Determination of landiolol, an ultra-short-acting 尾b>1b>-receptor antagonist, in human plasma by liquid chromatography-tandem mass spectrometry

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• 作者：Qun He^a ; ^b ; Meiyun Shi^a ; ^b ; Xidong Liu^a ; ^b ; Yantong Sun^a ; ^b ; Lianghai Hu^a ; ^b ; Yan Yang^a ; ^b ; J. Paul Fawcett^c ; Jingkai Gu^a ; ^b ; ^{gujk@mail.jlu.edu.cn} ; Limei Zhao^d ; ^{zhaolm@sj-hospital.org}
• 关键词：Landiolol ; 尾1-Receptor antagonist ; LC&ndash ; MS/MS ; Determination ; Plasma
• 刊名：Journal of Chromatography B ; Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2012
• 期刊代码：124_15700232
• 类别：ch
• 出版时间：1 April, 2012
• 卷：891-892
• 期：Complete
• 页码：7-11
• 文件大小：498 K

摘要

A method for the determination of landiolol, an ultra-short-acting 尾b>1b>-adrenoreceptor antagonist, in human plasma has been developed and validated. With the addition of pyridostigmine bromide to stabilize landiolol in the blood/plasma samples, and bisoprolol as internal standard, plasma samples were subjected to liquid-liquid extraction with diethyl ether:dicholoromethane (60:40, v/v) prior to assay by liquid chromatography-tandem mass spectrometry. Separation was performed on a TC-Cb>18b> column (150 mm 脳 4.6 mm, 5 渭m) using a mobile phase of methanol:10 mM ammonium acetate containing 1%formic acid (65:35, v/v) in a run time of 3.5 min. Detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring of the precursor-to-product ion transitions of landiolol at m/z 510.1 鈫?#xA0;157.2 and bisoprolol at m/z 326.3 鈫?#xA0;116.1. The method was linear over the concentration range 0.5-500 ng/ml with a lower limit of quantitation of 0.5 ng/ml. Intra- and inter-day precisions (as relative standard deviation, RSD) were <4.4%and <10.0%, respectively, with accuracy (as relative error, RE) <10.0%. The method was successfully applied to a clinical pharmacokinetic study involving a continuous infusion of landiolol hydrochloride to healthy Chinese volunteers.