[Objective] This study was conducted to develop a method for rapidly separating macranthoidin B and dipsacoside B from Flos Lonicerae. [Method] HP-20 and HP-SS macroporous resin were applied to separate and purify mac...[Objective] This study was conducted to develop a method for rapidly separating macranthoidin B and dipsacoside B from Flos Lonicerae. [Method] HP-20 and HP-SS macroporous resin were applied to separate and purify macranthoidin B and dipsacoside B from Flos Lonicerae. The extract of Flos Lonicerae was first loaded onto an HP-20 column to enrich saponins, which were then separated by an HP-SS macroporous resin column to get pure macranthoidin B and dipsacoside B.[Result] The optimal HP-20 purification conditions included： a concentration of sample liquid at 4.8 mg/ml, a sample volume of 2 BV, an adsorption flow rate at 1.5BV/h, an ethanol concentration for desorption at 60%, a desorption volume of 3 BV,and a desorption flow rate at 1.5 BV/h. Total saponins were then separated by an HP-SS macroporous resin column which was eluted sequentially by water, 20%ethanol, 30% ethanol, 40% ethanol and 50% ethanol. Two purified compounds were obtained in fractions eluted by 40% ethanol and 50% ethanol, respectively. The two compounds were identified as macranthoidin B and dipsacoside B by13 C and1H nuclear magnetic resonance spectroscopy. [Conclusion] The combination of HP-20 and HP-SS macroporous resin could efficiently separate macranthoidin B and dipsacoside B from Flos Lonicerae.展开更多
[Objective] A method for the determination of chlorogenic acid, macranthoidin B and dipsacoside B in Flos Lonicera by high performance liquid chromatography（HPLC） with evaporative light scattering detection（ELSD） ...[Objective] A method for the determination of chlorogenic acid, macranthoidin B and dipsacoside B in Flos Lonicera by high performance liquid chromatography（HPLC） with evaporative light scattering detection（ELSD） was established.[Method] The separation was carried out using a ZORBAX SB-C18 chromatographic column（4.6 mm ×250 mm, 5 μm）, with a simple mobile phase of acetonitrile and0.1% formic acid. Evaporative light scattering detector was employed. [Result] The result showed that chlorogenic aicd, macranthoidin B and dipsacoside B showed good linearities in the ranges of 3.00-6.40, 4.24-9.33 and 0.40-2.00 μg with correlation coefficient of 0.999, 0.993 and 0.999, respectively. [Conclusion] The method has the advantages of simple operation, good accuracy, repeatability and separation effect and high specificity and is suitable for overall quality control of Flos Lonicera.展开更多
基金Supported by Guangxi Scientific Research and Technological Development Planning Project(20130403-2)Technology Research and Development Program of Guangxi Province(GKH15104001-15)+1 种基金Special Fund for Bagui Scholars of the Guangxi Zhuang Autonomous RegionDirector Fund Project of Guangxi Key Laboratory of Functional Phytochemicals Research and Utilization(ZRJJ2016-4)~~
文摘[Objective] This study was conducted to develop a method for rapidly separating macranthoidin B and dipsacoside B from Flos Lonicerae. [Method] HP-20 and HP-SS macroporous resin were applied to separate and purify macranthoidin B and dipsacoside B from Flos Lonicerae. The extract of Flos Lonicerae was first loaded onto an HP-20 column to enrich saponins, which were then separated by an HP-SS macroporous resin column to get pure macranthoidin B and dipsacoside B.[Result] The optimal HP-20 purification conditions included： a concentration of sample liquid at 4.8 mg/ml, a sample volume of 2 BV, an adsorption flow rate at 1.5BV/h, an ethanol concentration for desorption at 60%, a desorption volume of 3 BV,and a desorption flow rate at 1.5 BV/h. Total saponins were then separated by an HP-SS macroporous resin column which was eluted sequentially by water, 20%ethanol, 30% ethanol, 40% ethanol and 50% ethanol. Two purified compounds were obtained in fractions eluted by 40% ethanol and 50% ethanol, respectively. The two compounds were identified as macranthoidin B and dipsacoside B by13 C and1H nuclear magnetic resonance spectroscopy. [Conclusion] The combination of HP-20 and HP-SS macroporous resin could efficiently separate macranthoidin B and dipsacoside B from Flos Lonicerae.
基金Supported by Technology Research and Development Program of Guilin City(20130403-2)~~
文摘[Objective] A method for the determination of chlorogenic acid, macranthoidin B and dipsacoside B in Flos Lonicera by high performance liquid chromatography（HPLC） with evaporative light scattering detection（ELSD） was established.[Method] The separation was carried out using a ZORBAX SB-C18 chromatographic column（4.6 mm ×250 mm, 5 μm）, with a simple mobile phase of acetonitrile and0.1% formic acid. Evaporative light scattering detector was employed. [Result] The result showed that chlorogenic aicd, macranthoidin B and dipsacoside B showed good linearities in the ranges of 3.00-6.40, 4.24-9.33 and 0.40-2.00 μg with correlation coefficient of 0.999, 0.993 and 0.999, respectively. [Conclusion] The method has the advantages of simple operation, good accuracy, repeatability and separation effect and high specificity and is suitable for overall quality control of Flos Lonicera.
