LC-MS／MS法测定人血浆中盐酸度洛西汀浓度及其应用

目的建立测定人血浆中盐酸度洛西汀浓度的IJC—MS／MS法。方法以丙咪嗪为内标，血浆样品经乙腈沉淀蛋白后，以水-乙腈-甲酸（64：36：0．04，V/V/V）为流动相，流速0．3mL·min^-1，Diamonsil C18柱分离，采用电喷雾离子源（ESI），以多离子反应监测（期谢）方式进行正离子检测。用于定量分析离子反应分别为m／z 298．2→44．2（盐酸度洛西汀）和m／z 281．2—86．2（IS）。结果测定血浆中盐酸度洛西汀的线性范围为0．2-100ug·L^-1，定量下限为0．2μg·L^-1；批内、批间精密度（RSD）均〈6％；方法回收率为92％～104％；提取回收率均〉95％。结论本法专属性强，灵敏度高，样品处理简单、快速，适合用于盐酸度洛西汀在人体内的药动学研究。

LC-MS/MS determination of duloxetine hydrochloride in human plasma and its application

AIM To develop a method for direct determination of duloxetine hydrochloride in human plasma. METHODS Duloxetine hydrochloride and intemal standard imipramine were extracted from plasma using acetonitrile and separated on a Diamonsil C18 column. The mobile phase consisted of water-aeetonitrile-fonnic acid （64：36：0.04, V/V/ V）. The flow rate was 0.3 mL·min^-1. A mass spectrometer equipped with electrospray ionization source was used as detector operated in the positive ion mode. Multiple reaction monitoring（MRM） mode using the transition of m/z 298.2→44.2 and m/z 281.2→86.2 was used to quantify duloxietine hydrochloride and internal standard （IS）, respectively. RESULTS The linearity was obtained in the concentration range of 0.2 - 100 μg·L^-1 and the lower limit of quantification was 0.2μg·L^-1. The inter-batch and intra-bateh precision was lower than 6% . The method recovery rate was between 92% and 104%. The extraction recovery rate was higher than 95%. CONCLUSION The method is sensitive, rapid, convenient and is proved to be suitable for investigation of duloxetine hydrochloride phannacokinetics.