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 %.
出处
《理化检验（化学分册）》
CSCD
北大核心
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)
