To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liq...To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.展开更多
目的:采用超高效液相色谱-飞行时间质谱(UPLC-Q-TOF/MS)对参芪归芍汤中的化学成分进行分析和鉴定。方法:采用ACQUITYTM UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸-乙腈为流动相进行快速梯度洗脱,流速1.0 m L·min^...目的:采用超高效液相色谱-飞行时间质谱(UPLC-Q-TOF/MS)对参芪归芍汤中的化学成分进行分析和鉴定。方法:采用ACQUITYTM UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸-乙腈为流动相进行快速梯度洗脱,流速1.0 m L·min^(-1),柱温35℃,进样量10μL。电喷雾离子源负离子模式,毛细管电压分别为1.4 k V和1.3 k V,锥孔电压分别为40 V和23 V,离子源温度120℃,脱溶剂气温度350℃,锥孔气流量50 L·h^(-1),脱溶剂气流量600 L·h^(-1),碰撞能量10~40 e V,离子能量1 e V。结果:从参芪归芍汤中鉴定了42个化合物,结果显示,参芪归芍汤中的主要化学成分包括皂苷、黄酮和酚酸等类化合物。结论:该研究比较全面地阐明了参芪归芍汤的化学组成,对参芪归芍汤的质量控制和药效物质基础的研究具有十分重要意义。展开更多
基金Supported by Plan Issue of Shanghai Science &Technology Committee(No.13401901100)
文摘To establish a method for determining five saponins(notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ammonium glycyrrhizinate) in Glycyrrhizae, Notoginseng and Ginseng, the high performance liquid chromatography with diode array detector(HPLC-DAD) method was applied to an Inertsil ODS-SP column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of acetonitrile-0.05% phosphoric acid in a gradient elution manner. The flow rate was 1.0 mL/min. The column temperature was 30 ℃ and the detection wavelengths were 203 nm and 237 nm, respectively. The linear ranges were 0.700,0—7.000,0 μg for R1(r=1.000,0), 0.751,1— 7.511,4 μg for Rg1(r=1.000,0), 0.677,2—6.771,6 μg for Re(r=1.000,0), 0.733,9—7.339,1 μg for Rb1(r= 1.000,0), and 0.540,0—5.399,8 μg for ammonium glycyrrhizinate(r=0.999,9), respectively. In addition, their average recoveries were 100.28%, 105.83%, 104.09%, 99.36% and 98.54%, respectively. The relative standard deviations(RSDs) of precision, reproducibility and recovery were all less than 1.5%. The results indicate that the method is simple, accurate and reproducible so that it can be used for the simultaneous determination of the five saponins in Chinese patent medicines containing the three kinds of herbs.
文摘目的:采用超高效液相色谱-飞行时间质谱(UPLC-Q-TOF/MS)对参芪归芍汤中的化学成分进行分析和鉴定。方法:采用ACQUITYTM UPLC BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以0.1%甲酸-乙腈为流动相进行快速梯度洗脱,流速1.0 m L·min^(-1),柱温35℃,进样量10μL。电喷雾离子源负离子模式,毛细管电压分别为1.4 k V和1.3 k V,锥孔电压分别为40 V和23 V,离子源温度120℃,脱溶剂气温度350℃,锥孔气流量50 L·h^(-1),脱溶剂气流量600 L·h^(-1),碰撞能量10~40 e V,离子能量1 e V。结果:从参芪归芍汤中鉴定了42个化合物,结果显示,参芪归芍汤中的主要化学成分包括皂苷、黄酮和酚酸等类化合物。结论:该研究比较全面地阐明了参芪归芍汤的化学组成,对参芪归芍汤的质量控制和药效物质基础的研究具有十分重要意义。