摘要
建立了一种同时检测奈玛特韦、利托那韦、莫诺拉韦、奥司他韦和达卡他韦5种小分子抗病毒药物的高效液相色谱-质谱分析方法。样品经甲醇溶解超声提取后,经CNWShell C18 Core-Shell色谱柱(100×2.1 mm,2.6μm)分离,以0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,电喷雾正离子模式下,同时采用多反应监测(MRM)和二级全扫(MS^(2))模式扫描分析。5种抗病毒药物在一定浓度范围内线性良好;检出限(S/N=3)为0.15~0.5μg/g;定量限(S/N=10)为0.5~1.2μg/g;加标平均回收率为90.0%~97.4%,精密度(n=6)均小于5%。采用本方法对10份样品进行测定,发现7份样品不含标示的有效成分奈玛特韦,有效成分利托那韦含量远低于标示含量,且检出奥司他韦或达卡他韦等非法添加化学成分。所建立方法灵敏、快速、可靠,可用于药品制剂中5种抗病毒药物的定性及定量分析。
A HPLC-MS/MS method was established for the simultaneous detection of five small molecule antivirals,namely nirmatrelvir,ritonavir,molnupiravir,oseltamivir and daclatasvir.Samples were extracted by methanol with ultrasound extraction,and separated on a CNWShell C18 Core-Shell column(100×2.1 mm,2.6 μm) by gradient elution using 0.1% formic acid solution and methanol as the mobile phase.The electrospray ion source was operated in the positive ion mode and both multiple reaction monitoring and product ion scanning were used in this method.There were good linearities for five small molecule antivirals in their linear ranges.The limits of detection(LODs) were 0.15-0.5 μg/g and the limits of quantitation were 0.5-1.2 μg/g.Average recoveries of three spiked levels ranged from 90% to 97.4%(n=6) with the relative standard deviations(RSDs) less than 5%.The method was used to test 10 samples and 7 samples were found not to contain the active ingredient nirmatrelvir as labelled.Active ritonavir was found to be much lower than labelled,and illegally added chemicals such as oseltamivir or daclatasvir were detected.The method was proved to be sensitive,rapid and accurate for the qualitative and quantitative analysis of 5 small-molecule antivirals.
作者
庄玥
黄艳婷
蔡霞
邱蕴绮
罗卓雅
ZHUANG Yue;HUANG Yanting;CAI Xia;QIU Yunqi;LUO Zhuoya(Guangdong Institute for Drug Control,NMPA Key Laboratory for Rapid Testing Technology of Drugs,National Medical Products Administration,Guangzhou 510663)
出处
《分析科学学报》
CAS
CSCD
北大核心
2024年第1期65-69,共5页
Journal of Analytical Science
基金
广东省药品监督管理局科技创新项目(2021YDZ07)
广东省医学科学技术研究基金项目(B2021409、B2020185)
广东省中医药局科研项目(20221055)。