论文部分内容阅读
目的建立快速、灵敏的HPLC-MS/MS法测定人体内美沙拉嗪血药浓度。方法血浆样品经乙腈沉蛋白进行提取,用Agilent-C_(18)(150 mm×4.6 mm,5μm)色谱柱分离,以喷昔洛韦为内标,流动相为甲醇-乙腈-体积分数为0.05%的甲酸溶液(体积比为50∶20∶30),流速为500μL·min~(-1)(柱后分流比为1∶1),采用ESI源,正离子检测,多反应监测(MRM)扫描方式。结果人体血浆中的内源物质不干扰美沙拉嗪的测定,美沙拉嗪在50~2 500μg·L~(-1)内峰面积与质量浓度线性关系良好(r=0.996 8),最低检测限为50μg·L~(-1),低、中、高3个质量浓度质控样品的日内,日间精密度均小于15%,准确度为97.0%~101.8%,提取回收率在71.4%~73.4%,基质效应可忽略不计。结论HPLC-MS/MS法可用于人血浆中美沙拉嗪测定。
Objective To establish a rapid and sensitive HPLC-MS / MS method for the determination of mesalazine in human serum. Methods The plasma samples were extracted with acetonitrile-precipitated protein and separated on a Agilent-C 18 column (150 mm × 4.6 mm, 5 μm). Penciclovir was used as the internal standard and the mobile phase consisted of methanol-acetonitrile with a volume fraction of 0.05 % Of formic acid solution (volume ratio of 50:20:30), the flow rate of 500μL · min -1 (column split ratio of 1: 1), using ESI source, positive ion detection, multiple reaction monitoring (MRM) scanning method. Results The endogenous substances in human plasma did not interfere with the determination of mesalazine. Mesalazine showed a good linear relationship (r = 0.996 8) with the peak area of 50 ~ 2 500 μg · L -1, the lowest detection limit The precision of the quality control samples with 50 μg · L -1, low, medium and high quality control was less than 15%, the accuracy was 97.0% ~ 101.8%, the extraction recovery was 71.4% 73.4%, matrix effect is negligible. Conclusion HPLC-MS / MS method can be applied to the determination of mesalazine in human plasma.