| Epimedium is a traditional Chinese herbal medicine for tonic benefit.It is warm in nature,sweet and sweet,and belongs to the liver and kidney meridians.It has the effects of nourishing kidney yang,strengthening bones,and removing rheumatism,and is suitable for treating kidney yang deficiency,impotence nocturnal emission,soft bones,rheumatism and pain,numbness and paralysis.Epimedium has rich flavonoids.Modern pharmacological research showed that Epimedium flavone has a wide range of biological activities,such as anti-osteoporosis,anti-tumor and so on.In this article,the extraction and purification of total Epimedium flavones were investigated and a preliminary study was also conducted on the partial molding process of total Epimedium flavones to be prepared into the contents of enteric-coated capsules by using Epimedium tablets as raw materials.It is expected to provide a preliminary research basis for the development of a new anti-osteoporotic Chinese medicine preparation total Epimedium flavones Enteric-Coated Capsules.In this paper,we first review the literature on the anti-osteoporosis pharmacological activity of Epimedium flavonoids,the extraction and purification of flavonoids and the research on new preparations of Epimedium flavonoids;And the following three aspects of the experimental part of the research:1.Optimization of Extraction Process of Total Flavones EpimediumThe extraction process of total Epimedium flavones was investigated by ethanol reflux extraction.Taking the content of total Epimedium flavones and five representative flavonoids as indicators of investigation,four factors such as ethanol concentration,solid-liquid ratio,extraction time,and extraction times were screened by single factor experiments.On the basis of single-factor experiments,the orthogonal experiment was used to optimize the extraction process of total Epimedium flavones.Determine the optimal extraction process conditions:weighing a certain amount of Epimedium tablets,in addition to adding 3.5 times the amount of alcohol absorption for the first time,the rest is added at 60%ethanol according to a solid-liquid ratio of 1:15,and refluxed for 3 times 1.5 h each time,And the optimized process obtained is enlarged and verified.The content of total flavonoids Epimedium is 105.55 ± 4.86 mg/g crude drug,RSD is 4.61%,the sum of 5 flavonoids components is 19.52± 0.68 mg/g crude drug,RSD value is 3.49%,which showed that the optimized optimal process is stable and feasible.2.Optimization of Purification Process of Total Epimedium Flavones by Macroporous Adsorption ResinTaking the adsorption and desorption performance of macroporous adsorption resin for total Epimedium flavones and 5 representative components(Icariin,Epimedin A,Epimedin B,Epimedin C,Baohuoside I)as indicators of investigation.Adopting a combination of static adsorption and dynamic adsorption to compare the adsorption characteristics of five different types of macroporous adsorption resins,HPD100,HPD600,AB-8,X-5,and D101.The HPD100 macroporous adsorption resin obtained was more suitable for the enrichment and purification of total Epimedium flavones;And screening HPD100 macroporous adsorption resin from five different manufacturers,The HPD 100 macroporous adsorption resin of Xi'an Lanxiao Technology New Materials Co.,Ltd.was found to be more suitable for the enrichment and purification of total Epimedium flavones.The physical adsorption characteristics of total Epimedium flavones by HPD 100 macroporous adsorption resin were investigated.Taking total Epimedium flavones and 5 representative flavonoid monomers as indicators,To investigate the adsorption kinetics and adsorption thermodynamic process of Epimedium flavonoids by HPD 100 macroporous adsorption resin,The results showed that the adsorption kinetics of total Epimedium flavones and five representative flavonoids by the HPD 100 macroporous adsorption resin conforms to the pseudo-second-order kinetic model,and the adsorption thermodynamic process of total Epimedium flavones conforms to the Freundlich adsorption isothermal model,the adsorption thermodynamics process for the sum of the five flavonoids complies with the Langmuir adsorption isotherm model;The adsorption process of HPD 100 macroporous adsorption resin for total Epimedium flavones is an exothermic process dominated by physical adsorption,and the optimal adsorption temperature is 25?.The process parameters of total Epimedium flavones purification by macroporous adsorption resin were optimized.Taking total Epimedium flavones and 5 representative flavonoid monomers as indicators,column solutions with different ethanol concentrations(0%,5%,10%,15%,20%,30%),sample flowrate(0.5,1,2,4,6 BV/h),sample concentration(0.05,0.1,0.5,1.0,1.5 g/mL),sample loading(40,20,4,1.2,1.2 BV),water washing amount(3?18 BV),decontamination ethanol concentration(20%,25%,30%)and dosage(1-8 BV),elution ethanol concentration(40%,50%,60%,70%)and dosage(1?8 BV)purification parameters of macroporous resins were examined.The final preferred purification process is:taking total Epimedium flavones extract(containing 15%ethanol)with a crude drug mass concentration of 0.5 g/mL,load it on the column,and load it at 25? for 1 h at a flow rate of 1 BV/h.8 BV of distilled water washes away water-soluble impurities such as sugars,5 BV of 25%ethanol to remove other impurities,and then eluted with 4 BV of 60%ethanol.The eluate was collected and dried under vacuum at 40? to obtain total Epimedium flavones extract.In the small test,the yield of total flavonoids of Epimedium prepared by the preferred process in this thesis was 3.53%,Among them,The purity of icariin,epimedin A,epimedin B,epimedin C,baohuoside I,the total flavonoids and the sum of the five flavonoid components are 16.94%,3.45%,5.55%,3.65%,1.04%,64.09%,30.63%,compared to the total flavonoids of Epimedium extract from different manufacturers are higher.Using the above-mentioned preferred extraction and purification process for pilot scale-up,the total flavonoid extract yield of Epimedium is 3.36%,Among them,the purity of icariin,epimedin A,epimedin B,epimedin C,baohuoside I was 27.24%,3.51%,4.76%,3.52%,and 1.30%,compared with the results of the small test,the purity of icariin was increased by nearly 10%,and the remaining components were all within 0.8%.The purity of the total flavonoids and the sum of the five flavonoid monomers is 74.00%and 40.34%,which is nearly 10%higher than the results of the small test.It shows that HPD100 macroporous adsorption resin can effectively purify the total flavonoids of Epimedium,and the purification process is stable and feasible.3.Preliminary Study on The Formulation of Total Epimedium Flavones Enteric-coated CapsulesThe forming process of the contents of total Epimedium flavones enteric-adhesive capsules was discussed.Taking the setting rate of the granules,the setting parameters of the granulation at one time,and the cumulative release of total flavones Epimedium in 12 h and the enzymatic hydrolysis as indicators,the effects of fillers(dextrin,corn starch ratio),snail enzyme,carbomer,and addition ratio on the contents of enteric-coated capsules prepared by dry granulation were investigated.Experimental results showed that dextrin is more suitable as a filler for dry granulation;The addition of snail enzyme will affect the compressibility of the overall material of the formulation,resulting in difficult granulation.The addition of carbomer has little effect on the molding rate of the particles,but it can improve the effect of snail enzyme on the material and increase compressibility.In addition,the formability of the particles is increased,but the addition of carbomer will delay the release of total Epimedium flavones;Total Epimedium flavones enteric-adhesive capsules were granulated by dry granulation with a prescription ratio of:total Epimedium flavones extract:snail enzyme:dextrin:carbomer=6:1:2:0.25. |
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