分子氧氧化四氢呋喃产物中γ-丁内酯、4-羟基丁酸与1,4-丁二酸的反相高效液相色谱法测定

RP- HPLC Determination of Ester and Organic Acids in the Oxidative Products of Tetrahydrofuran with Molecular Oxygen

建立了钴（Ⅱ）配合物催化分子氧氧化四氢呋喃（THF）产物中的γ-丁内酯（GBL）、γ-羟基丁酸（GHB）和1,4-丁二酸的反相高效液相色谱（RP-HPLC）分析方法.反应产物经离心、旋蒸后,以InertsilODS-3 C18色谱柱（250 mm×4.6 mm,5μm）进行分离,以0.01％甲酸-甲醇溶液为二元流动相,按流速为0.80 mL/min进行等度洗脱,采用二极管阵列检测器（波长220 nm）检测,外标法定量.实验结果表明,3种目标化合物在10.0～1 000 mg/L质量浓度范围内呈良好的线性关系,相关系数均不小于0.999 8,方法的检出限为0.019 ～0.052 mg,定量下限为0.064～0.173 mg,3个加标水平下3种待测物的回收率为95％～ 107％,相对标准偏差（RSD）为0.09％～4.7％.该法简便、准确,可用于THF氧化产物中3种目标化合物的分析及催化剂效果评价.

A reversed phase high performance liquid chromatographic （RP-HPLC） method was developed for the separation,quanlitative and quantitative analysis of 4-hydroxy butyric acid （GHB）,γ-butyrolactone（GBL） and 1,4-succinic acid in the catalytically oxidative products of tetrahydrofuran（THF）,which was oxydized with molecular oxygen catalyzed by cobalt（Ⅱ） complex.After centrifuged and evaporated,the reaction mixtures were separated on an Inertsil ODS-3 C18 column（250 mm ×4.6 mm,5 μm） by isocratic elution with 0.01％ formic acid-methanol as mobile phase at a flow rate of 0.80 mL/min.The detection wavelength was set at 220 nm.The identification of three substances were achieved by the retention times and the PAD spectra.Quantification analysis was performed by the external standard method under the optimal conditions.The calibration curves of three compounds were linear in the range of 10.0-1 000 mg/L with correlation coefficients not less than 0.999 8.The detection limits （LODs） were in the range of 0.019-0.052 mg and the quantitation limits（LOQs） were 0.064-0.173 mg.The average recoveries at three spiked levels ranged from 95％ to 107％ with relative standard deviations（RSDs） of 0.09％-4.7％.The method was applied in the real sample,and the results indicated that the method was simple,sensitive and accurate,and was suitable for the analysis of GHB,GBL and 1,4-succinic in the oxidative products of THF and the evaluation of catalysts.