液相色谱-串联质谱法测定人全血兰地洛尔浓度  

Determination of Landiolol Concentration in Human Blood by LC-MS /MS

作　　者：俞蕴莉[1] 张全英[1] 华雯妍[1] 黄明[1] 王蒙[1] 

机构地区：[1]苏州大学附属第二医院临床药理实验室,苏州215004

出　　处：《医药导报》2014年第8期1009-1012,共4页Herald of Medicine

基　　金：江苏省中医药局科技项目(LZ13159)

摘　　要：目的采用液相色谱-串联质谱（ LC-MS/MS）法测定全血兰地洛尔的浓度,为注射用盐酸兰地洛尔的人体药动学研究提供检测手段。方法全血样本加入甲硫酸新斯的明后经乙腈沉淀蛋白,采用WATERS公司XTerra？ RP18（150 mm＆#215;4.6 mm,5μm）色谱柱,以乙腈10 mmol·L-1醋酸铵缓冲液（含0.1%甲酸）=3664（V/V）为流动相,流速为1 mL·min-1；质谱采用电喷雾离子化,正离子-多反应监测模式对兰地洛尔（m/z 510.5→423.1）和内标文拉法辛（m/z 278.2→215.1）的浓度进行测定。结果兰地洛尔的全血浓度在1.010~2020μg·L-1范围内线性良好,定量下限为1.010μg·L-1,批内精密度RSD〈6.5%,批间精密度RSD〈4.8%,提取回收率为92.6%-100.9%。结论该样品处理方法简便,测定方法灵敏、准确,适用于注射用盐酸兰地洛尔的人体药动学研究。Objective To establish an LC-MS/MS method for the detection of landiolol concentration in human blood.Methods After pretreatment with neostigmine and a deproteinization procedure, landiolol and the internal standard venlafaxine were eluted isocratically using a mobile phase consisting of acetonitrile and 10 mmoL·L-1 ammonium acetate with 0. 1% formic acid in a ratio of 3664 （ V/V ） . Separation of the respective compounds was achieved on a Waters XTerra？ RP18 column （150 mm＆#237;4. 6 mm,5 μm）. Quantitative analysis of landiolol was conducted by a triple-quadrupole mass spectrometer with positive-electrospray ionization source,monitored under a multiple reaction monitoring （ MRM） mode. The extracted ions monitored following MRM transitions were m/z 510. 5→423. 1 for landiolol and m/z 278. 2→215. 1 for the internal standard venlafaxine. ResultsThe calibration curve of landiolol in human blood showed good linear relationship in the range of 1. 010-2 020 μg·L-1 . The lower limit of quantitation was 1. 010 μg · L-1 . The RSD of within-day and between-day precision was less than 6. 5% and 4. 8%, respectively. The recovery rate was 92. 6%-100. 9%. Conclusion The method is proven to be simple,rapid and reliable,and can be applied to study the pharmacokinetics of landiolol hydrochloride in healthy Chinese volunteers.

关 键 词：兰地洛尔 血药浓度 液相色谱-串联质谱法 

分 类 号：R972.2[医药卫生—药品] R969.1[医药卫生—药学]