中国临床药理学杂志2025，Vol.41Issue(3)：393-396,4.DOI:10.13699/j.cnki.1001-6821.2025.03.019
用LC-MS/MS法测定人血浆中乌帕替尼的浓度
Determination of upatinib honcentration in human plasma by LC-MS/MS method
摘要
Abstract
Objective To establish liquid chromatography-mass spectrometry(LC-MS/MS)quantitative method for determining the blood concentration of Upatinib in human plasma.Methods Upatinib 15N-d2 was used as the internal standard,and acetonitrile was used for protein precipitation pretreatment.Separate using a Waters BEH C18(2.4 mm × 50.0 mm,1.7 μm)chromatographic column;acetonitrile(containing 0.1％formic acid)and 0.1％formic acid aqueous solution were used as mobile phases,with gradient elution at a flow rate of 0.3 mL·min-1 and column temperature of 40 ℃.The ion pair used for quantitative analysis was m/z 388.90→255.90(Upatinib)and m/z 384.10→256.20(Upatinib-15N-d2,internal standard)respectively by using an electrospray ion source and positive ion multi reaction monitoring mode scanning.The specificity,standard curve,quantitative cutoff,precision,recovery rate,dilution reliability,matrix effect and stability of the method were examined.Results There is no mutual interference between endogenous components,internal standards and Upatinib in plasma.The linear relationship between the mass concentration of 0.75-60.00 ng·mL-1Upatinib and peak area is good(r=0.998 6),the standard curve equation was y=8.24 × 10-2x+0.61 × 10-2,with a lower limit of quantification of 0.75 ng·mL-1.The intra-day and inter-day batch precision coefficients of variation of the quality control samples are both ≤5.3％.The accuracy of the sample concentration after 5-fold dilution is 1.1％,and the coefficient of variation is 4.6％.The matrix effect factors of low and high-quality plasma quality control samples are 1.1 and 1.0,respectively.The stability of whole blood samples and plasma samples meets the requirements of biological sample analysis.Conclusion The method used is simple,rapid,highly accurate,and sensitive,and is suitable for determining the concentration of Upatinib in human plasma.It can be used for pharmacokinetic and bioequivalence studies of Upatinib in healthy individuals.关键词
乌帕替尼/液相色谱-质谱联用/血药浓度Key words
Upatinib/liquid chromatography-mass spectrometry/human plasma分类
医药卫生引用本文复制引用
高瑶瑶,田晓彤,王茉莉,闫凯,王柳,李姿,高燕霞..用LC-MS/MS法测定人血浆中乌帕替尼的浓度[J].中国临床药理学杂志,2025,41(3):393-396,4.基金项目
中央引导地方科技发展资金资助项目(226Z2402G) （226Z2402G）
