高温1HNMR鉴别8种海参硫酸软骨素  

Identification of Eight Species of Sea Cucumber Chondroitin Sulfates by High Temperature 1H NMR

作　　者：陈士国[1] 李国云[1] 尹利昂[1] 黄万成 董平[1] 徐杰[1] 常耀光[1] 薛长湖[1] 

机构地区：[1]中国海洋大学食品科学与工程学院,山东青岛266003 [2]獐子岛渔业集团技术研发部,辽宁大连116650

出　　处：《分析测试学报》2010年第8期782-786,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(30871944)

摘　　要：提取了8种海参中的粗多糖,经DEAE-52阴离子交换柱分离纯化得到其中的海参硫酸软骨素(SC-CHS),除日本刺参CHS外其余均为首次获得的海参多糖。对获得的SC-CHS进行分子量、单糖组成及硫酸基含量等基本性质分析后,利用高温1HNMR对SC-CHS结构进行初步鉴别。结果表明,高温条件下SC-CHS的1HNMR图谱具有较好的分辨度。对其支链硫酸化岩藻糖的异头氢进行归属和比较,并以此为指标鉴别不同种类海参硫酸软骨素的结构差异,建立了一种以海参硫酸软骨素结构特征为指标的海参指纹图谱;初步探讨了不同海域生长的海参中硫酸软骨素支链岩藻糖硫酸基的特点,比较发现:寒带海域海参的硫酸软骨素岩藻糖上硫酸基取代以2,4-di OSO3、3,4-di OSO3双取代为主,含部分4-OSO3单取代;温带海域海参以2,4-di OSO3双取代为主,含部分4-OSO3单硫酸基取代;热带亚热带海域海参以2,4-di OSO3双取代和4-OSO单取代为主。这将为海参构效关系的进一步分析鉴定提供理论依据。Crude polysaccharides, extracted from eight species of sea cucumbers were separated and purified through the cellulose DEAE-52 anion-exchange column to obtain the corresponding sea cucumber chondroitin sulfates （SC -CHS）. The chemical properties of SC -CHS, such as the monosaccharide composition, the sulfate content and the molecular weight were determined and their structures were identified by high temperature 1H NMR. The result showed that the high temperature I H NMR spectra of SC - CHS were better resolved, particularly the anomer hydrogen signals of their fucose branches. A fingerprint of sea cucumbers based on the indices of the anomer hydrogen signals of fueose branches was thus established for the identification of different species of SC - CHS. By reference of the characteristics of the growth of sea cucumbers in different sea regions, it was found that the fucoses of SC - CHS of sea cucumber living in frigid waters were mainly substituted with disulphate, 2, 4-di OS03, 3, 4-di OSO3, and some were substituted with monosulphate, 4-OSO3 ; Those in temperate waters were mainly substituted with 2, 4-di OSO3 and some were substituted with 4-OS03 ; and those in tropical and subtropical waters were mainly substituted with 2, 4-di OSO3 and 4-OSO3. The above results may provide theoretical basis for further studying of the structure-activity relationship of SC - CHS.

关 键 词：海参硫酸软骨素 组成分析 核磁共振 鉴别 

分 类 号：O482.532[理学—固体物理] Q915.821[理学—物理]