乙醇酸甲酯水解制乙醇酸中组分的测定

Simultaneous Analysis of Compounds for Methyl Glycolate to Glycolic Acid by High-performance Liquid Chromatography

建立了乙醇酸甲酯水解制乙醇酸中组分及含量的高效液相色谱快速测定方法。采用超高效液相色谱与二极管阵列检测器/四级杆-飞行时间串联质谱（UPLC-PDA/Q-To F MS/MS）联用技术对乙醇酸产品进行定性分析,高效液相色谱进行检测,外标法定量。本方法,乙醇酸和乙醇酸甲酯在0.01~100 mg/m L范围内呈现良好的线性关系（r2〉0.999）;检出限分别为0.0102 mg/m L和0.0208 mg/m L;加标回收率为95%~105%;相对标准偏差（RSD）为0.01%~0.86%。本方法已用于乙醇酸工业生产的过程分析及乙醇酸产品的质量控制。

A novel method was presented for identification and quantification of compounds in Glycolic Acid（GA）by using high-performance liquid chromatography.Methyl glycolate（MG） and glycolic acid dimer were identified as impurities in GA products by ultra-performance liquid chromatography with photo-diode array and quadrupole-time of flight mass spectrometry（UPLC-PDA/Q-To F MS/MS）.High-performance liquid chromatography-diode array detector（HPLC-DAD） was used for quantification analysis of compounds in GA.External standard method was applied in this study.The linear range of GA and MG was 0.01 ~ 100 mg/m L（r2 〉0.9999）,limits of detection（LOD,S/N =3） of GA and MG were 0.0102 mg/m L and 0.0208 mg/m L,respectively,and recoveries of GA and MG were between95% ~ 105%.Relative standard deviations were below 0.01% ~ 0.86% for both GA and MG.Processing condition optimization,process control and quality control of GA production could be applied effectively by using this method.