| The research to the Pharmacopoeia received load variety Yinqiaojiedu particles as the research object, according to the prescription dose of various ingredients, composition characteristics, by using modern analysis technology, to establish a method for determination of Yinqiao Jiedu Granule by HPLC characteristic spectrum and multi component content, to further improve the current standards for the preparation, by the establishment of the content determination method for evaluation of different manufacturers to produce the Yinqiao Jiedu Granule Preparation quality, the same manufacturers from batch to batch process stability and consistent quality of control. Also consider to prescription are the main ingredients of honeysuckle, honeysuckle since and Lonicera confusa varieties after the breakdown, Pharmacopoeia only Caprifoliaceae honeysuckle dried buds or primal flower honeysuckle, market honeysuckle price also than Lonicera confusa is much higher, so this topic also increased the examination of Yinqiao Jiedu Granule Zhongshan Yinhua, to investigate whether there are manufacturers in the presence of illegal feeding and so on.Objective (1) The establishment of Yinqiaojiedu particles HPLC characteristic spectrum, provide a reference for the quality evaluation of Yinqiao Jiedu granules (2) to establish multi component content determination method of Yinqiao Jiedu Granule by HPLC fingerprint, and further improve the Yinqiao Jiedu Granule quality control standards (3) to establish the TLC method for the determination of Yinqiao Jiedu Granule in examination of Flos Lonicerae, improve quality standardsMethods (1) by ultrasonic solvent extraction method to extract the principal components in Yinqiao Jiedu granules, combined with chromatography, spectrometry, mass spectrometry and other modern analysis methods, through for simultaneous determination of single herb, to determine the attribution of the ingredients; through the optimization of chromatographic conditions, the establishment of Yinqiao Jiedu Granule by HPLC characteristic spectrum. Through the comparison of quality control and mass spectrometry method of characteristic peaks were identified. Zorbax XDB C18 column (150×4.6mm,5μm) column, acetonitrile (a) 0.1% formic acid (b) for flow by gradient elution (0～10 min,5%A～15%A; 20～45min, 15%A～22%A; 45～80min,22%A-52%A), column temperature:30℃, the flow rate: 1.0ml/min. The detection wavelength:245nm. Using quality control method and mass spectrometry, the characteristic peaks were identified. (2) to establish a determination method for and chlorogenic acid in Yinqiao Jiedu granules forsythia ester glycoside A, arctiin, ammonium glycyrrhizinate. (3) Check the Macranthoidin B of Yinqiaojiedu particles’s characteristic components of Lonicera confusa by TLC, With HPLC was further confirmed.Results (1) by high performance liquid chromatography combined with spectral and fluid combined with technical analysis, forsythiaside Aas the reference peak. The calculation of the relative retention time of the main chromatographic peaks, the establishment of Yinqiao Jiedu Granule by HPLC fingerprint, identified total of 19 characteristic peaks, and identify the neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, forsythoside A, forsythia ester glycoside B, forsythiaside C, forsythin, arctiin, liquiritin and glycyrrhizic acid ammonium total of 10 characteristic peaks. Produced by different manufacturers of Yinqiao Jiedu Granule by HPLC fingerprint analysis. The results show that samples of different manufacturers, in addition to the chlorogenic acid content is relatively high in general and other chemical components exist bigger difference. (2) the established Yinqiao Jiedu Granule HPLC characteristic spectrum method, choose a kind of active ingredients of honeysuckle, forsythia, arctium fruit, licorice in content and control, chlorogenic acid, forsythoside a, arctiin, ammonium glycyrrhizinate respectively in sample volume 6.204～279.2,2.016～90.72, 13.40～60.29 and 1.660-74.70ng range showed a good linear relationship; chlorogenic acid, the average recovery of forsythoside A, arctiin, ammonium glycyrrhizinate rate 99.79% and 99.58% and 98.56% and 100.2%, respectively. (3) by thin layer chromatography of Yinqiao Jiedu granules were identified and the established TLC spots were clear. Determination of the 56 batches of samples showed that there are 13 manufacturers to detect Macranthoidin B.Conclusion (1) the operation of the establishment of the Yinqiao Jiedu granules HPLC fingerprint method, is simple and has good repeatability and stability, which can provide a more comprehensive basis for the formulation of standards; (2) to establish a method for determination of multi index content Yinqiaojiedu particles content, can simultaneously control 4 components in the feature map the method is simple and accurate, and can provide a more effective method for controlling the quality of the preparation, but also for the comprehensive evaluation of the preparation to provide a reference value (3) check Yinqiaojiedu particles in the presence of the mountain honeysuckle by TLC, The method is simple and easy to operate, To provide a scientific basis for better control of Yinqiao Jiedu granules preparation quality, standardize production behavior. |
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