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

KeyWord:cobalt£¨¢ò£© complex  tetrahydrofuran  reversed phase high performance liquid chroma-tography  ¦Ã-butyrolactone

Abstract:

      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£©,¦Ã-butyrolactone£¨GBL£© and 1,4-succinic acid in the catalytically oxidative products of tetrahydrofuran£¨THF£©,which was oxydized with molecular oxygen catalyzed by cobalt£¨¢ò£© complex.After centrifuged and evaporated,the reaction mixtures were separated on an Inertsil ODS-3 C18 column£¨250 mm¡Á4.6 mm,5 ¦Ìm£© 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.