液-质联用法测定健康受试者血浆中他林洛尔的浓度  被引量:4

Determination of the concentration of Talinolol in healthy volunteers by LC-MS

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作  者:王亦男[1] 谭志荣[1] 陈尧[1] 郭栋[1] 韩仰[1] 陶共由[1] 陈豪[1] 陈英[1] 肖昌琼[1] 张敏[1] 周宏灏[1] 

机构地区:[1]中南大学临床药理研究所,长沙410078

出  处:《中南药学》2008年第1期45-48,共4页Central South Pharmacy

摘  要:目的 建立液-质联用法测定人血浆中他林洛尔的浓度。方法 空白血浆加他林洛尔和内标,用乙腈直接沉淀,然后用质谱进行检测。色谱柱为Cosmosil C18 (2.0mm×150mm,5μm),柱温40℃,流动相为乙腈-10mmol·L^-1甲酸胺水溶液(含0.05%甲酸)(60:40,v/v),流速为0.2mL·min^-1,进样量为20μL,采用正离子方式扫描,他林洛尔的监测离子为m/z:364.3→308.1,内标普萘洛尔的监测离子为m/z:260.1→184.2。结果 他林洛尔的线性范围为1.00~522.40ng·mL^-1,r^2=0.999,最小检出浓度为1.00ng·mL^-1,绝对回收率在80%左右,相对回收率在80%~115%,日内、日间RSD均〈15%。结论 本方法简便、灵敏,适用于他林洛尔血药浓度检测和药物动力学研究。Objective To establish an I.C MS method to determine talinolol in human plasma. Methods Propranolol was added to samples as internal standard and the plasma protein was sedimented by acetrinile. A Cosmosil C18 (2.0 min× 150 mm, 5 μm) column was used to separate the analytes and the column temperature was 40 ℃. The mobile phase, acetonitrile and 10 mmol·L^-1 ammonium formate water solution (with 0.05% formic acid), was 60 : 40 (v/ v), and the flow rate was 0.2 mL·min^-1. Positive ion scan mode was performed for the target ions, rn/z 364→308 for talinolol and m/z 260→184 for propranolol. Results Talinolol was linear from 1.00~522.40 ng·mL^-1 , r^2 =0. 999, and the limitation of detection for talinolol was about 1.00 ng·mL^-1. The extracted recovery was〉80%. The relative recovery was 80%~115%, and the intra- and inte-day RSD were〈15%. Conclusion The method is simple, accurate, and repetitive for the determination of talinolol and is successfully used for pharmacokinetic study in healthy volunteers.

关 键 词:液-质联用 他林洛尔 血药浓度 沉淀 

分 类 号:R917[医药卫生—药物分析学]

 

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