LC-MS/MS法测定人血浆中比拉斯汀含量的不确定度评定  

Uncertainty Evaluation of the Determination of Bilastine in Human Plasma by LC-MS/MS

作　　者：梁璐[1] 凌飒[1] 赵一朗 宋汉骋 王敏 Liang Lu;Ling Sa;Zhao Yilang;Song Hancheng;Wang Min(Hubei Institute of Pharmaceutical Industry Company,Wuhan 430061,China)

机构地区：[1]湖北省医药工业研究院有限公司,武汉430061

出　　处：《中国药师》2018年第10期1850-1853,共4页China Pharmacist

摘　　要：目的:建立液相色谱-串联质谱(LC-MS/MS)法测定人血浆中比拉斯汀浓度的方法,并对其方法不确定进行评定。方法:对测定人血浆中比拉斯汀的浓度过程中的不确定度来源进行分析,包括测定精密度、仪器、称量、标准溶液配制、含药血浆配制、标准曲线拟合、血浆样本的处理等,计算各分量的不确定度和合成不确定度,最终计算扩展不确定度。结果:低(15 ng·ml^(-1))、中(400 ng·ml^(-1))、高(1 200 ng·ml^(-1))各浓度的扩展不确定度分别为1. 45 ng·ml^(-1)、28. 72 ng·ml^(-1)、74. 61 ng·ml^(-1)(k=2,P=95%)。结论:人血浆中比拉斯汀含量的不确定度主要是由仪器允差,标准溶液的配制,血浆样本的处理,标准曲线拟合(低浓度)引入。Objective： To establish a method for the determination of bilastine in human plasma,and evaluate the uncertainty by LC-M/S. Methods： The uncertainty sources were obtained from the whole process of the determination including repeatability,equipment error,weighting,solution preparation,calibration fitting and plasma sample handling. The uncertainty and synthesized uncertainty of each component were calculated,and then the expanded uncertainty was obtained. Results： The expanded uncertainty for low（ 15 ng·ml^-1）,medium（ 400 ng·ml^-1） and high（ 1 200 ng·ml^-1） level of bilastine was 1. 45 ng·ml^-1,28. 72 ng·ml^-1 and 74. 61 ng·ml^-1,respectively（ k = 2,P = 95%）. Conclusion： The uncertainty in the determination of bilastine in human plasma is mainly caused by equipment error,solution preparation,protein precipitation and calibration fitting（ especially at low level）.

关 键 词：比拉斯汀 不确定度 人血浆 液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]