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液相色谱串联质谱法测定人血浆中巴洛沙韦酸浓度OA

Concentration Determination of Baloxavir Acid in Human Plasma by LC-MS/MS Method

中文摘要英文摘要

目的 建立测定人血浆中巴洛沙韦酸浓度的液相色谱串联质谱(LC-MS/MS)法.方法 血浆样品经甲醇沉淀蛋白后,以度鲁特韦为内标.色谱柱为Phenomenex Luna®-C8 柱(50mm×2.1mm,3μm),流动相为甲醇-0.1%甲酸水溶液(梯度洗脱),流速为0.35 mL/min,柱温为 25℃,进样量为 10 μL,采用电喷雾电离离子源,正离子模式下进行多反应监测,用于分析的离子对质荷比(m/z)分别为 484.20→247.20(巴洛沙韦酸)、420.00→277.10(度鲁特韦).结果 巴洛沙韦酸的质量浓度在 0.50~80.00 ng/mL范围内与待测物和内标峰面积比值的线性关系良好(r=0.9993,n=8),定量下限为 0.50 ng/mL,日内、日间精密度的RSD分别为 3.27%~5.87%(n=3)、0.62%~9.12%(n=3),稳定性试验的RSD均小于 5%,提取回收率为 89.90%~96.94%,基质效应为 100.76%~115.00%.结论 该方法操作简便、专属性强、准确度高、稳定性好,可用于测定人血浆中巴洛沙韦酸的浓度.

Objective To establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining the concentration of baloxavir acid in human plasma.Methods After protein precipitation with methanol,plasma samples were analyzed with dolutegravir as the internal standard.The chromatographic column was Phenomenex Luna®-C8 column(50 mm×2.1 mm,3 μm),the mobile phase was methanol-0.1%aqueous formic acid solution(gradient elution),the flow rate was 0.35 mL/min,the column temperature was 25℃,and the injection volume was 10 μL.Electrospray ionization was used with a positive ion mode for multiple reaction monitoring.The ion pairs for analysis with mass-to-charge ratios(m/z)of 484.20 → 247.20(baloxavir acid)and 420.00 → 277.10(dolutegravir)were adopted.Results The linear range of baloxavir acid was 0.50-80.00 ng/mL(r=0.999 3,n=8).The lower limit of quantification was 0.50 ng/mL.The RSDs of the intra-day and inter-day precision tests were in the ranges of 3.27%-5.87%(n=3)and 0.62%-9.12%(n=3),respectively.The RSD of the stability test was lower than 5%.The extraction recovery rate was in the range of 89.90%-96.94%,and the matrix effect was in the range of 100.76%-115.00%.Conclusion This method is simple,highly specific,accurate,and stable,which can be used to determine the concentration of baloxavir acid in human plasma.

何文娟;崔文彦;安雪松;张心慧;李梦豪;李德强;刘秀菊

河北医科大学第二医院,河北 石家庄 050000河北医科大学,河北 石家庄 050017河北医科大学,河北 石家庄 050017河北医科大学,河北 石家庄 050017河北医科大学,河北 石家庄 050017河北医科大学第二医院,河北 石家庄 050000河北医科大学第二医院,河北 石家庄 050000

医药卫生

液相色谱串联质谱法巴洛沙韦酸血药浓度

LC-MS/MSbaloxavir acidblood drug concentration

《中国药业》 2026 (3)

76-80,5

河北省卫生健康委员会医学科学研究课题计划项目[20211192].

10.3969/j.issn.1006-4931.2026.03.014

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