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

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,3.5μm)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0.1μg/g、1μg/g、0.001μg/g,定量限分别为0.5μg/g、2μg/g、0.005μg/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。

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 0.001μg/g,and the limits of quantification were 0.5,2 and 0.005μg/g,respectively.Conclusion:The method is simple and accurate to detect the contents of three antidepressants in feces,such as duloxetine,fluoxetine and escitalopram.