良附滴丸HPLC指纹图谱的建立及同时测定6种指标成分的含量
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摘要
目的:建立良附滴丸高效液相色谱法(high performance liquid chromatography,HPLC)指纹图谱以及同时测定6种成分含量的分析方法,评价良附滴丸质量均一性并进行质量分析。方法:采用HPLC色谱柱为Luna PFP(2) 100A(250 mm×4. 60 mm,5μm);流速1. 0 m L·min~(-1);柱温40℃;以流动相乙腈-0. 1%磷酸水溶液为流动相;在190 nm波长下进行梯度洗脱,建立良附滴丸HPLC指纹图谱;乙腈-0. 1%磷酸水(40∶60)为流动相;波长为254 nm对6个指标成分进行含量测定。结果:建立了良附滴丸HPLC指纹图谱及含量测定分析方法,对15批良附滴丸进行了相似度评价,相似度值均> 0. 9;确定了21个共有峰,其相对保留时间和相对峰面积RSD值均<0. 3%,并指认了其中6种成分,分别为高良姜素、鼠李柠檬素、高良姜素-3-O-甲醚、香附烯酮、诺卡酮、α-香附酮; 6种指标成分在一定浓度范围内线性良好,平均加样回收率良好。结论:建立的高效液相色谱指纹图谱及多指标成分同时测定。分析方法简单、专属性强,灵敏度和重复性高,可为良附滴丸的质量控制提供参考。
Objective: To establish the fingerprint of Liangfu dropping pills by high performance liquid chromatography( HPLC) and the method for simultaneous determination of six components to evaluate the quality uniformity of Liangfu dropping pills and analyze the quality. Methods: HPLC was used with Luna PFP( 2) 100 A( 250 mm × 4. 60 mm,5 μm) as the chromatographic column eluted at a flow rate of 1. 0 m L·min~(-1),and the column temperature was set at 40 ℃. The fingerprint of Liangfu dropping pills was established by gradient elution of mobile phase consisting of acetonitrile-0. 1% phosphoric acid aqueous solution detected at 190 nm,and the contents of six components were determined at 254 nm using acetonitrile-0. 1% phosphoric acid water( 40 ∶ 60) as mobile phase. Results: The fingerprint and content determination methods of Liangfu dropping pills by HPLC were established. The similarity of 15 batches of Liangfu dropping pills was evaluated,and the similarity values weregreater than 0. 9. Twenty-one common peaks were identified,and the RSD values of relative retention time and relative peak area were less than 0. 3%. Besides,six components were identified,namely,galangarin,rhamnolidin,galangin-3-O-methyl ether,geranyl ketone,nocardione and alpha-geranyl ketone. The linearity of the six index components was good in a certain concentration range,and the average recovery rate was satisfying. Conclusion:The established high performance liquid chromatography fingerprint and simultaneous determination method of multi-index components are simple,specific,sensitive and repeatable. It could provide reference for the quality control of Liangfu dropping pills.
Objective: To establish the fingerprint of Liangfu dropping pills by high performance liquid chromatography( HPLC) and the method for simultaneous determination of six components to evaluate the quality uniformity of Liangfu dropping pills and analyze the quality. Methods: HPLC was used with Luna PFP( 2) 100 A( 250 mm × 4. 60 mm,5 μm) as the chromatographic column eluted at a flow rate of 1. 0 m L·min~(-1),and the column temperature was set at 40 ℃. The fingerprint of Liangfu dropping pills was established by gradient elution of mobile phase consisting of acetonitrile-0. 1% phosphoric acid aqueous solution detected at 190 nm,and the contents of six components were determined at 254 nm using acetonitrile-0. 1% phosphoric acid water( 40 ∶ 60) as mobile phase. Results: The fingerprint and content determination methods of Liangfu dropping pills by HPLC were established. The similarity of 15 batches of Liangfu dropping pills was evaluated,and the similarity values weregreater than 0. 9. Twenty-one common peaks were identified,and the RSD values of relative retention time and relative peak area were less than 0. 3%. Besides,six components were identified,namely,galangarin,rhamnolidin,galangin-3-O-methyl ether,geranyl ketone,nocardione and alpha-geranyl ketone. The linearity of the six index components was good in a certain concentration range,and the average recovery rate was satisfying. Conclusion:The established high performance liquid chromatography fingerprint and simultaneous determination method of multi-index components are simple,specific,sensitive and repeatable. It could provide reference for the quality control of Liangfu dropping pills.
引文
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[11]孙楠. HPLC法测定香附丸中α-香附酮含量[J].亚太传统医药,2017,13(1):24-25.
[12]王立立,张云,孙玲,等.香附丸中4种成分的多波长HPLC法测定[J].中国医药工业杂志,2017,48(12):1796-1799.
[13]班小军,杨雪梅,赵翠琴.高效液相梯度洗脱法同时测定复方救必应胶囊中紫丁香苷、长梗冬青苷、圆柚酮和α-香附酮含量[J].中国中医药科技,2016,23(4):431-433.
[2]李洪福,李永辉,王勇,等.高良姜化学成分及药理活性的研究[J].中国实验方剂学杂志,2014,20(7):236-244.
[3]吕玮,蒋伶活.高良姜的化学成分及药理作用[J].中国药业,2006,15(3):19-21.
[4]祝永仙,李尚秀,赵升逵,等.高良姜的化学成分研究[J].云南民族大学学报,2013,22(4):239-241.
[5]徐晓婷,邓志鹏,仲浩,等.香附化学成分及药理作用研究进展[J].齐鲁药事,2012,31(8):473-475.
[6]陈志坚,胡璇,刘国道.香附的化学成分及药理作用研究进展[J].安徽农业科学,2017,45(36):113-115.
[7]张萍,杨燕,鄢丹,等.多指标成分含量测定与指纹图谱分析在中药制备工艺与质量控制中的应用[J].中华中医药杂志,2010,25(1):120-123.
[8]梁小银,陈少旭,吴垠.中药制剂质量控制演技趋势[J].中国药房,2014,25(3):280-283.
[9]王哲,申书昌. UPLC-MS法测定高良姜中高良姜素的含量[J].齐齐哈尔医学院学报,2015,36(22):3364-3365.
[10]彭贵龙,周光明,秦红英. HPLC法同时测定高良姜中6个成分的含量[J].药物分析杂志,2014,34(6):966-970.
[11]孙楠. HPLC法测定香附丸中α-香附酮含量[J].亚太传统医药,2017,13(1):24-25.
[12]王立立,张云,孙玲,等.香附丸中4种成分的多波长HPLC法测定[J].中国医药工业杂志,2017,48(12):1796-1799.
[13]班小军,杨雪梅,赵翠琴.高效液相梯度洗脱法同时测定复方救必应胶囊中紫丁香苷、长梗冬青苷、圆柚酮和α-香附酮含量[J].中国中医药科技,2016,23(4):431-433.