Optimization of the Purification Technology of Total Triterpenoids of Ligustrum lucidum by Box-Behnken Re- sponse Surface Methodology / 中国药房

OBJECTIVE：To i mprove the transfer rate and purity of oleanolic acid and ursolic acid in total triterpenoids from Ligustrum lucidum ，so as to optimize the purification technology. METHODS ：Oleanolic acid and ursolic acid were used as representative components of total triterpenoids ，and their contents were determined by HPLC. The determination was performed on Thermo BDS Hypersil C 18 column with mobile phase consisted of methanol- 0.02％ ammonium acetate solution （80∶20，V/V）at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm，and column temperature was 30 ℃. The sample size was 20 μ L. In single factor tests，using transfer rate of oleanolic acid and ursolic acid as index ，the effects of water precipitation temperature and time ，the amount of redissolved ethanol on the purification technology was investigated ；using transfer rate and purity of two components as indexes ，the effects of the amount of activated carbon and volume fraction of crystallization ethanol were investigated. Based on it ，using the amount of redissolved ethanol and activated carbon ，volume fraction of crystallization ethanol as factors ，Box-Behnken response surface methodology was used to optimize the purification technology ，and validation tests were performed. RESULTS ：The optimal purification technology was adding 4-fold（mL/g，the same below ）water in L. lucidum concentrated solution ，placing for 2 hours at 0 ℃（water precipitation ）；adding 1-fold ethanol to dissolve （redissolution）； adding 4％ activated carbon （edulcoration）；finally adding water to adjust the volume fraction of ethanol to 80％，placing at 4 ℃ for 12 hours（crystallization），centrifuging and drying. The results of 3 times of validation tests showed that the transfer rates of oleanolic acid and ursolic acid in total triterpenoids prepared by optimized technology were 61.11％ and 65.78％，the purities of them were 53.44％ and 19.79％，and RSDs were both lower than 3％. CONCLUSIONS ：The optimized purification technology has high extraction efficiency and simple operation ，which can be used for industrial production of purification of total triterpenoids from L. lucidum and the development of corresponding preparations.

Study on the Optimization of Purification Technology of Total Flavonoids from Amomum tsao-ko by Macroporous Adsorption Resin / 中国药房

OBJECTIVE：To establish a method for the content determination of to tal flavonoids from Amomum tsao-ko ，and to optimize the purification technology by macroporous resin. METHODS ：The content of total flavonoids was measured by HPLC. The determination was performed on Eclipse Plus C 18 column with mobile phase consisted of acetonitrile- 1％ acetic acid solution （15∶85，V/V）at the flow rate of 0.8 mL/min. The column temperature was 40 ℃，and the detection wavelength was set at 256 nm. The sample size was 10 μL. Taking the adsorption and desorption performance as indexes，6 kinds of macroporous resins were screened out by static adsorption and desorption tests ；adsorption and desorption time were investigated by static adsorption and desorption kinetics tests. Using the content of total flavonoids （calculated by rutin ）as index ，with sample concentration ，sample pH，ethanol volume fraction and elution amount as factors ，based on single factor test ，orthogonal design was used to optimize the purification technology of total flavonoids from A. tsao-ko ，and validation test was performed. RESULTS ：The linear range of rutin were 0.028-0.281 mg/mL（r＝0.999 9）. The limit of quantification was 437.5 ng/mL and the limit of detection was 109.4 ng/mL. RSDs of precision ，stability and reproducibility tests were all lower than 2％；the recoveries were 96.24％-99.75％（RSD＜2％，n＝ 6）. The comprehensive capacity of adsorption and desorption of HPD 450 macroporous resin was the most suitable ，and the best static adsorption and desorption time both were 12 h. The optimal purification technology was 1.854 4 mg/mL ； ethanol elution was 8 times of the column volume. Vertificationtests show that after optimized ，the content of total flavonoids from A. tsao-ko increased from 22.556 7 mg/g to 57.728 2 mg/g. The purity of was 2.56 and stable for the content determination. Optimal purification technology is stable and feasible ，which is suitable for purifieation of total flavonoids from A. tsao-ko .

Optimization of Purification Technology of Gastrodia elata Total Polyphenols by Macroporous Resin / 中国药房

OBJECTIVE： To establish a method for content determination of total polyphenols from Gastrodia elata， and to optimize the purification technology of macroporous resin. METHODS： The content of total polyphenols from G. elata was determined by Folin-ciocaileu colorimetry. Using the absorption and desorption performance as index， 4 kinds of macroporous adsorption resins were selected by static adsorption and desorption tests. The flow rate and mass concentration of the sampling solution， volume fraction of eluent， eluent flow rate and eluent volume were investigated by dynamic adsorption and desorption tests. The purification technology of macroporous resin was optimized. RESULTS： The linear range of gallic acid was 4-32 μg/mL （r＝0.999 9）. RSDs of precision， stability and repeatability tests were all less than 2％. The recovery rate of the sample was 95.51％-102.94％（RSD＝2.54％，n＝6）. D301 macroporous resin had strong static adsorption and desorption ability from G. elata polyphenols. The optimal purification technology included that the sample solution flow rate 2 BV/h； the sample solution mass concentration 4 mg/mL； the elution solvent 70％ ethanol； the elution flow rate was 3 BV/h， and the eluent volume 5 BV. The content of total polyphenols from G. elata optimized by the optimal purification technology was 0.381 mg/g. CONCLUSIONS： Established method is sensitive and stable. The optimized purification technology is stable and feasible.

Optimization of Purification Technology of N-（E）-p-coumaroyltyrosine in Leaves of Abrus cantoniensis / 中国药房

OBJECTIVE： To establish a method for content determination of N-（E）-p-coumaroyltyrosine in leaves of Abrus cantoniensis， and to optimize its purification technology. METHODS： HPLC method was adopted for the content determination of N-（E）-p-coumaroyltyrosine in A. cantoniensis. The determination was performed on Hypersil BDS C18 column with mobile phase consisted of 0.1％ formic acid water （A）-methanol （B） （gradient elution） at a flow rate of 1.0 mL/min. The column temperature was set at 25 ℃. The detection wavelength was set at 300 nm， and sample size was 10 μL. Using polyamide resin as material， the yield of N-（E）-p-coumaroyltyrosine as indicators， single factor test was used to optimize the purification technology of N-（E）-p-coumaroyltyrosine， such as concentration， sample size， stationary adsorption time. RESULTS： The linear range was 2.575-51.50 μg （r＝0.999 9） for N-（E）-p-coumaroyl-tyrosine. The limit of quantification was 0.000 618 μg， and the detection limit was 0.000 129 μg. RSDs of precision， stability and reproducibility tests were all lower than 3％. The recoveries were 97.04％-102.43％ （RSD＝2.06％， n＝6）. The optimal purification technology was as follows： the concentration of the sample solution was 0.04 g /mL （by the leaves of A. cantoniensis）； sample capacity 50 mL； the sample flow rate was 1.0 mL/min； the stationary adsorption time was 20 min； the eluting solvents were ammonia containing water （containing 0.1％ acetic acid）， 20％ ethanol （containing 0.1％ acetic acid） and ammonia（pH 10）. Average yield was 98.94％，average dry paste content was 61.17 mg/g， and average dry paste purity was 19.73％ by optimal purification technology. CONCLUSIONS： Established method is simple， accurate and stable. The optimized technology is stable and feasible.

Study on the Separation and Purification Technology of Total Flavonoids from Sparganium stoloni by Box-Behnken Design- response Surface Methodology / 中国药房

OBJECTIVE： To optimize the purification technology of total flavonoids from Sparganium stoloniferum. METHODS： Separation and purification by macroporus adsorption resin， using sample solution pH， flow rate and concentration of eluent， the purification rate of total flavonoids as evalution indexes， the purification technology of total flavonoids from S. stoloniferum were optimized by Box-Behnken design-response surface methodology based on single factor test. Validation test was conducted. RESULTS： The optimal purification technology was sample solution pH 4.8， flow rate of eluent 2.0 BV/h， concentration of eluent 72％. The purification rate of total flavonoids in 3 batches of samples was 72.34％ （RSD＝1.77％， n＝3） in validation test， relative errors of which to predicted value （73.99％） was 2.13％. CONCLUSIONS： The optimal purification technology is stable and feasible， and can be used for the purification of total flavonoids from S. stoloniferum.

Study on the Purification Technology of Total Alkaloids from the Leaves of Nitraria sibirica with Macroporous Resin and Its Antioxidant Activity / 中国药房

OBJECTIVE:To optimize the purification technology of total alkaloids from the leaves of Nitraria sibirica with macroporous resin,and to evaluate its antioxidant activity. METHODS:Using the content of total alkaloids(by atropine sulfate)as index,static adsorption and analytical method were used to investigate the type of macroporous resin. Dynamic adsorption and analytical method were used to investigate the concentration of the sample solution,the pH of the sample solution,the flow rate of the sample solution,diameter-height ratio of column,sample capacity,the volume of elution water and volume fraction of elution solvent so as to optimize macroporous resin purification technology. Using vitamin C as positive control,scavenging capacity of total alkaloids to 1,1- diphenyl-2-diphenyl picryl hydrazinyl(DPPH)radicals was investigated to evaluate its antioxidant activity. RESULTS:The adsorption and desorption effects of HPD-450 macroporous resin on total alkaloids were the best. The optimal purification technology included the sample solution concentration 0.88 mg/mL,sample solution pH 6,sample solution flow rate 2 BV/h,diameter-height ratio of column 1∶8,sample capacity 5 BV,the volume of elution water 5 BV,elution solvent 30%ethanol. The content of total alkaloid was 16.94 mg/g,and IC50was (58.78 ± 3.00)μ g/mL by optimal purification technology. CONCLUSIONS:Optimized purification technology is stable and feasible,and can separate and purify total alkaloids from the leaves of N. sibirica. Purified total alkaloids display good antioxidant activities. The total alkaloids eluted with 30% ethanol show the strongest scavenging activity to DPPH radicals.

Simultaneous purification of shikimic acid and total flavonoids from pine needles of Cedrus deodara by macroporous adsorption resin / 中草药

Objective: To research the simultaneous purification process of shikimic acid and total flavonoids from pine needles of Cedrus deodara (Roxb.) G. Don. Methods: Taking the purity of shikimic acid and total flavonoids as the evaluation indicator, the purification effect of six macroporous resins were evaluated. Orthogonal design L9(34) and single factor experiments were employed to optimize the purification conditions by comprehensive scoring. The purification capacity of the best resin was investigated by the sample mass concentration, the volume flow of the sample, the ratio of the resin to the drug, the amount of water for washing, the concentration of ethanol, and the elution of ethanol. Results: XAD 7HP macrophous resin offered better purification effect of shikimic acid and total flavonoids from pine needles of C. deodara than other macrophous resins. The optimum purification condition was confirmed as follows: The concentration of shikimic acid in the sample was 11.59 mg/mL, and total flavonoids concentration was 6.9 mg/mL; The flow rate was 8 BV/h, and the sample volume was 2.0 mL/g; The shikimic acid was eluted with loading capacity and 4 BV of water; The total flavonoids was eluted with 4 BV of 70% ethanol successively. The purity of shikimic acid can be increased from 19.25% to 28.98%, and the purity of total flavonoids can be increased from 11.92% to 54.45%. Conclusion: The optimized purification process is stable, feasible and suitable for pilot enrichment of shikimic acid and total flavonoids from pine needles of C. deodara.

Study on purification, concentration and drying technic of Fushubao gel / 国际中医中药杂志

Objective To study the purification, concentration and drying technology of Fushubao gel. Methods The purification technology of Fushubao gel was optimizing by the total retention rate of Rhein, emodin, physcion and purity of content. The concentration, drying technology of Fushubao gel was optimized by the transfering rate of Rhein, emodin, physcion and Berberine hydrochloride. Results Best refining technology included in the condition of the water extract of 0.2 g/ml at 70 ℃, the ZTC1+1-II clarifying agent B 0.6 ml/g was mixed10 min in a 70 ℃ water bath thermal insulation 30 min; And then agent A 0.3 ml/g was added and mixed 10 min in a 70 water bath thermal insulation 30 min; after 12 h, filter it. Best thickening, drying technology was in the vacuum for -0.08~-0.09 MPa, a temperature of 60 ℃, the pressure was reduced to concentrate its relative density about 1.05 and concentrated liquid spray was dryed. Conclusions The purification, concentration and drying technology of Fushubao gel is reasonable, and can be used in the production.

Study on the Purification Technology of Sanhuang Yishen Formula / 中国药房

OBJECTIVE:To study the purification technology of Sanhuang yishen formula. METHODS:Using retention rate and impurity rate of purified total polysaccharide,astragaloside and calycosin glucoside as index,the purification effects of water extraction and alcohol precipitation method (50%,60%,70% ethanol) and clarifying agent method (101 juice clarifying agent, ZTC natural clarifying agent,chitosan clarifying agent) were respectively detected to screen the purification method;orthogonal test was used to optimize the technology parameters(mass concentration of liquid,amount of clarifying agent and pH of liquid)by the optimized purification method,and the verification test was conducted. RESULTS:The purification was better when using chito-san as clarifying agent with comprehensive score of 98.62;the purified technology parameters were mass concentration of liquid 1 g/mL,1% chitosan solution amount of 2 mL/g,pH 5.1;the average value of retention rate and impurity rate of purified total poly-saccharide, astragaloside and calycosin glucoside in verification test were 79.56%(RSD=1.24%, n=3), 78.11%(RSD=0.97%,n=3),79.46%(RSD=1.03%,n=3)and 32.18%(RSD=1.16%,n=3),respectively. CONCLUSIONS:Using chito-san as clarifying agent shows good purification effect for Sanhuang yishen formula,which is simple. The optimized technology is stable and feasible.

Study on the Purification Technology of Total Saponins from Asparagus cochinchinensis with Macroreticu-lar Resin / 中国药房

OBJECTIVE:To optimize the purification technology of total saponins from Asparagus cochinchinensis with macro-reticular resin. METHODS:Using content of total saponins from A. cochinchinensis as index,single factor test was used to investi-gate the macroreticular resin model,sampling adsorption time,mass concentration of the column,adsorption capacity,volume frac-tion and the amount of elution solvent,elution rate,and optimize the purification technology. And verification test was conducted. RESULTS:HPD-300 macroreticular resin showed strong absorption and desorption property. The optimal purification technology was that sampling adsorption time was 60 min,mass concentration of sample liquid was 0.1 g/mL,adsorption capacity was 120 mL(15 BV),it was eluded with 60% ethanol solution with 3 BV and elution rate was 4 BV/h. In the verification test,the average desorption rate of total saponins was 68.30%(RSD=0.95%,n=3). CONCLUSIONS:Optimized purification technology is sta-ble,feasible,and can easily separate and purify the total saponins from A. cochinchinensis.

Optimization of Extraction and Purification Technology of Total Flavonoids from Engelhardia roxburghi-ana and Content Determination of 3 Kinds of Effective Components / 中国药房

OBJECTIVE:To optimize the extraction and purification technology of total flavonoids from Engelhardia roxburghi-ana,and to establish the method for the content determination of 3 kinds of effective components. METHODS:Using the extrac-tion transfer rate of astilbin as index,single factor test was used to investigate extraction solvent,extraction method,volume frac-tion of percolation solvent ethanol,percolation material-liquid ration,soaking time before percolation and percolation rate of extrac-tion technology,and volume fraction of eluant ethanol in AB-8 resin purification technology. The contents of 3 effective compo-nents as astilbin,texifolin and engelitin in total flavonoids from E. roxburghiana were determined by HPLC. RESULTS:The opti-mal extraction technology was using 70% ethanol as extraction and percolation solvent,percolation extraction,soaking for 8 h be-fore percolation,percolation material-liquid ratio of 1∶16(g/ml),percolation rate of 30 ml/(min·kg). The purification technology was diluting the solution to 0.5 g (crude drug)/ml with water,ethyl acetate extraction,dissolved extract with 50% ethanol after evaporated to dryness,AB-8 resin for sampling,eluted with 50% ethanol,concentrating and drying. In verification test,extraction transfer rate of astilbin was more than 80%(RSD=0.42%,n=3). The contents of astilbin,taxifolin and engeletin in total flavo-noids from E. roxburghiana by purified were 57.94%,3.72% and 2.83%,respectively;the contents of 3 components accounted for 64.00% of total flavonoids. CONCLUSIONS:The extraction and purification technology is stable,rational and reliable;the content determination method of 3 effective components in total flavonoids of E. roxburghiana is accurate,simple and producible.

Study on the Purification Technology of 4 Active Components from Tripterygium wilfordii by Macroporous Resin / 中国药房

OBJECTIVE:To study the purification technology of 4 active components from Tripterygium wilfordii by macropo-rous resin. METHODS:The purification abilities of nine macroporous resins(ADS-5,ADS-8,HPD100,HPD300,HPD400, HPD450,HPD700,HPD722 and HPD750) were studied with the adsorption and desorption rates of triptolide,wilforlide,trip-tonide and tripterine as the index by static adsorption and desorption experiments for 4 active components from T. wilfordii,so as to screen optimal macroporous resins. Using transfer rate of active component as index,single factor test was used to investigate the effects of different sampling method,ratio of mixing sample to total resin quantity,ratio of resin to medicinal material,cleaning so-lution(type,amount and cleaning flow rate),diameter- height ratio of resins,eluant(volume,flow rate)on adsorption,so as to determine the optimal elution technology;validation test was also conducted. RESULTS:HPD722 macroporous resin was chosen as adsorption resin;ratio of diameter to height was 1∶10,resin-medicinal material ratio was 1∶2,and ratio of mixing sample to to-tal resin quantity was 1∶10;wet column installing and mixing resin for sample loading were adopted. The macroporous resin was washed with 12 BV 20%ethanol at the rate of 12 BV/h,and then eluted with 12 BV 95%ethanol at the rate of 6 BV/h. The verifi-cation test results showed that the total transfer rate of 4 active components from T. wilfordii was more than 90%(RSD=0.99%, n=3). CONCLUSIONS:The optimized technology is stable and feasible,and suitable for the purification of 4 active components from T. wilfordii.

Effect of Different Purification Technology on Physical and Chemical Properties of Water Extract of Ophio-pogonin / 中国药师

Objective:To explore the effect of different separation and purification technology on the physical and chemical proper-ties of water extract of ophiopogonin. Methods:The water extraction process of total ophiopogon saponins was optimized by an orthogo-nal test. The macroporous resin adsorption and membrane separation technology were adopted to purify the ophiopogonin water extract. The physical and chemical parameters, such as electrical conductivity, pH value, viscosity and turbidity, and the contents of total sap-onins, proteins, tannins and polysaccharides were determined. Results:The optimum water extraction technology of total saponins was as follows:6-fold amount of water was added, boiling 3 times with 90 min for each time. The electrical conductivity, pH value and vis-cosity of different purified liquid of total saponins had no significant differences, while the contents of total saponins and the three kinds of macromolecules showed significant differences. Conclusion: The content of macromolecules can be used as the reference index of purification process of total saponins water extract. Compared with macroporous resin separation, membrane separation technology is more suitable for the separation and purification of total saponins water extract.

Optimization of Clarification and Purification Technology of Perillae folium Extract / 中国药房

OBJECTIVE:To optimize the clarification and purification technology of Perillae folium extract. METHODS:The effects of 3 clarification and purification methods as chitosan flocculation clarification,ZTC 1+1-Ⅱflocculation clarification,water precipitation on retention rate of total flavonoids and removal rate of solid of Perillae folium extract were compared to screen suit-able clarification and purification technology. With the retention rate of total flavonoids and removal rate of solid as comprehensive evaluation index,single factor and orthogonal test were designed to investigate the optimal value of concentration proportion,the amount of the flocculant,flocculation temperature and whisking speed in optimal clarification and purification method. RESULTS:Among 3 methods,the chitosan flocculation clarification was the best with concentration proportion of 1∶4,chitosan of 1.0 g/L, flocculation temperature at 60 ℃,whisking speed of 100 r/min,whisking time of 4 min,standing time of 12 h. Under the condi-tion of optimal processing,the retention rate of total flavonoids was (85.1 ± 0.75)%,and the removal rate of solid was (24.6 ± 1.33)%(n=5). CONCLUSIONS:Chitosan flocculation can be used to effectively remove the impurity of Perillae folium extract, and optimized clarification and purification technology is stable and feasible.

Purification of Total Flavonoids from Tripterospermi Chinensis Herba by Macroporous Resin / 中国中医药信息杂志

Objective To optimize the purification technology of total flavonoids from the Tripterospermi Chinensis Herba by macroporous resin. Methods The purification abilities of six kinds of macroporous adsorption resins for total flavonoids from Tripterospermi Chinensis Herba were studied with the adsorption and desorption rates as the index by static adsorption and desorption experiments. The column liquid concentration, adsorption rate, and the loaded amount were studied by using dynamic adsorption experiments. The optimal desorption technology was examined by orthogonal experiment. Results AB-8 macroporous resin was found to have good adsorption and desorption effects. The optimal purification conditions were as follows:the column liquid concentration was 5.285 mg/mL, adsorption rate was 2 BV/h;the loaded amount was 17.62 mg/mL. The sample was eluted by 10%ethanol with 4 BV and 50%ethanol of 5 BV at a flow rate of 4 BV/h. The purity of total flavonoids increased to 61.95% after the purification, and the yield was 87.28%. Conclusion This optimized process was stable, feasible and suitable for separation and purification of total flavonoids from Tripterospermi Chinensis Herba.

Study on Purification Technology of Total Alkaloid from the Flos of Aconitum kusnezoffii / 中国药房

OBJECTIVE:To optimize the purification technology of total alkaloid from the flos of Aconitum kusnezoffii. METH-ODS:The content of total alkaloid from the flos of A. kusnezoffii was determined by acid-base titration. The purification technology of total alkaloid from the flos of A. kusnezoffii was optimized by ion resin with resin type,mass concentration of loading liquid and exchange speed as factors,maximum adsorption quantity,desorption rate and mass fraction of total alkaloid as index,and verifica-tion test was conducted. RESULTS:The optimal purification technology was as follows as type 732 cation exchange resin,mass concentration of loading liquid 0.32 g/L,exchange speed of 7 column volume(BV)/h. In validation test,the content of total alka-loid was 86.88%(RSD=0.52%,n=3),and desorption rate was 92.81%(RSD=0.40%,n=3)averagely. The extraction trans-port rate of total alkaloid from 3 batches of the flos of A. kusnezoffii was 81.76% and purification transport rate was 89.47% in av-erage. CONCLUSIONS:The established method is stable and feasible,and shows high transport rate.

Study on Purification Technology of Total Flavonoids from Nelumbinis receptaculum by Macroporous Resin / 中国药房

OBJECTIVE:To study the purification technology of total flavonoids from Nelumbinis receptaculum by macropo-rous resin. METHODS:Using adsorption rate and desorption rate of total flavonoids from Nelumbinis receptaculum as index,the type of macroporous resin was selected by static adsorption-desorption tests;With adsorption rate of total flavonoids as index,sin-gle factor test was used to investigate the effects of the concentration of total flavonoids,adsorption time,adsorption speed, drug-loading amount,water amount,volume fraction and amount of eluant and other factors on the purification technology. The op-timal technology was validated. RESULTS:Among 10 kinds of resin,HPD-400 macroporous resin was found to have the best ad-sorption and desorption effects. The optimal purification conditions was as follows as the concentration of total flavonoids 7.00 mg/ml, adsorption time of 3 h,flow rate for sampling of 3 column volume (BV)/h,drug-loading amount of 8 BV,water amount of 6 BV,50% ethanol elution amount of 4 BV. In validation test,mass fraction of total flavonoids from purified Nelumbinis receptacu-lum were 63.88%,62.50% and 63.44%(RSD=1.11%,n=3). CONCLUSIONS:HPD-400 macroporous resin could purify total flavonoids from purified Nelumbinis receptaculum,and established purification technology is stable and practical.

Purification technology of salidroside by microporous adsorption resin / 中草药

Objective: To optimize the purification technology of salidroside with macroporous adsorption resin. Methods: The absorption and elution conditions of salidroside purificatin by various macroporous adsorption resins were investigated with the content of salidroside as index. Results: SP-825 type macroporous adsorption resin was the best choice for the purification of salidroside. The optimized parameters were as follows: the content of salidroside at 1.713-2.570 g/mL, eluting solvent of 10% aqueous ethanol, volume flow at 2 BV/h, and eluant volume at 30 BV. Conclusion: SP-825 type macroporous adsorption resin could significantly increase the purity of salidroside with the advantage of high absorption, high elution rate, low cost, environment friendly, and being applicable for the production in large scale.

Purification of total flavonoids from diaphragma of Juglans regia by macroporous resin / 中草药

Objective: To investigate the purification technology of total flavonoids from the diaphragma of Juglans regia by macroporous resin. Methods: Twelve macroporous resins were chosn with static and dynamic adsorption and desorption experiments to optimize the purification parameters. Results: AB-8 macroporous resin was found to have good adsorption and desorption effects. The optimal purification conditions were pH value of 4.70, sample mass concentration of 0.713 5 mg/mL, the loaded amount of 4 mL/g, and loading flow rate of 1.5 BV/h. The sample was eluted by water with 2 BV and 50% ethanol of 2.5 BV, respectively. The purity of total flavonoids increased to 72.25% after the purification, and the yield was 93.94%. Conclusion: AB-8 is an ideal resin with the best enrichment for separating and purifying the total flavonoids from diaphragma of J. regia.

Optimization of Purification Technology for Sambucus williamsii Hance. by Macroporous Resin Adsorption Column Chromatography / 世界科学技术-中医药现代化

This study was aimed to optimize the purification technology for Sambucus williamsii Hance. With the morroniside as a marker, the purification technology for Sambucus williamsii Hance was optimized by different types of macroporous resin. The results showed that the optimum purification technology was that, the extract of less than 1:250 (morroniside:resin) was adsorbed and the AB-8 resin was washed with distilled water, and then the morroni-side was eluted from the macroporous resin with 10% ethanol. And the content of the morroniside was more than 50%. It was concluded that the purification technology was simple, reliable, repeatable and suitable for industrial production.