高效液相法定量分析戊二酸、戊二酸单甲酯和戊二酸二甲酯混合物

Quantitative Analysis of Glutaric Acid, mono-Methyl Glutarate and Dimethyl Glutarate by High Performance Liquid Chromatography

中文关键词:  高效液相色谱  戊二酸  戊二酸单甲酯  戊二酸二甲酯

英文关键词:HPLC  glutaric acid  mono-methyl glutarate  dimethyl glutarate

中文摘要:

      己二酸生产过程中产生大量的混和二元酸副产物，其中戊二酸含量最高.在分离混合二元酸纯化戊二酸的工艺中，酯化分离水解法是其中一种常用的工艺方法.水解反应体系中，除了主产物戊二酸之外，还有戊二酸单甲酯和戊二酸二甲酯两种主要杂质，通过高效液相色谱法，建立了一种便捷快速，可以同时准确定量戊二酸、戊二酸单甲酯和戊二酸二甲酯含量的分析方法，采用SunFire C₁₈色谱柱（5 μm，4.6 mm×150 mm）和乙腈/水/三氟醋酸（体积比为60∶40∶1）流动相，在柱温40℃和流速0.5 mL/min的条件下，实现了3种物质之间的基线分离.戊二酸、戊二酸单甲酯和戊二酸二甲酯的线性范围分别为6~3 000 mg/L（r=0.998 0）、3~1 500 mg/L（r=0.999 1）及3~1 500 mg/L（r=0.999 4），加标回收率（n=5）分别为105.79%（RSD=1.63%）、96.21%（RSD=7.28%）、93.10%（RSD=11.22%）.方法实现了同时测定戊二酸、戊二酸单甲酯和戊二酸二甲酯，为酯化分离水解工艺提供准确可靠的数据支持.

英文摘要:

      A large amount of binary acid mixture by-product is generated during the production process of adipic acid, in which the content of glutaric acid is the highest. Esterification-separation-hydrolysis method is one of the commonly used purification technological methods for glutaric acid in binary acid mixture. In addition to the main product glutaric acid, mono-methyl glutarate and dimethyl glutarate are the two important impurities in the hydrolysis reaction system. In this paper, a convenient, accurate quantitative analysis method is established using a HPLC with a SunFire C₁₈ column (5 μm, 4.6 mm×150 mm) and CH₃CN/H₂O/CF₃COOH (60∶40∶1,V/V/V) as the mobile phase. Glutaric acid, mono-methyl glutarate and dimethyl glutarate were baseline separated under a flow rate of 0.5 mL/min and a column temperature of 40 ℃. Under the optimal conditions, linear correlations were obtained in the mass concentration range of 6~3 000 mg/L (r=0.998 0) for glutaric acid, 3~1 500 mg/L (r=0.999 1) for mono-methyl glutarate, and 3~1 500 mg/L (r=0.999 4)for dimethyl glutarate. The recoveries (n=5) of glutaric acid, mono-methyl glutarate and dimethyl glutarate were 105.79% (RSD=1.63%), 96.21% (RSD=7.28%) and 93.10% (RSD=11.22%), respectively. Using this method the simultaneously determination of the contents of glutaric acid, mono-methyl glutarate and dimethyl glutarate, respectively can be carried out. Which can provide accurate and reliable data for the esterification-separation-hydrolysis process.