叶酸有关物质的液相色谱-质谱联用分离与鉴定  

Separation and identification of folic acid and its related substances by liquid chromatography-mass spectrometry

作　　者：宁曼如 徐柯卉 杭太俊[1] 宋敏[1] NING Manru;XU Kehui;HANG Taijun;SONG Min(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]中国药科大学药物分析系,南京210009

出　　处：《中国药科大学学报》2025年第1期56-64,共9页Journal of China Pharmaceutical University

摘　　要：用ODS色谱柱和10mmol/L乙酸铵缓冲溶液-甲醇流动相(pH6.3)将叶酸有关物质进行线性梯度洗脱分离,电喷雾正离子化-四极杆-飞行时间质谱(ESI-Q-TOF/MS)高分辨测定各有关物质母离子及其子离子的准确质荷比和元素组成,通过质谱解析、有机反应机制分析、或对照品对照鉴定它们的结构。在所建立的LC-ESI-Q-TOF/MS条件下,叶酸及其有关物质分离良好,检测并鉴定叶酸及其强制降解试验样品中23个主要有关物质,其中2个为《欧洲药典》规定的已知杂质,4个与文献报道已知杂质一致,其余17个为新鉴定的未知杂质。鉴定结果可为叶酸质量控制提供参考依据。The related substances in folic acid were separated on an ODS column by linear gradient elution using the mixture of 10 mmol/L ammonium acetate buffer solution and methanol(pH 6.3)as the mobile phase,and their accurate mass-charge ratio and elemental composition of parent and product ions were detected by electrospray ionization quadrupole time-of-flight mass spectrometry(ESI-Q-TOF/MS).The structures of the related substances were then determined by MS spectra elucidation,organic reaction mechanism analysis,or reference substances confirmation.Under the established LC-ESI-Q-TOF/MS conditions,folic acid and its related substances were adequately separated.Among the 23 main related substances found,2 were known impurities listed in European Pharmacopoeia,4 were consistent with the literature reports,and the remaining 17 were newly identified unknown related substances in this study.The results of separation and identification can provide some useful reference for the quality control of folic acid.

关 键 词：叶酸 有关物质 降解产物 结构鉴定 液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]