| Objective: Conduct systematic research on the properties,identification,inspection items,extracts,and other items of Flueggea suffruticosa,and develop a draft quality standard for Flueggea suffruticosa;To study and establish a method for the determination of securinine in Flueggea suffruticosa;To establish a fingerprint of Flueggea suffruticosa,and determine the contents of rutin,bergenin,and gallic acid in Flueggea suffruticosa,providing a reference for further research on Flueggea suffruticosa;To establish HPLC fingerprints of different medicinal parts of Flueggea suffruticosa,determine the contents of five chemical components in different medicinal parts,and analyze the differences,so as to provide a reference for the collection and processing resources utilization of Flueggea suffruticosa;Based on the theory of processing excipients of traditional Chinese medicine,Flueggea suffruticosa was processed with vinegar and wine.By comparing the differences in chemical components between samples before and after processing,the feasibility of processing Flueggea suffruticosa was preliminarily explored,and ideas and references were provided for further research.Methods: 1.According to the relevant contents and methods in the appendix of Part IV of the Chinese Pharmacopoeia,2020,complete the characterization of Flueggea suffruticosa,microscopic and TLC identification,and detection of moisture,total ash,acid insoluble ash,heavy metals,harmful elements,and extracts.2.A HPLC method for the determination of securinine was established;The content of rutin,bergenin,and gallic acid was determined using a one test multiple evaluation method.HPLC technique was used to establish the HPLC characteristic chromatogram of Flueggea suffruticosa.3.HPLC method was used to establish the fingerprints of different medicinal parts of Flueggea suffruticosa,and cluster analysis and principal component analysis were conducted using their common peak areas as indicators.To determine the contents of securinine,allosecurinine,rutin,bergenin,and gallic acid in different medicinal parts of Flueggea suffruticosa,and analyze their differences.4.The method of vinegar and alcohol preparation in Appendix 0213 of Part IV of the Chinese Pharmacopoeia(2020)was used to prepare the medicinal material of Flueggea suffruticosa monophylla.The content of total alkaloids and total flavonoids in raw,alcoholic,and vinegar products of Flueggea suffruticosa monophylla was determined by UV spectrophotometry.The content of Flueggea suffruticosa monophylline,gallic acid,and rutin was determined by HPLC,and the differences between raw and processed products were compared and analyzed.Results: 1.Based on the observation and measurement of the medicinal herb Flueggea suffruticosa,combined with relevant literature,an objective and practical description of its properties was made.The medicinal powder has obvious microscopic identification characteristics,thin layer chromatography identification,good sample resolution,and clear spots.The water content of 16 batches of Flueggea suffruticosa monophylla herb ranged from 7.65% to 10.35%,with an average value of 9.26%;The total ash content is 5.67% to8.29%,with an average value of 6.96%;The acid insoluble ash content ranges from 0.61%to 1.98%,with an average value of 1.17%;The content of heavy metals and harmful elements does not exceed the inspection limit;The mass fraction of alcohol soluble extract determined by hot leaching method is between 22.77% and 37.24%,with an average value of 29.15%.2.Flueggea suffruticosanine content: The content of Flueggea suffruticosanine in 16 batches of samples ranges from 1.003 to 6.872 mg/g,with significant differences between batches,with the content of Flueggea suffruticosanine in dried leaves ranging from an average of 3.873 mg/g;The average content of securinine in twigs with mosaic leaves is2.276mg/g,and the content of securinine in dried leaves is higher than that in twigs with mosaic leaves.Rutin content: The content of rutin in 16 batches of medicinal materials ranges from12.4249 to 20.3034 mg/g,with an average value of 16.1082 mg/g.The average content of rutin in leaves and twigs with flower leaves is 16.9524 mg/g and 14.0706 mg/g,respectively.Gallic acid content: The content of gallic acid in 16 batches of medicinal materials ranges from 0.8206 to 1.6820mg/g,with an average value of 1.3071mg/g.The average content of gallic acid in leaves and twigs with flowers is 1.3056mg/g and 1.4258mg/g,respectively.Bergenin content: The content of bergenin in 16 batches of medicinal materials ranges from 0.1970 to 0.8045mg/g,with an average value of 0.4112mg/g.The average content of gallic acid in leaves and twigs with flowers is 0.4595mg/g and 0.3134mg/g,respectively.Fingerprint of Flueggea suffruticosa Herb: A total of 15 common peaks were calibrated,and three components,gallic acid,bergenin,and rutin,were identified.The similarity is greater than 0.920,indicating that the overall similarity of the chemical components of Flueggea suffruticosa is high,the quality of the medicinal material is relatively stable,and there is good consistency.3.Fingerprint of different medicinal parts: The similarity between fingerprints of different batches of the same part is greater than 0.920.A total of 14 common peaks have been marked for the leaves,9 common peaks have been marked for the stems,and 7common peaks have been marked for the roots.Through cluster analysis and principal component analysis,30 samples of 10 batches of medicinal materials are divided into two types,with leaves and stems being one type,and roots being one type.4.Determination of the content of different medicinal parts: The average content of securinine and allosecurinine in the leaves was 3.4560mg/g and 0.0821mg/g,respectively;The average content of securinine and allosecurinine in the stem was 0.7322mg/g and0.0397mg/g,respectively;The average content of securinine and allosecurinine in roots was5.1673mg/g and 18.1583mg/g,respectively.The order of average content from high to low is: root>leaf>stem,and the content of securinine in root is much higher than that in leaf stem(about 200 times as much as leaf and 400 times as much as stem).The average contents of gallic acid,bergenin,and rutin in leaves were 1.9855mg/g,0.4956mg/g,and 19.5427mg/g,respectively;The average contents of gallic acid,bergenin,and rutin in the stems were 0.7017 mg/g,0.2854 mg/g,and 3.5353 mg/g,respectively;The average content of gallic acid and bergenin in roots was 3.3405 mg/g and 93.9588 mg/g,respectively,with the order of gallic acid content from high to low: root>leaf>stem;The rutin content is: leaves>stems,and roots almost contain no rutin.The content of bergenin is as follows: root>leaf>stem,and the content in root is much higher than that in leaf and stem(about 300 times as much as stem and 180 times as much as leaf).5.Content of ingredients before and after processing: After preparing Flueggea suffruticosa vinegar,the contents of total alkaloids and Flueggea suffruticosa alkaloids in the sample were higher than those in the raw product(P<0.05),while the contents of total flavonoids and rutin were lower than those in the raw product(P<0.05).There was no difference between gallic acid and the raw product(P>0.05);After brewing,the contents of total alkaloids,securinine,and gallic acid were basically equivalent to those of the raw product without any difference(P>0.05);The content of total flavonoids and rutin was lower than that of raw products(P<0.05).Conclusion: 1.A draft quality standard for Flueggea suffruticosa monophylla was prepared.See Appendix 1 for details.2.A stable,reliable and reproducible method for the determination of securinine in Flueggea suffruticosa monophyllum was established,which can be used for the determination of the content of Flueggea suffruticosa monophyllum;The content of gallic acid,bergenin,and rutin in Flueggea suffruticosa was determined using a one test multiple evaluation method,and the HPLC fingerprint of Flueggea suffruticosa was established.A total of 15 common peaks were calibrated,and three characteristic peaks were identified after comparison with the mixed control sample chromatography,providing a basis for the quality control and further research of Flueggea suffruticosa.3.Comparative study on leaves,stems,and roots of different medicinal parts.According to the content determination results and the fingerprints of leaves,stems,and roots,the fingerprints of leaves and stems are more similar,with significant differences from roots.Although the contents of securinine,allosecurinine,gallic acid,and rutin in the roots are higher than those of the leaves and stems,due to the fact that the original plant of securinine is a perennial shrub,leaves,twigs,or flowering twigs can be harvested year by year during the flourishing and flowering stages of the branches and leaves;Roots cannot be harvested at any time,and harvesting is not easy."The content of the five components in the leaves is higher than that in the stems,so the medicinal site of Flueggea suffruticosa monophylla is designated as a dry leaf or a stem with floral leaves.".4.From the comparison of data only,the preparation method of Flueggea suffruticosa vinegar is slightly superior to the wine preparation method,but this is only a preliminary discussion based on the changes in chemical components before and after processing.Later,pharmacological experiments and clinical observations should be combined to make the processing research more convincing. |
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