中国药业2023，Vol.32Issue(24)：86-89,4.DOI:10.3969/j.issn.1006-4931.2023.24.020
柠檬酸三甲酯碱降解途径及其杂质结构初步解析
Alkaline Degradation Pathway of Trimethyl Citrate and Preliminary Analysis of Its Impurity Structure
摘要
Abstract
Objective To analyze the degradation pathway of trimethyl citrate and its alkaline degradation products,and to preliminarily analyze the structure of its main impurities.Methods Liquid-chromatography ion trap time-of-flight mass spectrometry(LC-IT-TOF/MS)method was adopted.The chromatographic column was Thermo Hypersil GOLD Dim column(250 mm×4.6 mm,5 μm),the mobile phase was acetonitrile-water(10 ∶90,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 214 nm,the column temperature was 35℃,and the injection volume was 20 μL.Electro-spray ionization(ESI)was adopted,the interface voltage was 4.5 kV,the scanning range of primary mass spectrometry was m/z at 10 to 1 500,the automatic grading range was m/z at 50 to 1 000,the atomized gas was nitrogen with a flow rate of 1.5 L/min,the drift tube temperature was 200℃,the dry gas was nitrogen with a flow rate of 10 L/min,the temperature of the heating module was 200℃,the collision gas was argon,and the detector voltage was 1.52 kV.Results It was preliminarily confirmed that the structures of impurities a and b were consistent with those of monomethyl citrate and dimethyl citrate,respectively,and a alkali degradation pathway of trimethyl citrate was proposed.Conclusion The established method can be used to study the alkali degradation products and degradation pathways of trimethyl citrate,which can provide a reference for improving the synthesis process and product quality of trimethyl citrate.关键词
柠檬酸三甲酯/液相色谱-离子阱-飞行时间质谱联用法/碱降解/杂质/结构解析Key words
trimethyl citrate/liquid-chromatography ion trap time-of-flight mass spectrometry/alkaline degradation/impurity/structural analysis分类
医药卫生引用本文复制引用
耿燕,李香荷,王月英,王永欣,张冬..柠檬酸三甲酯碱降解途径及其杂质结构初步解析[J].中国药业,2023,32(24):86-89,4.基金项目
河北省重点研发计划项目[21372002D]. （）
