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

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Sun Fire C_(18)色谱柱(5μm,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 m L/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.

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 CH3 CN/H2O/CF3 COOH （60 ： 40 ： 1, V/V/V） as the mobile phase. Glutaric a cid,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% ） , 9 6.21% （RSD = 7 .2 8%） 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.