摘要
目的:对液质联用色谱法测定血浆中雷贝拉唑的不确定度进行分析,找出影响因素,对不确定度进行评估,如实反映测量的置信度和准确度。方法:采用ZORBAX Eclipse plus C18(2.01 mm×100 mm,3.5μm)色谱柱,70%甲醇和30%甲酸铵溶液(1 mmol·L-1,pH 10.0),流速0.2 mL·min-1。质谱条件:选用电喷雾离子源,在正离子电离模式下,采用多反应监测(MRM)的质谱扫描方式,测定雷贝拉唑以及内标兰索拉唑的母/子离子对分别为:m/z 360.1→242.2和m/z 370.1→252.2。测定雷贝拉唑含量后,建立数学模型,分析过程中各分量引起的不确定度,采用A类评定程序评价随机效应引起的不确定度,B类评定程序评价其他因素引起的不确定度。结果:置信概率P为95%时,血浆中雷贝拉唑可表示为:低浓度(10.08±3.32)ng·mL-1,中浓度(103.85±5.29)ng·mL-1,高浓度(741.22±34.29)ng·mL-1。结论:该方法适用于LC/MS/MS法测定人血浆中雷贝拉唑含量的不确定度评定,能为复杂生物样品分析过程的不确定度评定提供一定参考。
Objective：To analyze the measurement uncertainty in determination of rabeprazole in plasma by LC/MS/MS and identify the influencing factors for the uncertainty assessment.Methods：ZORBAX Eclipse plus C 18 column（2.01 mm × 100 mm,3.5 μm） was used,the mobile phase consisted of 70% methanol and 30% ammonium formate（1 mmol·L-1,pH 10.0）,and the flow rate was 0.2 mL·min-1.Mass spectrometry was performed in multiple reaction monitoring（MRM） mode,with m/z of 360.1→242.2 for rabeprazole and m/z of 370.1→ 252.2 for lansoprazole.A mathematical model was established to analyze the source of uncertainty.The uncertainty caused by various factors in the whole process of determination was evaluated.The uncertainty caused by random effects was evaluated with type A model and by others with type B model.The combined uncertainty was then obtained by synthesizing the uncertainties of various component variables.Results：The expanded uncertainty for low,medium and high level of rabeprazole can be expressed as（10.08 ± 3.32）,（103.85 ± 5.29） and（741.22 ± 34.29） ng·mL-1,respectively（P =95%）.Conclusions：The method is applicable for the uncertainty evaluation of rabeprazole determination in plasma.It provides an important reference for the uncertainty evaluation for the de-termination of complex biological samples.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2014年第2期210-214,共5页
Chinese Journal of New Drugs
