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

Establishment of HPLC fingerprint of Liangfu dropping pills and simultaneous determination of six components

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,5μm)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.