1. .中国科学技术大学化学系
2. 安徽中烟工业有限责任公司技术中心安徽省烟草化学重点实验室
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田东, 朱栋梁, 徐志强, 等. 二维液相色谱分离及鉴定滁菊中的多酚类化合物[J]. 分析测试学报, 2015,34(8):917-922.
Separation and Characterization of Phenolic Compounds in Chuju by Two-dimensional Hydrophilic Interaction/Reversed Phase Liquid Chromatography Coupled to Diode Array Detection[J]. 2015,34(8):917-922.
将Lichrospher diol-5亲水柱和Cortecs C18+反相柱组合,构建了亲水/反相二维液相色谱系统(HILIC/RPLC),理论峰容量为1 117。采用表面积覆盖法定量计算该系统分离多酚类化合物的正交性指数SCG为0.56,表明二维柱系统有着良好的峰分辨率和正交性。利用该系统对滁菊样品甲醇提取液中的多酚进行分离和鉴定,在二维空间中分离得到23个物质的色谱峰,通过对比标准样品和滁菊样品的保留时间和紫外吸收光谱,鉴定出13种多酚类物质,包括芹菜素、香叶木素、金合欢素、金合欢素-7-O-葡糖苷、绿原酸、异鼠李素-3-O-葡糖苷、香叶木素-7-O-葡糖苷、金合欢素-7-O-芸香苷、圣草酚-7-O-葡糖苷、槲皮素苷、异绿原酸A、异绿原酸B、芹菜苷。首次发现滁菊中含有异鼠李素-3-O-葡糖苷、金合欢素-7-O-芸香苷、圣草酚-7-O-葡糖苷、芹菜苷等多酚类化合物。其中,异鼠李素-3-O-葡糖苷首次发现存在于菊属植物中。
An innovative analytical approach based on the use of comprehensive two-dimensional hydrophilic interaction/reversed phase liquid chromatography(HILIC/RPLC) was applied to obtain the profiling of phenolic compounds in Chuju.The method involved the use of a microbore hydrophilic interaction column containing a diol stationary phase(Lichrospher diol-5) in the first dimension combined with a reversed phase column(Cortecs C18+) in the second dimension,and applied two sample loops as interface between the first and the second dimension.Two different gradient elutions were employed in the two dimensions,respectively.Detecton wavelength was set at 330 nm,and sampling rate was 15 Hz in the diode array detection.The theoretical peak capacity was up to 1 117 while the surface coverage proposed by Gilar(SCG) was 0.56,indicating both good resolution and good orthogonality of this 2D-LC system.23 peaks in the 2D-LC separation space were found,and 13(apigenin,luteolin,acacetin,acacetin-7-O-glucoside,chlorogenic acid,isorhamnetin-3-O-glucoside,luteolin-7-O-glucoside,acacetin-7-O-rutinoside,acacetin-7-O-rutinoside,quercitrin,isochlorogenic acid A,isochlorogenic acid B,apioside)of them were allowed tentative identification according to comparing with retention times and maximum absorption wavelengths between the sample and standards.In which 4 phenolic compounds(isorhamnetin-3-O-glucoside,acacetin-7-O-rutinoside,eriodictyol-7-O-glucoside,apioside)were firstly found in Chuju and isorhamnetin-3-O-glucoside was firstly found in Dendranthema morifolium.
滁菊多酚类化合物二维液相色谱亲水作用色谱/反相色谱
Chujuphenolic compoundscomprehensive two-dimensional liquid chromatographyhydrophilic interaction/reversed phase liquid chromatography(HILIC /RPLC)
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