高效液相色谱-三重四极杆/复合线性离子阱质谱法测定血液中唑吡坦和扎莱普隆的含量  

HPLC QTRAP-MS/MS Determination of Zolpidem and Zaleplon in Blood

作　　者：时巧翠[1] 朱斌[1] 

机构地区：[1]浙江警察学院刑事科学技术系,杭州310053

出　　处：《理化检验（化学分册）》2017年第7期843-847,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：公安部重点研究计划项目(201202ZDYJ007)

摘　　要：血液样品0.50mL,加pH 10的乙酸铵缓冲溶液0.3mL,混匀后采用介质液液萃取柱净化,用二氯甲烷8mL洗脱。洗脱液经处理后进行色谱分离。以Kinetex C18色谱柱为固定相,以不同体积比的含5mmol·L^(-1)乙酸铵的0.1%(体积分数)甲酸溶液和乙腈混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式。唑吡坦、扎莱普隆的质量浓度分别在0.20~10.00μg·L^(-1),1.00~50.00μg·L^(-1)范围内与峰面积呈线性关系,检出限(3S/N)分别为0.02,0.10μg·L^(-1)。按标准加入法进行回收试验,回收率在85.0%~103%之间,测定值的相对标准偏差(n=6)在3.5%~8.5%之间。Blood sample （0. 50 mL） was mixed with 0. 3 mL of ammonium acetate buffer solution （pH 10）, and the mixture was purified on the supported liquid extraction column and 8 mL of dichloromethane was used as eluent. The treated eluate was separated by HPLC using Kinetex C18 eolumn as stationary phase and mixtures of acetonitrile and 0. 1% （φ） formic acid solution containing 5 mmol · L-1 ammonium acetate, mixed in various ratios, as mobile phase in gradient elution. ESI＋ and MRM were adopted in MS. Linear relationships between values of peak area and mass concentration were found in the ranges of 0. 20 -- 10. 00 μg · L^-1 for zolpidem and 1.00 -- 50. 00μg · L^-1 for zaleplon, with detection limits （3S/N） of 0. 02, 0. 10 μg · L^-1, respectively. Test for recovery was made by standard addition method, giving results in the range of 85.0%-103%, with RSDs （n = 6） ranged from 3. 5 % to 8. 5 %.

关 键 词：高效液相色谱-三重四极杆/复合线性离子阱质谱法 介质液液萃取 唑吡坦 扎莱普隆 血液 

分 类 号：O657.63[理学—分析化学]