LC-MS法测定大鼠血浆中EXH-1626的浓度
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科技部十二五“重大新药创制”科技重大专项课题(子课题)(2012ZX09103101-048)


Determination of EXH-1626 concentration in rat plasma by LC-MS
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    摘要:

    目的:建立测定大鼠血浆中EXH-1626浓度的液相色谱-质谱(LC-MS)方法-方法:大鼠血浆样品中加入内标卡马西平,经蛋白沉淀剂(甲醇∶5%硫酸锌溶液 = 70∶30,V/V)沉淀血浆蛋白后取上清液5 μl进行LC-MS测定-色谱条件:色谱柱为汉邦ODS C18柱(5 μm,150 mm × 4.6 mm),流动相为乙腈∶10 mmol/L醋酸铵水溶液(用乙酸调pH至3)70∶30,流速为0.6 ml/min,柱温30℃;质谱条件:采用电喷雾离子化(ESI)方式,以选择性离子监测(SIM)方式检测,EXH-1626和内标选择检测离子的质荷比(m/z)分别为453.3([M+H]+)和274.3([M+H]+)-结果:大鼠血浆中EXH-1626在5~10 000 ng/ml内线性关系良好(r = 0.999 7),最低定量限(LOQ)为5 ng/ml,由低到高(10-100-1 000和10 000 ng/ml)4个浓度的日内和日间精密度RSD均< 10%,绝对回收率均> 70%,相对回收率90%~110%-结论:该方法快速-准确,灵敏度高,操作简便,适用于EXH-1626血药浓度测定及其非临床药代动力学研究-

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    Objective: To develop a LC-MS method for the determination of EXH-1626 in rat plasma. Methods:Using carbamazepine as internal standard (IS),plasma samples were deposited by blood precipitation reagent(methanol∶5% zinc sulfate =70∶30,V/V) before sampling and determined by injecting 5 μl supernatant to LC-MS system. Chromatographic condition:the analytes were separated on a Han Bang ODS C18(5 μm,150 mm × 4.6 mm) analytical column with acetonitrile and 10 mmol/L ammonium acetate(using acetic acid to make pH = 3) (70∶30) as the mobile phase. Analysis was performed at a flow rate of 0.6 ml/min and the column temperature was 30℃. Mass sapectum determination was performed in electrospray ionization(ESI) mode and the selected ion monitoring(SIM) mode,EXH-1626 was monitored at m/z 453.3 and internal standard at m/z 274.3. Results: The linearity of EXH-1626 concentration curve was in a range of 5~1.0 × 104 ng/ml,r = 0.999 7,and the lowest limit of quantification(LOQ) was 5 ng/ml. The RSDs of inter-day and intra-day were less than 10%,absolute recoveries were greater than 70%,and relative recoveries were between 90% to 110%. Conclusion:The method is proved to be fast,precise,sensitive,convenient,and suitable for determination of concentration and non-clinical pharmacokinetic study of EXH-1626.

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李泰平,肖 红,向 华. LC-MS法测定大鼠血浆中EXH-1626的浓度[J].南京医科大学学报(自然科学版),2014,(1):

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  • 收稿日期:2013-07-15
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  • 在线发布日期: 2014-01-27
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