西兰花种子中分离纯化萝卜硫素及残留溶剂的方法学验证  

Isolation and purification methodology of sulforaphane from crude extract of broccoli seeds

作　　者：李欢 陈雄 康慧枝 谭凤明 韩静[2] 韩阳 LI Huan;CHEN Xiong;KANG Huizhi;TAN Fengming;HAN Jing;HAN Yang(School of Pharmaceutical Engineering,Shenyang Pharmaceutical University,Benxi 117004,China;School of Functional Food and Wine,Shenyang Pharmaceutical University,Benxi 117004,China;School of Traditional Chinese Materia Medica,Shenyang Pharmaceutical University,Benxi 117004,China)

机构地区：[1]沈阳药科大学制药工程学院,辽宁本溪117004 [2]沈阳药科大学功能食品和葡萄酒学院,辽宁本溪117004 [3]沈阳药科大学中药学院,辽宁本溪117004

出　　处：《沈阳药科大学学报》2023年第8期1078-1084,共7页Journal of Shenyang Pharmaceutical University

基　　金：2019年度辽宁省科学技术计划项目(2019JH2/10300039);辽宁省博士启动基金(2022-BS-154)。

摘　　要：目的介绍了一种从西兰花种子中分离纯化天然萝卜硫素高效、低成本方法。方法该方法包括种子自溶后的溶剂萃取、柱色谱分离和半制备高效液相色谱纯化。经MS、^(1)H-NMR、^(13)C-NMR谱对纯化后的化合物进行了表征。结果与传统的液-液萃取法相比,柱色谱分离法从西兰花种子中提取萝卜硫素的收率更高为(69.02±1.1)%。以SinoChrom ODS-BP柱为半制备高效液相色谱柱,以甲醇-水(体积比1∶4)为流动相,最大装载量小于60 mg,流量应控制在9 mL·min^(-1),可以获得纯度为95%的萝卜硫素。经HPLC、MS、^(1)H-NMR、^(13)C-NMR检测,结果表明,所得样品为目标化合物,且无有机溶剂残留。结论建立了一种分离纯化西兰花种子中萝卜硫素的方法。本方法经济、高效,有实用价值。Objective A new and low-cost method for the separation and purification of natural sulforaphane from broccoli seeds was introduced.Methods The method includes solvent extraction,atmospheric column chromatography and semi-preparative HPLC purification.The purified compounds were characterized by MS,^(1)H-NMR and^(13)C-NMR.Results The yield of sulforaphane extracted from broccoli seeds by column chromatography was(69.02±1.1)%,which was higher than that of the traditional liquid-liquid extraction method.A semi-preparative high performance liquid chromatographic column was prepared using SinoChrom ODS-BP column.The mobile phase was methanol-water(V/V=1∶4)with the flow rate of 9 mL min^(-1),and the maximum loading was less than 60 mg.High-purity sulforaphane(95%)could be obtained.The results of HPLC,MS,^1H-NMR and^(13)C-NMR showed that the samples were the target compound and no organic solvent remained.Conclusion An economical,efficient and practical method was established for the separation and purification of sulforaphane from broccoli seeds.

关 键 词：萝卜硫素 西兰花种子 分离纯化 残留溶剂 半制备高效液相色谱纯化 

分 类 号：R93[医药卫生—生药学]