摘要
目的 建立同时测定蒙药清肝玛努-4 醇提物中马钱苷酸、龙胆苦苷、芍药苷、牡荆素、甘草苷、甘草酸铵等成分的HPLC含量测定方法及指纹图谱研究.方法 采用Agilent Eclipse XDB-C18 色谱柱(250 mm×4.6 mm,5 μm),流动相为 0.1%磷酸水溶液-乙腈,梯度洗脱,流速为 1.0 mL/min,检测波长为 230 nm(芍药苷、牡荆素、甘草苷)、237 nm(马钱苷酸)、250 nm(甘草酸铵)、270 nm(龙胆苦苷),柱温为30℃,进样量为10 μL.结果 蒙药清肝玛努-4醇提物中马钱苷酸、龙胆苦苷、芍药苷、牡荆素、甘草苷和甘草酸铵的质量浓度分别在0.020 3～0.121 0、0.053 3～0.317 7、0.021 3～0.127 0、0.011 5～0.069 0、0.014 1～0.083 8 和 0.035 1～0.209 1 mg/mL范围内与色谱峰面积呈良好的线性关系(r≥0.999 8),平均回收率分别为 94.75%、99.49%、92.32%、95.82%、101.29%和98.04%,RSD分别为1.11%、0.76%、0.99%、2.75%、1.09%和 2.43%(n=6).建立了蒙药清肝玛努-4 醇提物的HPLC指纹图谱,以S1 号样品色谱图为参照图谱,通过多点校正和全谱峰匹配,生成对照指纹图谱,共确定10个共有峰,经与对照品比对指认了其中8个成分.结论 所建立的测定方法及指纹图谱准确、可靠、重复性好、专属性强,为蒙药清肝玛努-4 的质量控制及后续开发提供了依据.
Abstract
Objective To establish a HPLC method and fingerprints study for the simultaneous determination of loganic acid,gentiopicroside,paeoniflorin,vitexin,liquiritin,and ammonium glycyrrhizinatein,and other components in the alcohol extract of Mongolian medicine Qinggan Manu-4.Methods The Agilent Eclipse XDB-C18 column(250 mm×4.6 mm,5 μm)was used,with the detection wavelength of 230 nm for paeoniflorin,vitexin and liquiritin,237 nm for loganic acid,250 nm for glycyrrhizic acid,and 270 nm for gentiopicroside.The mobile phase was 0.1%phosphoric acid aqueous solution-acetonitrile with gradient elution.The flow rate was 1.0 mL/min,the column temperature was 30℃,and the injection volume was 10 μL.Results The mass concentrations of loganic acid,gentiopicroside,paeoniflorin,vitexin,liquiritin and ammonium gentiopicroside in the alcohol extract of Mongolian medicine Qinggan Manu-4 showed good linear relationships with the chromatographic peak area in the range of 0.020 3-0.121 0,0.053 3-0.317 7,0.021 3-0.127 0,0.011 5-0.069 0,0.014 1-0.083 8 and 0.035 1-0.209 1 mg/mL,respectively(r≥0.999 8).The average recovery rates of the six components were 94.75%,99.49%,92.32%,95.82%,101.29%and 98.04%,with the RSDs of 1.11%,0.76%,0.99%,2.75%,1.09%and 2.43%,respectively(n=6).The HPLC fingerprint of the alcoholic extract of Mongolian medicine Qinggan Manu-4 was established,using the chromatogram of sample S1 as the reference chromatogram,the control fingerprints were generated through multi-point correction and full-spectrum peak matching.A total of ten common peaks were identified,and after comparison with the reference substance,eight components were identified.Conclusion The established method and fingerprints are accurate,reliable,reproducible and specific,which provide a basis for the quality control and subsequent development of Mongolian medicine Qinggan Manu-4.
基金项目
内蒙古自治区教育厅高等学校青年科技英才计划(NJYT23135)
内蒙古医科大学中药学(蒙药学)"一流学科"研究生科研能力提升项目(MYX2023-R17)
内蒙古医科大学面上项目(YKD2021MS040)
内蒙古医科大学蒙药成分体内分析科技创新团队项目(YKD2022TD037)
维普
万方数据