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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。
A method for the determination of succinic acid, glutaric acid and adipic acid in cyclohexane oxidation products by high performance liquid chromatography was established. The column was ZORBAX SAX 4.6 mm × 250 mm 5 μm and the mobile phase was methanol: 50 mmol / L KH2PO4 aqueous solution = 5:95 (V / V). The column temperature was 25 ℃ and the flow rate was 1.0 mL / min. Results The linear relationships of succinic acid, glutaric acid and adipic acid in the range of 10 ~ 200μg / mL were good (r = 0.9998, 0.9996, 0.9997). The detection limits of the three dibasic acids were 1.50μg / mL. The spiked recoveries of different grades were between 89.8% and 102.6%, and the relative standard deviations (RSDs) ranged from 1.6% to 4.5% (n = 6). The method has been applied to the quantitative analysis of organic dibasic acids in cyclohexane oxidation products.