1,2,3,4,6-penta-O-acetyl-β-D-glucose is prepared by the reaction of glucose and acetic anhydride.Based on the activity difference and steric hindrance of acetyl in 1,2,3,4,6-pen-ta-O-acetyl-β-D-glucose,4,4’-bis(2,3...1,2,3,4,6-penta-O-acetyl-β-D-glucose is prepared by the reaction of glucose and acetic anhydride.Based on the activity difference and steric hindrance of acetyl in 1,2,3,4,6-pen-ta-O-acetyl-β-D-glucose,4,4’-bis(2,3,4,6-tetra-O-acetyl-β-D-glucoside)-2,2-diphenol propane is prepared by the reaction with1,2,3,4,6-penta-O-acetyl-β-D-glucose and bisphenol-A which structure is symmetric in the presence of dichloromethane.All acetyls of the synthetic products are eliminated in alkali methanol,then a new kind of intermediate of glycophane,4,4’-Bisglucoside-2,2-diphenol propane is obtained.A series of analysis methods including IR analysis、nuclear magnetism resonance(1H NMR)、elementary analysis(EA)and melting point determination are applied to determine products purity and characterize products structure.展开更多
目的建立能同时测定冠心安口服液中蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷含量的HPLC分析方法。方法Capcell Pak UG C_(18)色谱柱分离;蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷检测...目的建立能同时测定冠心安口服液中蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷含量的HPLC分析方法。方法Capcell Pak UG C_(18)色谱柱分离;蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷检测波长分别设定为334、281、320 nm;柱温为室温;进样体积为10μL;以乙腈为流动相A,1 mL·L^(−1)磷酸溶液(三乙胺调节pH至6.0)为流动相B,梯度洗脱。结果蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的质量浓度分别在0.0245~2.4500、0.0457~4.5700、0.0474~4.7400μg·mL^(−1)范围内线性良好;平均回收率分别为100.8%、99.9%、101.4%;精密度和重复性RSD值(n=6)均在5.0%以内;供试品溶液在24 h内稳定。结论此方法具有前处理简单、分析时间短和检测结果准确等优点,适用于冠心安口服液制剂的质量控制。展开更多
文摘1,2,3,4,6-penta-O-acetyl-β-D-glucose is prepared by the reaction of glucose and acetic anhydride.Based on the activity difference and steric hindrance of acetyl in 1,2,3,4,6-pen-ta-O-acetyl-β-D-glucose,4,4’-bis(2,3,4,6-tetra-O-acetyl-β-D-glucoside)-2,2-diphenol propane is prepared by the reaction with1,2,3,4,6-penta-O-acetyl-β-D-glucose and bisphenol-A which structure is symmetric in the presence of dichloromethane.All acetyls of the synthetic products are eliminated in alkali methanol,then a new kind of intermediate of glycophane,4,4’-Bisglucoside-2,2-diphenol propane is obtained.A series of analysis methods including IR analysis、nuclear magnetism resonance(1H NMR)、elementary analysis(EA)and melting point determination are applied to determine products purity and characterize products structure.
文摘目的建立能同时测定冠心安口服液中蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷含量的HPLC分析方法。方法Capcell Pak UG C_(18)色谱柱分离;蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷检测波长分别设定为334、281、320 nm;柱温为室温;进样体积为10μL;以乙腈为流动相A,1 mL·L^(−1)磷酸溶液(三乙胺调节pH至6.0)为流动相B,梯度洗脱。结果蒙花苷、延胡索乙素和2,3,5,4’-四羟基二苯乙烯-2-O-β-D-葡萄糖苷的质量浓度分别在0.0245~2.4500、0.0457~4.5700、0.0474~4.7400μg·mL^(−1)范围内线性良好;平均回收率分别为100.8%、99.9%、101.4%;精密度和重复性RSD值(n=6)均在5.0%以内;供试品溶液在24 h内稳定。结论此方法具有前处理简单、分析时间短和检测结果准确等优点,适用于冠心安口服液制剂的质量控制。
