呋喃酮和酱油酮的填充柱超临界流体色谱对映体拆分  

Resolution of Furaneol and Homofuraneol by Packed Column Supercritical Fluid Chromatography

作　　者：孙蕾[1] 都荣强[1] 谢建春[1] 孙宝国[1] 

机构地区：[1]北京工商大学北京市食品风味化学重点实验室,北京100048

出　　处：《食品科学》2013年第24期77-82,共6页Food Science

基　　金：国家自然科学基金面上项目(31171755);北京市自然科学基金面上项目(21222013);北京市自然科学基金项目(KZ201010011011);北京市教委科技发展计划重点

摘　　要：采用填充柱超临界流体色谱对外消旋呋喃酮和酱油酮进行手性拆分。首先在分析型条件下,考察手性柱种类、改性剂种类和含量、柱温、柱压、流速等参数对容量因子、选择性因子、分离度的影响,获得拆分呋喃酮的较佳条件为手性柱Chiralpak AD-H、柱温30℃、柱压10MPa、改性剂1.0%(V/V)甲醇、流速1.5mL/min,得到分离度1.54;拆分酱油酮的较佳条件为手性柱Chiralpak AD-H、柱温33℃、柱压13MPa、改性剂1.5%(V/V)乙醇、流速1.5mL/min,得到分离度1.51。利用较佳条件进行制备规模放大,获得呋喃酮和酱油酮的对映体产品,光学纯度(对映体过量,e.e,%)均≥90%,回收率≥70%。对映体产品的获得可为探讨手性呋喃酮和酱油酮应用于食品加香的可行性提供基础条件。The separation of racemic furaneol and homofuraneol by packed column supercritical fluid chromatography was studied. First, on an analytical scale, the effects of chiral column type, modifier solvent type and modifier solvent content in mobile phase, column temperature, column pressure and flow rate on capacity factor （k＇）, selectivity factor （a） and resolution factor （Rs） were investigated. The optimum conditions for resoluting furanone were Chiralpak AD-H column, column temperature of 30 ℃, column pressure of 10 MPa, 1.0% （V/V） methanol in mobile phase and flow rate of 1.5 mL/min, whereby Rs was 1.54. The optimum conditions to resolute homofuraneol were Chiralpak AD-H column, column temperature of 33 ℃, column pressure of 13 MPa, 1.5% （V/V） ethanol in mobile phase and flow rate of 1.5 mL/min, whereby Rs was 1.51. Second, experiments on a preparative scale were carried out under the above optimum conditions, and the enantiomers of furaneol and homofuraneol were successfully obtained with a purity of no less than 90% as well as a recovery yield of no less than 70%. The present work will be helpful for evaluating the potential applications of chiral furaneol or chiral homofuraneol to enhance food flavor, where the enantiomers of furaneol and homofuraneol are prerequisite.

关 键 词：填充柱超临界流体色谱 呋喃酮 酱油酮 手性拆分 对映体 

分 类 号：TQ65[化学工程—精细化工]