HPLC-MS/MS法测定人体内美沙拉嗪血药浓度  

Determination of mesalazine in human plasma by HPLC-MS / MS

作　　者：姜悦[1] 韩雨钊 林茂[1] 李淼[1] 李野[1] 刘茜[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2016年第4期293-297,共5页Journal of Shenyang Pharmaceutical University

摘　　要：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 develop a newrapid and sensitive HPLC-MS / MS method for the determination of mesalazine in human plasma. Methods Plasma samples were analyzed after protein precipitation by acetonitrile and the separation was achieved with a mobile phase consisting of 0. 05%（ φ） formic acidmethanol-acetonitrile（ V ∶ V ∶ V = 30 ∶ 50 ∶ 20） by using a C_（18） Agilent column（150 mm × 4. 6 mm,5 μm） at a500 μL·min^-1flowrate. Penciclovir was used as internal standard. Selctive detection was carried out by multiple reaction monitoring with an API 2 000 triple quadrupole mass spectrometer equipped with an electrospray ionization source,operating in positive ionization mode. Results The endogenous substance in human plasma did not interfere with the determination of mesalamine. The linear calibration curve was obtained in the range of 50- 2 500 μg·L^-1for mesalazine. The lower limit of quantitation was 50 μg·L^-1,the intra-day and inter-day precision RSD was less than 15%,the accuracy was within 97. 0%^-101. 8%,and the recovery was 71. 4%- 73. 4%. Conclusions The method is rapid,sensitive,specific and reproducible,and can be used for the determination of mesalazine

关 键 词：美沙拉嗪 高效液相色谱-串联质谱 血药浓度 

分 类 号：R917[医药卫生—药物分析学]