百合磷茎中Regaloside A、Acetylregaloside C与Regaloside B高速逆流色谱分离及生物活性研究  

Separation of Regaloside A,Acetylregaloside C and Regaloside B in Bulbs of Lilium Species by High Speed Counter-current Chromatography and Research on Their Biological Activities

作　　者：陆英[1,2] 刘仲华[1,2] 肖文军[1,2] 傅冬和[1,2] 谢红旗[1,3] 曾建国 LU Ying;LIU Zhong-hua;XIAO Wen-jun;FU Dong-he;XIE Hong-qi;ZENG Jian-guo(College of Horticulture and Landscape,Hunan Agricultural University,Changsha 410128,China;National Research Center of Engineering Technology for Utilization of Functional Ingredients from Botanicals,Hunan Agricultural University, Changsha 410128,China;National Herbal Medicine Production(Hunan)Technology Center, Changsha 410128,China)

机构地区：[1]湖南农业大学园艺园林学院,湖南长沙410128 [2]湖南农业大学国家植物功能成分利用工程技术研究中心,湖南长沙410128 [3]国家中药材生产(湖南)技术中心,湖南长沙410128

出　　处：《分析测试学报》2018年第9期1027-1033,共7页Journal of Instrumental Analysis

基　　金：现代农业产业技术体系建设专项资金资助(CARS-21);湖南省科技创新计划项目(S2017SFXYZ0116)

摘　　要：建立了高速逆流色谱分离制备药食同源植物百合磷茎中3个酚酸甘油酯苷的方法,同时测定了化合物对1,1-二苯基-2-三硝基苯肼(DPPH)自由基的清除作用、脂质的过氧化抑制作用及对α-淀粉酶活性的促进作用。以乙酸乙酯-正丁醇-水(0. 5%乙酸,3∶1. 5∶5,体积比)为溶剂系统,上相为固定相,下相为流动相,从250 mg百合磷茎提取物中分离得到4. 2 mg纯度为96. 2%的化合物1,2. 3 mg纯度为95. 1%的化合物2,5. 8 mg纯度为98. 8%的化合物3。经质谱及核磁共振鉴定化合物1~3分别为王百合苷A(Regaloside A)、乙酰化王百合苷C(Acetylregaloside C)、王百合苷B(Regaloside B);活性研究表明,Acetylregaloside C对DPPH自由基清除作用及脂质过氧化抑制作用均最强,Regaloside A与Regaloside B对DPPH自由基清除作用很弱,对脂质过氧化有一定的抑制作用且相近,化合物抗氧化作用强弱为:化合物2> 1≈3。化合物在不同浓度下对α-淀粉酶活性的促进作用具有一定差异,但化合物间无显著差异。A method of high speed counter-current chromatography was developed for the separation and preparation of three active compounds,phenolic glycerol glycosides from the bulbs of Lilium species used as Chinese tradition medicine.The ethylacetate-n-butanol-water(0.5%acetic acid,3∶1.5∶5,by volume)was used as a two-phase solvent system,in which the upper phase was stationary phase and the lower phase was mobile phase for the isolation of the compounds from the extract of Lilium brownii F.E.Brown var.viridulum Baker by high speed counter-current chromatography(HSCCC).Additionally,the antioxidant activities on free radical scavenging and lipid peroxidation,and the effects onα-amylase activity were evaluated.Results showed that 4.2 mg of compound 1(96.2%,purity),2.3 mg of compound 2(95.1%)and 5.8 mg of compound 3(98.8%)were obtained from the 250 mg extract by one-step using high-performance liquid chromatography(HPLC).The chemical structures of the compound 1-3 were identified as regaloside A,acetylregaloside C and regaloside B,respectively by mass spectrometry(MS)and nuclear magnetic resonance imaging(NMR).Biological activity test showed that acetylregaloside C exhibited a strong capacity scavenging DPPH and inhibiting lipid peroxidation,while regaloside A and regaloside B had weak capacity scavenging DPPH and definite inhibitory effects on lipid peroxidation.The antioxidant effects of the compounds were as follows:acetylregaloside C>regaloside A≈regaloside B.The promoting effects of the compounds on the activity ofα-amylase were different in different concentrations,but no significant difference existed among the compounds.

关 键 词：分离 中药百合 酚酸甘油酯苷 高速逆流色谱(HSCCC) 生物活性 

分 类 号：O657.7[理学—分析化学] TQ450.2[理学—化学]