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L-谷氨酸钴配合物催化O2氧化四氢呋喃产物的分离与定性分析

发表时间:2014-04-15  浏览量:1969  下载量:660
全部作者: 张雪华,任水英,王猛,王静静,惠永海,王吉德
作者单位: 新疆大学化学化工学院,石油天然气教育部和自治区共建重点实验室;新疆产品质量监督检验研究院
摘 要: 利用反相高效液相色谱(reversed phase high performance liquid chromatography,RP-HPLC)技术和气相色谱质谱联用(gas chromatography-mass spectrometry,GC-MS)技术对L-谷氨酸钴配合物催化O2氧化四氢呋喃(tetrahydrofuran, THF)的产物进行分离和定性分析。考察流动相配比、pH值对RP-HPLC测试的影响。在优化条件下,通过保留时间对照法定性出催化氧化产物γ-丁内酯(γ-butyrolactone, GBL)、γ-羟基丁酸(γ-hydroxybutyrate, GHB)、2-羟基四氢呋喃、1,4-丁二酸、异丁酸酐和四氢糠醇6种产物。利用溶剂萃取法、柱层析法分离提纯目标产物之一GBL,并通过核磁共振(nuclear magnetic resonance, NMR)法对其进行验证,证明了测定结果的可靠性。
关 键 词: 分析化学;钴配合物;四氢呋喃;γ-丁内酯
Title: Separation and qualitative analysis of the products of catalytic oxidation of tetrahydrofuran with O2 by
Author: ZHANG Xuehua, REN Shuiying, WANG Meng, WANG Jingjing, HUI Yonghai, WANG Jide
Organization: Key Laboratory of Oil and Gas Fine Chemicals, Ministry of Education and Xinjiang Uyghur Autonomous Region, College of Chemistry and Chemical Engineering, Xinjiang University; Product Quality Supervision and Inspection Academy of Xinjiang
Abstract: The reversed phase high performance liquid chromatography (RP-HPLC) and gas chromatography-mass spectrometry (GC-MS) were used to the separation and qualitative analysis of the catalytically oxidative products of tetrahydrofuran (THF) by L-glutamic acid cobalt complex with O2. The effects of mobile phases and pH values were investigated for optimization in RP-HPLC on separation. γ-butyrolactone (GBL), γ-hydroxybutyrate (GHB), 2-hydroxyl tetrahydrofuran, 1,4-succinic acid, isobutyric anhydride and tetrahydrofurfuryl alcohol were detected by retention time comparing method under the optimal conditions. In addition, one of the target products GBL was separated and purified by the methods of solvent extraction and column chromatography, and was verified by nuclear magnetic resonance (NMR), which demonstrated that the qualitative results were reliable.
Key words: analytical chemistry; cobalt complex; tetrahydrofura; γ-butyrolactone
发表期数: 2014年4月第7期
引用格式: 张雪华,任水英,王猛,等. L-谷氨酸钴配合物催化O2氧化四氢呋喃产物的分离与定性分析[J]. 中国科技论文在线精品论文,2014,7(7):643-648.
 
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