Study On Quality Control Methods Of Xihuang Pills

Xihuang pill,is starched pill blending with bezoar,musk,frankincense、myrrh and millet,showing dark brown,aromatic odor and slightly bitter taste.Which have been mainly used in the forfurunculosis,scrofula and cancer caused by heat accumulation.ObjectiveThis topic aimed at improving the quality control of Xihuang pills based on the pharmacopoeia method.Qualitative and quantitative researches were carried out on characteristic components.Descripte and evaluate the overall quality by fingerprint analysis and clustering analysis method.The constituents were studied by mass spectrometry.The research provides the experimental basis for the quality control of Xihuang pill research.Methods1.1 Qualitative and quantitative study on characteristic componentsThrough the durability investigation of chromogenic agent and durability,hyodeoxycholic acid was identificated qualitatively by TLC methods,as well as the source of frankincense and myrrh.Bilirubin was quantified by RP-HPLC-UV method.Muskone was quantified by GC-FID.11-carbonyl-β-boswellic acid,acetyl-11-carbonyl-β-boswellic acid,a-boswellic acid,β-boswellic acid,3-acetyl-α-boswellic acid,and 3-acetyl-β-boswellic acid were quantified by RP-HPLC-ELSD method.Amino acid and polysaccharide was quantified by UV method.1.2 Study on fingerprintAfter the optimization of chromatographic conditions and extraction conditions,the fingerprints of 10 batches of Xihuang pills were determinated by RP-HPLC-ELSD and GC-FID.The fingerprint was evaluated by the system clustering analysis,principal component analysis and similarity.1.3 Mass spectrometry identificationAfter the optimization of mass spectrometry conditions,identificate the chemical composition by RP-HPLC/ESI-MS method through established Chemical component library and import to Peak view software.The volatile components was identified through the standard library NIST MS search 2.0 and PBM Quick search matching by combining with the pyrolysis rule in GC-MS.Results1.1 Qualitative and quantitative study on characteristic componentsIn the quantitative study,there wasn’t the plot parallelise to hyodeoxycholic acid between samples and standard in TLC.In the TLC of medicinal materials of frankincense and myrrh,frankincense,natural myrrh control medicine solution had shown corresponding spots at the same Rf value with sample.In quantitative study,all ingredients had shown good linear relationship and survey of methodology.Component content had shown good stability.1.2 Study on fingerprintThe fingerprint of different extraction parts in 10 batches of Xihuang pill meets the methodology requirements,in which determines the 25 and 22 common peak respectively.Through pattern recognition analysis,the inherent differences between different batches of Xihuangwan were reflected.The concept of "dimension" was introduced to analyze the peak information,to identify the main chemical constituents of the difference and its contribution to the sample differences.1.3 Qualitative researchRP-HPLC/ESI-MS and GC-MS intense matches the 188 compounds,including 55 frankincense compositions,114 myrrh compositions,15 ingredients bezoars and 4 musk compositions.32 compounds were detected by GC-MS.There were 6 kinds of alcohols,4 kinds of hydrocarbons,4 kinds of ketone compounds,2 lactone compounds and 1 nitrogen compound.ConclusionThis present study could validate and improve the original quality control method of Xihuang pill gradually.Fingerprint,cluster analysis,principal component analysis and similarity analysis show good applicability on complex component quality control and evaluation in traditional Chinese medicine could better reflect on the overall intrinsic quality of Xihuang pill.LC-MS/MS and GC-MS qualitative research matches and identificate 210 chemical compositions,expanded the qualitative study of Xihuang pill,clarify the basic fragmentation pattern,and provide an experimental basis for the related research of Xihuang pill.