药桑叶中金丝桃苷及其异构体分离鉴定  

Isolation and Identification of Hyperic and Its Isomers in Leaves of Morus nigra L.

作　　者：张贵会 刘佳洁 赵金梅 ZHANG Guihui;LIU Jiajie;ZHAO Jinmei(Zhalute Banner Market Inspection and Testing Center,Tongliao 029100,China;Yihe School Zhalute Tongliao City,Tongliao 029100,China;Horqin Left Wing Middle Banner Menda Central School Tongliao City,Tongliao 029100,China)

机构地区：[1]扎鲁特旗市场检验检测中心,内蒙古通辽029100 [2]扎鲁特旗伊和学校,内蒙古通辽029100 [3]通辽市科尔沁左翼中旗门达中心校,内蒙古通辽029100

出　　处：《现代食品》2022年第23期171-174,共4页Modern Food

摘　　要：应用色谱分离法和高效制备液相色谱法研究药桑叶中金丝桃苷及其异构体分离制备方法。结果表明,药桑叶95%醇提物经乙酸乙酯萃取,过已活化的D-101型大孔吸附树脂经中压柱色谱可得到金丝桃苷及其异构体的混合物。将混合物用高效制备液相分离,制备液相色谱柱为Waters Xbridge(300 mm×21 mm,10μm),流动相为95%乙腈-5%水(含0.1%甲酸),上样量100 mg,流速15 mL·min^(-1),柱温40℃,检测波长285 nm,得到纯度为98.7%、97.8%以上两种纯物质,经核磁共振和质谱分析鉴定其结构为金丝桃苷、槲皮素-3-O-葡萄糖苷,二者互为同分异构体。The separation and preparation methods of hyperin and its isomers in leaves of Morus nigra L. were studied by chromatographic separation and high-performance preparative liquid chromatography. The results showed that 95% ethanol extract of leaves of Morus nigra L. was extracted by ethyl acetate, and the mixture of hyperin and its isomers was obtained by medium pressure column chromatography with activated D-101 macroporous adsorption resin. The mixture is separated by high-performance preparative liquid phase, and the preparative liquid chromatographic column is Waters Xbridge(300 mm × 21 mm,10 μm). The mobile phase was 95% acetonitrile-5% water(containing 0.1% formic acid),the loading amount was 100 mg, and the flow rate was 15 mL·min^(-1), column temperature 40 ℃, the detection wavelength was 285 nm, and two pure substances with purity of 98.7% and 97.8% were obtained. Their structures were identified as hypericin and quercetin-3-O-glucoside by NMR and MS analysis, and they were isomers of each other.

关 键 词：药桑叶 中压柱色谱 高效制备液相色谱 金丝桃苷 槲皮素-3-O-葡萄糖苷 

分 类 号：R284.1[医药卫生—中药学]