草酸二甲酯和草酸的反相高效液相色谱分析

摘要

建立了反相高效液相色谱定量分析草酸二甲酯生产过程中的草酸二甲酯及草酸含量的方法。采用带有紫外检测器的Shimadzu LC-20A型高效液相色谱仪,C18色谱柱(4.6 mm×150 mm,5 μm),流动相是体积比为60:40的乙腈-磷酸水溶液(pH=2.7),流速为0.7 mL/min,柱温25 ℃,254 nm波长下紫外检测。探讨了pH值及其它条件对色谱分离的影响。该方法测得的草酸及草酸二甲酯线性回归曲线的相关系数分别为0.9996和0.9998,相对标准偏差为0.8%~1.0%,满足定量分析要求。

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	石蕾
	李伟松
	师浩淳
	许春建

关键词：反相高效液相色谱草酸二甲酯草酸

Abstract：

A reversed-phase high performance liquid chromatographic (RP-HPLC) separation method with UV photodiode-array detection has been developed for the simultaneous determination of dimethyl oxalate and oxalic acid. The chromatographic analysis was carried out after their elution with acetonitrile and phosphoric acid solution (pH=2.7) whose volume ratio was 60:40 from C18 stationary phase (4.6 mm×150 mm, 5 μm). The flow rate of the mobile phase was 0.7 mL/min for the whole run. The column temperature was 25 ℃ and the detection wavelength was 254 nm. Effects of pH and other conditions on the separation were investigated. Under the optimized conditions, the liner correlation coefficients of oxalic acid and dimethyl oxalate were 0.9996 and 0.9998, respectively. The relative standard deviations were 0.8%—1.0%. This method was suitable for the determination of dimethyl oxalate and oxalic acid.

Keywords： RP-HPLC； dimethyl oxalate； oxalic acid

Received 2014-04-08;

Corresponding Authors: 许春建,E-mail:cjxu@tju.edu.cn。 Email: cjxu@tju.edu.cn

About author: 石蕾(1987-),女,硕士研究生, 从事化工分离方向研究。

引用本文:

石蕾, 李伟松, 师浩淳, 许春建.草酸二甲酯和草酸的反相高效液相色谱分析[J]. 化学工业与工程, 2016,33(2): 91-95

Shi Lei, Li Weisong, Shi Haochun, Xu Chunjian.Determination of Dimethyl Oxalate and Oxalic Acid by Reversed-Phase High Performance Liquid Chromatography[J]. Chemcial Industry and Engineering, 2016,33(2): 91-95

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