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介质液液萃取-HPLC-MS/MS法同时测定血液中5种吩噻嗪类药物 被引量:2

Determination of 5 phenothiazines in blood by supported liquid extraction and HPLC-MS/MS
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摘要 结合介质液液萃取技术建立了高效液相色谱-串联质谱法同时测定血液中5种吩噻嗪类药物的检测方法。采用Kinetex C18色谱柱,以0.1%甲酸+5 mmol·L^(-1)乙酸铵水溶液-乙腈为流动相,梯度洗脱分离。在电喷雾正离子模式下,以多反应检测(MRM)扫描模式采集数据对血液中的5种吩噻嗪类药物进行定性与定量分析。5种吩噻嗪类药物在5.0~100 ng·m L^(-1)范围内具有良好的线性关系,相关系数均大于0.9939;检出限在0.07~0.30 ng·m L^(-1)之间;添加浓度水平为10,20和50 ng·m L^(-1)时,方法的平均回收率为78.2%~105.7%;相对标准偏差为3.5%~10.8%。该方法可用于血液中五种吩噻嗪类药物的法庭与临床毒物分析。 An analytical method based on supported liquid extraction(SLE)coupled with high performance liquid chromatography tandem mass spectrometry was developed for the determination of 5 phenothiazines in Blood.The samples were extracted with the supported liquid extraction columns and the analyses were carried out on HP LC-MS/MS.The chromatographic separation was performed on a Kinetex C18 analytical column(50 mm×3.0 mm,2.6μm)using 5 mM ammonium formate and 0.1%formic acid in water-acetonitrile as the mobile phase.Detection was carried out under the multiple reaction monitoring(MRM)in positive ionization mode.The linear range of calibration curve was from 5.0~100 ng·mL-1 for 5 phenothiazines.The detection limits of the method were 0.07~0.30 ng·mL-1 The mean recoveries at the three spiked levels of 10,20 and 50 ng·mL-1 were 78.2%~105.7%and the relative standard deviations were 3.5%~10.8%.The method is applicable to analyze antidepressants in forensic and clinical toxicology.
作者 时巧翠 陈升俊 王洲鼎 SHI Qiao-cui;CHEN Sheng-jun;WANG Zhou-ding(Department of Criminal Science and Technology,Zhejiang Police College,Hangzhou 310053,China)
出处 《化学研究与应用》 CAS CSCD 北大核心 2018年第4期627-631,共5页 Chemical Research and Application
基金 浙江省公益计划研究项目(LGF18B050002)资助
关键词 介质液液萃取 高效液相色谱-串联质谱 吩噻嗪类药物 血液 supported liquid extraction(SLE) HPLC-MS/MS phenothiazines blood
作者简介 联系人简介:时巧翠(1977-)女,副教授,从事理化分析研究。E-mail:shiqiaocui@zjjcxy.cn。
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