HPLC-DAD法测定环己烷氧化产物中的二元酸  

Determination of the dicarboxylic acid of the cyclohexane oxidation products by high performance liquid chromatography with diode array detector

作　　者：李建[1] 刘燕[1] 干丰丰 杨运信[1] 

机构地区：[1]中国石化上海石油化工研究院,上海201208

出　　处：《分析试验室》2017年第6期726-728,共3页Chinese Journal of Analysis Laboratory

摘　　要：建立了高效液相色谱法测定环己烷氧化产物中丁二酸、戊二酸和己二酸含量的方法。色谱柱为ZORBAX SAX 4.6 mm×250 mm 5μm,流动相为甲醇:50 mmol/L KH2PO4水溶液=5:95(V/V),柱温:25℃,流速:1.0 mL/min。结果丁二酸、戊二酸和己二酸在10~200μg/mL范围内线性关系良好(r=0.9998,0.9996,0.9997),3种二元酸的检出限均为1.50μg/mL,目标分析物不同级别加标回收率在89.8%~102.6%之间,相对标准偏差(RSD)在1.6%~4.5%之间(n=6)。方法已用于环己烷氧化产物中有机二元酸的定量分析。In this study, a new analytical method was proposed to simuhaneously determine succinic acid （SA）, glutaric acid （GA） and adipic acid （AA） in product of cyclohexane oxidation. The solvent, column, and mobile conditions which affected the result of separation were studied. Using ZORBAX SAX column, linear correlation coefficient of the method of succinic acid, glutaric acid and adipic acid were 0. 9994,0. 9997 and 0. 9992, respectively. The average recovery of succinic acid, glutaric acid and adipic acid spiked in samples ranged from 89.8% to 102.6%. And the relative standard deviations （RSD） were between 1.6% and 4.5% （n = 6）. The method has high sensitivity and low detection limit. And the method could rapidly and accurately meet the analysis requirements of succinic acid, glutaric acid and adipic acid in product of cyclohexane oxidation.

关 键 词：HPLC-DAD 丁二酸 戊二酸 己二酸 

分 类 号：TQ014[化学工程] O657.8[理学—分析化学]