A rapid method of microwave assisted acid hydrolysis was established to prepare κ-carra-oligosaccharides. The optimal hydrolysis condition was determined by an orthogonal test. The degree of polymerization （DP） of ...A rapid method of microwave assisted acid hydrolysis was established to prepare κ-carra-oligosaccharides. The optimal hydrolysis condition was determined by an orthogonal test. The degree of polymerization （DP） of oligosaccharides was detected by high performance thin layer chromatography （HPTLC） and polyacrylamide gel electrophoresis （PAGE）. Considering the results of HPTLC and PAGE, the optimum condition of microwave assisted acid hydrolysis was determined. The concentration of κ-carrageenan was 5 mgmL-1; the reaction solution was adjusted to pH 3 with diluted hydrochloric acid; the solution was hydrolyzed under microwave irradiation at 100 ℃ for 15 min. Oligosaccharides were separated by a Superdex 30 column （2.6 cm × 90 em） using AKTA Purifier UPC100 and detected with an online refractive index detector. Each fraction was characterized by electrospray ioni- zation mass spectrometry （ESI-MS）. The data showed that odd-numbered κ-carra-oligosaccharides with DP ranging from 3 to 21 could be obtained with this method, and the structures of the oligosaccharides were consistent with those obtained by traditional mild acid hydrolysis. The new method was more convenient, efficient and environment-friendly than traditional mild acid hydrolysis. Our results provided a useful reference for the preparation of oligosaceharides from other polysaccharides.展开更多
A pressured microwave-assisted hydrolysis （PMAH） technique has been developed for hydrolyzing the crude glycyrrhizic acid （GA） extracted from licorice root to prepare glycyrrhetinic acid （GRA）. In order to optim...A pressured microwave-assisted hydrolysis （PMAH） technique has been developed for hydrolyzing the crude glycyrrhizic acid （GA） extracted from licorice root to prepare glycyrrhetinic acid （GRA）. In order to optimize the efficiency of PMAH, several experimental parameters were investigated, including liquid-solid ratio, hydrolysis time, sulfuric acid concentration and hydrolysis temperature. The optimized hydrolysis conditions were as follows：pressured microwave-assisted hydrolysis of crude GA for 21 min （taking 15 min to reach 150 ℃, and holding it for 6 rain） at 150 ℃ （at a radiation power of 450 W） in 3%-5% sulfuric acid solution with the liquid-solid （ml.g-1 crude GA） ratio of 25 ： 1. As a result of the considerable saving in time and higher product yields （up to 90%）, PMAH was proved more effective than conventional methods.展开更多
基金supported by the Special Fund for Marine Scientific Research in the Public Interest (201005024)NSFC-Shandong Joint Fund for Marine Science Research Centers (U1406402)+1 种基金Qingdao Science & Technology Project (11-2-2-1-hy)National Science & Technology Support Program of China (2013BAB 01B02)
文摘A rapid method of microwave assisted acid hydrolysis was established to prepare κ-carra-oligosaccharides. The optimal hydrolysis condition was determined by an orthogonal test. The degree of polymerization （DP） of oligosaccharides was detected by high performance thin layer chromatography （HPTLC） and polyacrylamide gel electrophoresis （PAGE）. Considering the results of HPTLC and PAGE, the optimum condition of microwave assisted acid hydrolysis was determined. The concentration of κ-carrageenan was 5 mgmL-1; the reaction solution was adjusted to pH 3 with diluted hydrochloric acid; the solution was hydrolyzed under microwave irradiation at 100 ℃ for 15 min. Oligosaccharides were separated by a Superdex 30 column （2.6 cm × 90 em） using AKTA Purifier UPC100 and detected with an online refractive index detector. Each fraction was characterized by electrospray ioni- zation mass spectrometry （ESI-MS）. The data showed that odd-numbered κ-carra-oligosaccharides with DP ranging from 3 to 21 could be obtained with this method, and the structures of the oligosaccharides were consistent with those obtained by traditional mild acid hydrolysis. The new method was more convenient, efficient and environment-friendly than traditional mild acid hydrolysis. Our results provided a useful reference for the preparation of oligosaceharides from other polysaccharides.
基金Supported by the Yunnan Provincial Department of Education Key Foundation (07Z10311)
文摘A pressured microwave-assisted hydrolysis （PMAH） technique has been developed for hydrolyzing the crude glycyrrhizic acid （GA） extracted from licorice root to prepare glycyrrhetinic acid （GRA）. In order to optimize the efficiency of PMAH, several experimental parameters were investigated, including liquid-solid ratio, hydrolysis time, sulfuric acid concentration and hydrolysis temperature. The optimized hydrolysis conditions were as follows：pressured microwave-assisted hydrolysis of crude GA for 21 min （taking 15 min to reach 150 ℃, and holding it for 6 rain） at 150 ℃ （at a radiation power of 450 W） in 3%-5% sulfuric acid solution with the liquid-solid （ml.g-1 crude GA） ratio of 25 ： 1. As a result of the considerable saving in time and higher product yields （up to 90%）, PMAH was proved more effective than conventional methods.
