Study On Chemical Characteristics Of Magnoliae Flos And Production Quality Of Its Extract

Magnoliae Flos is dry bud of Magnolia biondii Pamp,Magnolia sprengeri Pamp or Magnolia denudate Desr It is one of the traditional Chinese herbal medicines and has a long history.It is a necessary treatment for headache and nasal congestion.In recent years,Magnoliae Flos has a wide range of applications.Not only being used in the clinical formula,but also used as a raw material for extracts and high-grade spices,that is widely used in medicine,food processing,high-grade cigarettes,cosmetics,and daily-use chemicals and so on.In the market,the main variety of Magnoliae Flos is M.biondii Pamp,which is produced mainly in Henan and circulates nationwide;followed by M.sprengeri Pamp,which is mainly produced in Sichuan,Hubei,and is generally producing and marketing all by itself.M.denudate Desr almost has no medicinal materials in the maket.There are many manufacturers of magnoliae Flos extract on the market,and the product categories can be divided into powder and volatile oil,the specifications and prices are different,they are sold at home and abroad,and are used for the addition of medicines,health products,and foods.However,the chemical composition and content of different varieties of Magnoliae Flos is different.In view of the complex source of medicinal materials and the quality of market extracts,this paper looks for the chemical characteristics of different varieties of medicinal materials,and then conducts a systematic research on the quality of commercially available extracts of Magnoliae Flos,which provided the reference frame for extracts of Magnoliae Flos about identifying variety and formulating quality standards.The research content and results are as follows:1 Through survey of production and market,we have ascertained the mainstream varieties of Magnoliae Flos and the production status of extract of Magnoliae Flos in maket.On the basis of literature research and previous work,through on-the-spot investigation of the mainstream varieties of Magnoliae Flos and their main producing areas on the market,it was ascertained that the main varieties of Magnoliae Flos is M.biondii Pamp,less M.sprengeri Pamp,no M.denudate Desr on the market,and there are still grafted varieties flowing in the commodity.Extract of Magnoliae Flos has pulverescent and volatile oil,pulverescent extract are divided into water extract and alcohol extract,and the excipients are starch,dextrin,or maltose.Its manufacturers are mainly concentrated in Xian of Shanxi,in addition,Lanzhou of Gansu,Changsha of Hunan,Ningbo of Zhejiang,also have production.Volatile oil extract manufacturers are mainly concentrated in Jian of Jiangxi,Guangdong of Guangzhou,in addition to Xian of Shanxi,Shenzhen of Guangdong,Nanzhao of Henan also have production.2 HPTLC,HPLC,and GC-MS methods for the different varieties of Magnoliae Flos were established to find the characteristic chemical composition,aimed to provide scientific basis for variety identification,the source of the extract,and then study on the extract of Magnoliae Flos.2.1 With magnolin and Lysopride B Dimethyl ether as the reference substances,the HPTLC identification method of Magnoliae Flos was established for the first time through the experiments of extraction method,spread system,spread distance,sample volume,temperature,and humidity.The method had a good resolution and rapidness,the development time was about 10 minutes,which greatly shortened the time compared with TLC,as well as having a good stability and repeatability.By HPTLC,20 batches different origins and varieties of Magnoliae Flos and 2 batch of grafted varieties were conducted.The results showed that the chromatogram spots of 10 batches M.biondii Desr were consistent,but No.1,No.6,and No.10 samples were smaller and lighter,and the other samples had larger chromatographic spots and darker colors.the chromatogram spots of 10 batches M.sprengeri Pamp were consistent,but No.3,No.4,No.5 and No.12 samples were smaller and lighter,and the other samples had larger chromatographic spots and darker colors.The Magnoliae Flos among different varieties appeared the same color spots in the spots corresponding to Magnolin reference substance,the spots of M.biondii Pamp were obvious.M.sprengeri Pamp,and M denudate Desr only faintly visible;In the spot corresponding to the spots of Lysopride B Dimethyl ether reference substance,spots of the same color were found in the M.biondii Pamp,but none in the M.sprengeri Pamp,and M denudate Desr.Lysopride B Dimethyl ether is a unique chemical composition of M denudate Desr and can distinguish M.biondii Pamp from M.sprengeri Pamp,In addition,compared with the chromatograms of M.sprengeri Pamp and M denudate Desr,the spots were basically consistent.But at Rf 0.39,spots could be detected in M denudate Desr,while it could not be detected in M.sprengeri Pamp It can be used as a reference in the variety identification.The chromatographic spots of grafted varieties 1 were the same as those of M.biondii Pamp Lysopride B Dimethyl ether was not detected in the grafted varieties 2,and its overall Chromatogram was basically the same as that of M denudate Desr,but there was a spot where the Rf was 0.50 was not detected in M denudate Desr and other varieties,so the grafted varieties of Henan can be distinguished.In summary,the chemical components of the same varieties of Magnoliae Flos medicinal materials among different origins were consistent,but their content were different.The chemical components and content of the diffrent varieties of Magnoliae Flos and grafted varieties were different,it can be distinguished by chemical characteristics.2.2 The HPLC-DAD analysis method was first established for different varieties of Magnoliae Flos that has good stability,reliability,and repeatability.Compared reference fingerprints of M.biondii Pamp and M.sprengeri Pamp,there were 13 common peaks conformed in the former and 5 in the latte,and there were three common peaks,that indicating that the chemical components of the different varieties of Magnoliae Flos were quite different.By analyzing the similarity of different varieties of Magnoliae Flos,it could be concluded that the similarity among the 11 samples of the M.biondii Pamp.was high.While among the samples of the 11 batches of M sprengeri Pamp was relatively low,It shows that there are differences in the chemical composition among the samples of M sprengeri Pamp,which may be related to the origin,processing and storage.22 batches of Magnoliae Flos from M.biondii Pamp and M sprengeri Pamp can be divided into two groups by cluster analysis.And there is no inclusion between different varieties,indicating that there are significant differences in chemical composition among different varieties.Comparing grafted varieties with different varieties of Magnoliae Flos can find out their own similarities and differences.The chromatogram of grafted variety 1 was consistent with M.biondii Pamp,and the peak area of magnolin and Lysopride B Dimethyl ether was also large.The chromatogram of grafted variety 2 were different from different varieties of Magnoliae Flos.This is consistent with the results of high performance thin layer chromatography.2.3 GC-MS analysis method was used to analyze the volatile oils extracted from the samples of different varieties of Magnoliae Flos and grafted varieties,to find similarities and differences.33,40,25,31,27 chemical compositions were identified in the volatile oil of M.biondii Pamp,M sprengeri Pamp.,M denudate Desr,grafted varietie 1,grafted varietie 2.The chemical composition of different varieties of Magnoliae Flos and grafted varieties has a great different.Piperone,alpha-pinene,(2Z,6E)-farnesol was identified in the volatile oil of M.biondii Pamp,while other varieties were not.methyl heptenone,cuminyl alcohol,perilla alcohol,(+)-cycloparene,isoeugenol methyl ether,a-gurjunene,3,7(11)-eucalyptus,Espatulenol,a-eucalyptus alcohol was identified in the volatile oil of M sprengeri Pamp,while other varieties were not.methyleugenol was identified in the volatile oil of M denudate Desr,while other varieties were not.In addition to the unique components of M.biondii Pamp,the chemical composition of the volatile oil of the grafted varieties 1 is basically the same as that of M.biondii Pamp,the composition is coincident with other varieties.was identified in the volatile oil of grafted varieties 2,while other varieties were not.3 HPLC-DAD method was established for the determination of magnolin and Lysopride B Dimethyl ether in Magnoliae Flos,and the content of magnoliae Flos samples was determined,which provided a reference for improving the quality standard of the Magnoliae Flos and evaluating the quality of extracts of Magnoliae Flos.In this experiment,the chromatographic conditions were investigated,the method for extracting the test solution,and the methodological verification of the linear relationship,precision,stability,and repeatability were performed.The HPLC-DAD determination method of magnolin and Lysopride B Dimethyl ether was established,and the content of 25 batches Magnoliae Flos and grafted varieties were determined.The results showed that the content of Magnolin of 11 batches M.biondii Pamp was up to 5.03%,the lowest was 1.90%,and the average was 3.43%,Lysopride B Dimethyl ether was up to 1.41%,the lowest was 0.51%,and the average was 0.83%.Grafted varieties 1 contained high magnolin and Lysopride B Dimethyl ether,and the contents were 4.01%,0.62%.magnolin and Lysopride B Dimethyl ether had not detected in M sprengeri Pamp,M denudate Desr,and grafted varieties 2.4 Based on the established research method for the Magnoliae Flos,the first systematic research on the quality evaluation of the magnolia Flso extracts on the market was carried out,combing the basic profile of extracts on the market,and provided a reference for the further study of quality standard4.1 The established HPTLC chromatography was used for the variety identification of 10 batches of water extracts of Magnoliae Flos and 4 batches of alcohol extracts of Magnoliae Flos collected from 9 manufacturers on the market.Comparing with homemade alcohol extracts and water extracts of Magnoliae Flos,The results show that only 3 manufacturers of 4 batches extract powders can determine the feeds of the magnolia varieties through the comparison of chromatography spots,namely A7,A8 and A9 water extracts may be expected to be M.biondii Pamp,A7-1 alcohol extracts may be expected to be M sprengeri Pamp No chromatographic spots were detected in the water or alcohol extract powders of the remaining manufacturers.It was suspected that no medicinal materials were being fed at all,and only processing excipients were included.4.2 The established HPTLC chromatography was used for the variety identification of 10 batches of water extracts of magnoliae Flos and 4 batches of alcohol extracts of Magnoliae Flos collected from 9 manufacturers on the market.Compared with the homemade alcoholic extracts and water extracts of Magnoliae Flos,The results show that only 4 manufacturers of 5 batches extract powders can determine the feeds of the magnolia varieties through the comparison of chromatography spots,namely A7,A8 and A9 water extracts may be expected to be M.biondii Pamp,A7-1 alcohol extracts may be expected to be M sprengeri Pamp.A10-1 water extracts may be expected to be M.biondii Pamp No chromatographic peak were detected in the water or alcohol extract powders of the remaining manufacturers.This result is consistent with HPTLC.4.3 GC-MS was used for the variety identification of 10 batches of volatile oils magnoliae Flos collected from different manufacturers on the market.By comparing the total ion chromatograms,mass spectrum and the chemical characteristics,the results showed that only 2 batches of 10 batches extracts were consistent with the characteristics of the M.biondii Pamp,namely B15,B16.Other samples is different from the M.biondii Pamp and M sprengeri Pamp,.it may be related to raw materials and production processes.4.4 Routine inspections such as particle size,weight loss on drying,residue on ignition,heavy metals and harmful elements inspections of extracts of Magnoliae Flos from different manufacturers.which provided a reference for the further development of the quality standard of extracts of Magnoliae Flos.4.5 The physical constan include refractive index,optical rotation rate,relative density and inspection of insoluble in ethanol of volatile oil of Magnoliae Flos about different manufacturers were detected.which provided a reference for the further development of quality standard for volatile oil extracts of magnoliae Flos.