min-1;④ 萃取温度为30℃;⑤ 萃取时间为25 min;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0.03~5.00 mg·L-1,方法的检出限(3S/N)为0.006~0.010 mg·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%。
Abstract
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 0.1 μm; 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-5MS 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 and 5.00 mg·L-1 with detection limits (3S/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%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201811020
所属栏目 工作简报
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收稿日期 2017/11/6
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备注耿忠兴,助理实验师,硕士研究生,主要从事理化检验工作,gruxing@163.com
引用该论文: GENG Zhongxing,ZOU Qinglong. LPME-GC-MS Determination of 3 Benzodiazepine Drugs in Blood with Hollow Fiber Membranes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(11): 1334~1338
耿忠兴,邹清龙. 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[J]. 理化检验-化学分册, 2018, 54(11): 1334~1338
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