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机构地区:[1]浙江医院药剂科浙江省老年医学重点实验室,杭州310013
出 处:《中国临床药学杂志》2015年第1期13-17,共5页Chinese Journal of Clinical Pharmacy
基 金:国家科技重大专项项目-老年病新药临床技术平台(编号2013ZX09303005)
摘 要:目的建立LC—MS/MS法同时测定人血浆中阿罗洛尔、阿替洛尔、比索洛尔和美托洛尔的浓度。方法人血浆样晶用乙酸乙酯萃取后,选用ZORBAXSBC18(100mm×2.1mm,3.5μm)色谱柱,以甲醇-0.1%甲酸为流动相梯度洗脱,采用电喷雾离子化源、正离子方式和多反应监测(MRM)扫描方式进行监测。结果血浆中阿罗洛尔、阿替洛尔、比索洛尔和美托洛尔的线性范围均为1.0~500μg·L^-1(r〉0.99),定量下限均为1.0μg·L^-1;平均回收率94.4%~107.9%;日内、日间RSD均〈15%;提取回收率在78.8%。89.4%。结论该方法快速、灵敏、准确,专属性强,重复性好,适用于人血浆中同时测定阿罗洛尔、阿替洛尔、比索洛尔和美托洛尔浓度。AIM To develop an LC-MS/MS method for simultaneous determination of arotinolol, atenolol, biso- prolol and metoprolol concentrations in human plasma. METHODS The plasma samples were processed with ethyl ac- etate extraction. The separation was achieved on ZORBAX SB C18 column (100 mm× 2.1 mm, 3.5μm) and eluted with linear gradient using methanol and 0.1% formic acid. Detection of the analytes were achieved using positive ion electro- spray ionization (ESI) in the multiple reaction monitoring (MRM) mode. RESULTS The linear calibration curves of arotinolol, atenolol, bisoprolol and metoprolol were obtained in the concentration range of I. 0 - 500 μg· L- 1 ( r 〉 0.99), with the lower limit of quantitation (LLOQ) of 1.0μg· L-1. The average recovery was between 94.4 % - 107.9 %. Intra- day and inter-day relative standard deviations were both below 15 %. The recoveries of low, middle and high concentra- tions were 78.8 % - 89.4 %, respectively. CONCLUSION The established method is rapid, sensitive, accurate, spe- cific and reliable, and suitable for simultaneous determination of arotinolol, atenolol, bisoprolol and metoprolol in human plasma.
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