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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 uncertainty of the determination of rabeprazole in plasma by LC-MS, identify the influencing factors, evaluate the uncertainty and accurately reflect the confidence and accuracy of the measurement. Methods: The chromatographic column of ZORBAX Eclipse plus C18 (2.01 mm × 100 mm, 3.5 μm) was used. The flow rate was 0.2 mL · min-1 with 70% methanol and 30% ammonium formate solution (1 mmol·L-1, pH 10.0) Mass spectrometry conditions: The electrospray ionization source was used. In positive ionization mode, the mass spectrometry scan mode of multiple reaction monitoring (MRM) was used to determine the parent / daughter ion pair of rabeprazole and the internal standard lansoprazole as follows: m / z 360.1 → 242.2 and m / z 370.1 → 252.2. The determination of rabeprazole content, the establishment of mathematical models to analyze the uncertainty caused by the various components of the process, the use of A-type assessment program to evaluate the random effects caused by uncertainty, B-type assessment program to assess the uncertainty caused by other factors. RESULTS: Rabeprazole in plasma was 95% lower than that in low concentration (10.08 ± 3.32) ng · mL-1, middle concentration (103.85 ± 5.29) ng · mL-1 and high concentration (741.22 ± 34.29) ng · mL-1. Conclusion: This method is suitable for evaluating the uncertainty of the determination of rabeprazole in human plasma by LC / MS / MS. It can provide some references for the evaluation of the uncertainty of complex biological samples.