富马酸替诺福韦双特戊酯有关物质的鉴定

目的:采用色谱-质谱联用技术对富马酸替诺福韦双特戊酯中有关物质进行结构鉴定。方法:采用BDS Hypersil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.2%醋酸铵溶液,梯度洗脱,对富马酸替诺福韦双特戊酯有关物质进行分离;LC-PDA测定各有关物质的UV吸收,甲醇辅助电喷雾正离子化LC-TOF和LC-MS/MS分别测定各有关物质的精密质量和二级质谱。结果:检测到富马酸替诺福韦双特戊酯中存在多个有关物质,其中仅3个的含量在0.1%以上,并鉴定出4个主要有关物质的结构。结论:色谱-质谱联用技术能够有效地鉴定药物中的有关物质,富马酸替诺福韦双特戊酯有关物质鉴定结果对其质量控制和工艺优化提供了参考依据。

Identification of the related substances in tenofovir dipivoxil fumarate with hyphenated techniques

Objective:To identify the related substances in tenofovir dipivoxil fumarate by hyphenated techniques.Methods:An LC-PDA-MS/MS method was established by using acetonitrile-0.2% ammonium acetate as the mobile phase with gradient elution on a BDS Hypersil C18(250 mm×4.6 mm,5 μm) column with 0.2 mL·min-1 methanol aided electro-spray positive ionization.The UV spectrum,accurate molecular weight and formula,and product ion MS spectrum of each related substance was obtained by LC-PDA,LC-TOF and LC-MS/MS,respectively.Results:Several related substances were found in tenofovir dipivoxil fumarate with only 3 of them had the area normalization content over 0.1%,and 4 of them were identified and elucidated.Conclusion:The hyphenated LC-MS method is useful for the determination and identification of related substances in pharmaceuticals.Identification of the related compounds in tenofovir dipivoxil fumarate is valuable for its manufacturing process optimization and quality control.