高效液相色谱串联质谱法同时检测粪便中三种抗抑郁药物*

doi:10.12047/j.cjap.6173.2020.139

中国应用生理学杂志 ›› 2020, Vol. 36 ›› Issue (6): 668-672.doi: 10.12047/j.cjap.6173.2020.139

• 技术方法 • 上一篇

高效液相色谱串联质谱法同时检测粪便中三种抗抑郁药物^*

邵一帆, 张安琪, 陈天姣, 李海北, 陈郑珊, 尹静, 杨栋, 师丹阳, 梁永兵, 程春燕, 谭蓉, 孙栋良, 李君文, 金敏^△

军事科学院军事医学研究院环境医学与作业医学研究所, 天津 300000

收稿日期:2020-10-10 修回日期:2020-11-25 发布日期:2021-03-15
通讯作者: ^△Tel: 022-84655366; E-mail: jinminzh@126.com
基金资助:
^*国家自然科学基金面上项目(81972994)

Simultaneous determination of three antidepressant drugs in feces by HLPC-MS

SHAO Yi-fan, ZHANG An-qi, CHEN Tian-jiao, LI Hai-bei, CHEN Zheng-shan, YIN Jing, YANG Dong, SHI Dan-yang, LIANG Yong-bing, CHENG Chun-yan, TAN Rong, SUN Dong-liang, LI Jun-wen, JIN Min^△

Tianjin Institute of Environmental and Operational Medicine, Tianjin 300000, China

Received:2020-10-10 Revised:2020-11-25 Published:2021-03-15

摘要/Abstract

摘要： 目的:建立同时检测粪便中度洛西汀、氟西汀、艾斯西酞普兰三种抗抑郁药物的高效液相色谱串联质谱(HPLC-MS)方法。方法:样品经正己烷-异丙醇(95:5,v/v)预处理后,以超纯水和乙腈混合液作为流动相进行梯度洗脱,在Agilent ZORBAX SB-C18液相色谱柱(2.1 mm×100 mm,3.5 μm)上分离后用电喷雾串联质谱法检测,内标法定量。结果:粪便样品中度洛西汀、氟西汀、艾斯西酞普兰的加标回收率为61.6%～116.5%,精密度为 2.80%～12.9%(n=5),线性方程相关系数(r)均大于0.995,检出限分别为0.1 μg/g、1 μg/g、0.001 μg/g,定量限分别为0.5 μg/g、2 μg/g、0.005 μg/g,符合高效液相色谱串联质谱的分析要求。结论:该方法能够简单、准确检测出粪便中度洛西汀、氟西汀、艾斯西酞普兰这三种抗抑郁药的含量。

关键词: 粪便, 高效液相色谱-串联质谱法, 抗抑郁药物, 小鼠

Abstract: Objective: To establish a high performance liquid chromatography tandem mass spectrometry (HPLC / MS) method for the simultaneous determination of three antidepressant drugs in feces. Methods: Samples were pretreated with n-hexane isopropanol (95:5, v/v). Gradient elution was carried out with mixed liquid of ultrapure water and acetonitrile as mobile phase and separated by Agilent ZORBAX SB-C18 liquid chromatography column (2.1 mm×100 mm, 3.5 m). The samples were detected by electrospray ionization tandem mass spectrometry and quantified by internal standard method. Results: The recoveries of duloxetine, fluoxetine and escitalopram in fecal samples were 61.6% - 116.5%, with precision of 2.80% - 12.9% (n=5). The correlation coefficients (r) of linear equations were all greater than 0.995. The detection limits were 0.1, 1, and 0.001 μg/g, and the limits of quantification were 0.5, 2 and 0.005 μg/g, respectively. Conclusion: The method is simple and accurate to detect the contents of three antidepressants in feces, such as duloxetine, fluoxetine and escitalopram.

Key words: feces, HPLC-MS, antidepressants, mice

中图分类号:

邵一帆, 张安琪, 陈天姣, 李海北, 陈郑珊, 尹静, 杨栋, 师丹阳, 梁永兵, 程春燕, 谭蓉, 孙栋良, 李君文, 金敏. 高效液相色谱串联质谱法同时检测粪便中三种抗抑郁药物^*[J]. 中国应用生理学杂志, 2020, 36(6): 668-672.

SHAO Yi-fan, ZHANG An-qi, CHEN Tian-jiao, LI Hai-bei, CHEN Zheng-shan, YIN Jing, YANG Dong, SHI Dan-yang, LIANG Yong-bing, CHENG Chun-yan, TAN Rong, SUN Dong-liang, LI Jun-wen, JIN Min. Simultaneous determination of three antidepressant drugs in feces by HLPC-MS[J]. CJAP, 2020, 36(6): 668-672.

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高效液相色谱串联质谱法同时检测粪便中三种抗抑郁药物^*

Simultaneous determination of three antidepressant drugs in feces by HLPC-MS

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