Preparation Process And Quality Control Study Of The Preparation Of Salidroside From Ligustrum Lucidum Based On Alkali Transformation

This paper includes six chapters.The first chapter is the summary of the related literatures;the second chapter is the investigation preparation technology of the salidroside in Ligustrum lucidum Ait. by alkaline hydro lys is;the third chapter is the quality control method of the saIidroside preparations;the forth chapter is the quality control method of the fructus ligustri lucidi;the fifth chapter is the correlation analysis of different places of Fructus ligustri lucidi medicinal materials of convertible composition;the sixth chapter Summary and discussion.The first chapter:Summary of the related literaturesSummary the current situation of research about the Ligustrum lucidum Ait. The introduction includes the following aspects of the Ligustrum lucidum Ait:the resources, species identification,processing methods,chemical composition,pharmacological action and enrichment process.In addition, pharmacological literatures of salidroside and the study of toxic reactions were also summarized.Through the literature review found that rhodiola glucoside of preparation technology and Ligustrum lucidum Ait medicinal materials quality control remains to be firther improved,this topic is the study of these two issues.The second chapter:The investigation preparation technology of the salidroside in Ligustrum lucidum Ait by alkaline hydrolysisThe preparation of Rhodiola glucoside parts reference to Lijuan's dissertation chapter 2 of 3 quarter.By extraction,alkalization, macroporous resin enrichment the results were?extracting rate was Al%, salidroside preparation 1 (enrichment) yield A2%, salidroside content was A3% and salidroside conversion (equivalent to crude drug) was A4%.Establish a process for the preparation of Salidroside impurity content of more than 90% of salidroside preparations. Salidroside as index component, using HPLC detection method, impurity conditions investigated by E, F crystallization conditions study to guide established Salidroside content greater than 60%,90% of salidroside preparations impurity removal processes.Extraction Process validation results for three batches:Salidroside preparation 1 (enrichment),the average yield of As%,the average content of salidroside were A6%; Salidroside preparation 3 (pure substance) of the average yield was A7%, the average content of salidroside wsa Ag%, indicating that the process s stable and feasible.The third chapter:Quality control method of the salidroside preparationsQuality control method of the salidroside was established based on alkaline conversion. Salidroside content was determined by HPLC.The regression equation of salidroside was Y=251659X+95112,r=0.9998,The regression equation of tyrosol was Y=654860X+35312,r=0.9990 (n=6) indicating that the content of salidroside and tyrosol respectively had a favourable linear relationship in the range of 0.50?g?10.00?g and 0.05?g?1.00?g.Precision,stability,repeatability, sample recovery rate all meet the requirements. The experiment results as follows,In Salidroside preparation 1 (enrichment) the average content of salidroside was B1%,the average content of tyrosol was B2%, Salidroside preparation 2 Salidroside average content was B3%, the average content of tyrosol was B4%, salidroside preparation 3 (pure substance) in the average content of salidroside was B5%, average abohol content of casein was B6%.With TLC controlling the Salidroside preparations qualitative quality, salidroside and tyrosol as reference,with chloroform - methanol - formic acid (5:1:0.2) as the agent, r the test chromatogram and the reference substance chromatography corresponding position had the same the same color spots.TLC analysis quickly,a small amount of qualitative preparation ingredients.High performance liquid chromatography analysis, by adding the reference method were compared,it can clear the main ingredient preparation salidroside and tyrosol.Seven characteristic peaks in HPLC feature maps,were phenylethanoid glycosidessubstance.By joining reference to identify the four index components, salidroside, salidroside,tyrosol.The forth chapter:Quality control method of the fructus ligustri lucidiQuality control method of the salidroside and butyl alcohol were established based on alkaline conversion.Salidroside and butyl alcohol was determined by HPLC.The regression equation of salidroside was Y= 250015X+ 38698, r=0.9995 (n=6),The regression equation of tyrosol was Y=573935X-11118,r=0.9998 (n=6), indicating that the content of salidroside and tyrosol respectively had a favourable linear relationship in the range of 0.50?g?10.00?g and 0.05?g?1.00?g.Precision,stability,repeatability,sample recovery rate all meet the requirements. The measured results:herbs Salidroside average C1%,the average content of tyrosol C2%. Precision,stability,repeatability,sample recovery rate all meet the requirements.Quality control method of the Specnuezhenide was established based on alkaline conversion.Specnuezhenide was determined by HPLC. The regression equation of salidroside was Y=1055353X-5055,r=0.9999,(n=8), indicating that the content of Specnuezhenide had a favourable linear relationship in the range of 1.50?g?20.00?g. Precis ion, stability, repeatability, sample recovery rate all meet the requirements. Measured results:fructus ligustri lucidi medicinal materials in privet nucleoside average content is D1%, total conversion component relative peak area should be not less than D2, the relative content should not be less than D3%.Quality control method of the thin layer chromatography of fructus ligustri lucidi was established.Salidroside and Specnuezhenide as reference substance,the chromatogram condition was Chloroform-methanol-formic acid (8:1:0.2). In the chromatogram of the test, in the position of the same as the reference substance chroma to graphy,the same color spots. From the thin layer chromatography analysis,it can quickly know the qualitative composition of a small amount of fructus ligustri lucidi.A total of eleven characteristic peaks in HPLC feature maps, including two C, five D,four B. By joining reference to identify the four index components, salidroside, salidroside,tyrosol, Specnuezhenide and Quercetin.The fifth chapter:The correlation analysis of different places of Fructus ligustri lucidi medicinal materials of Convertible compositionPrepared by Chapter ?' based on the production technology base into Ligustrum Salidroside series preparation of research" 15 batches of different origin Ligustrum lucidum salidroside crystals were yield in the order of Sample 15>11>6>13>9>7>1>12>14>5>2>3> 10>4>8,using liquid chromatography with salidroside,tyrosol,especially privet glycosides reference,the origin of the 15 index components Ligustrum lucidum quality characterize the different habitats found the biggest difference can be converted into components of 49.43 times,in the order of15>11>6>13>9>7>1>12>14>5>2>3>10>4>8;content thus known in different Areas Ligustrum salidroside yield components and can be converted into a positive correlation,namely in Ligustrum lucidum the more ingredients can be converted salidroside higher yield.The sixth chapter:Summary and discussion1 To establish the investigation preparation technology of the Salidroside in Ligustrum lucidum Art. by akaline hydrolysis.2 To establish the quality control method of the Salidroside in Ligustrum lucidum Ait. by akaline hydrolysis.3 For the first time based on rhodiola glucoside,tyrosol,transformation of material substances established the quality cortrol of fructus ligustri lucidi medicinal materials.4 Transformations in fructus ligustri lucidi medicinal materials different regions are analyzed for the first time associated with the yield of rhodiola glucoside.