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Objective To screen the macroporous adsorption resin suitable for the separation and purification of total polyphenols from purple tea and establish the purification process parameters to prepare high-purity total polyphenols from purple tea. Methods The static adsorption-elution test was used to screen macroporous adsorption resin for the purification of total polyphenols from purple tea. Based on the single factor test, the comprehensive score of adsorption rate was used as the index to investigate the effects of different factors on the purification process and identify the optimal parameters for the purification process. Those factors included sample concentration, the pH value of the sample solution, the ratio of column diameter to height, sample size, ethanol percentage in the eluent, eluent volume and elution flow rate. Results The best process parameters for purification of total polyphenols from purple tea by AB-8 macroporous adsorption resin were as following. The sample concentration was 375 μg/ml with flow rate 2 ml/min. The sample volume was 3 BV. The sample solution pH was 2. The ratio of colume diameter to height was 1∶6. The impurities were removed first by water 3 BV. 50% ethanol 4 BV was used for elution with flow rate 2 ml/min. Conclusion AB-8 macroporous resin was selected for the purification of polyphenols from purple tea under the optimized technological conditions. The mass fraction of total polyphenols increased from 40.2% to an average of 69.8%. The solid content decreased from 56.0 mg to 29.9 mg. The established purification process has good stability and feasibility. It can be used as a purification process for total polyphenols from purple tea.
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Objective::To compare the adsorption characteristics of different macroporous adsorption resins for the total flavonoids in Epimedii Folium, clarify the adsorption mechanism, and screen the optimal resin for the purification of total flavonoids in Epimedii Folium. Method::Taking the adsorption and desorption capacities of the total flavonoids in Epimedii Folium and five representative flavonoids (epimedin A, epimendin B, epimendin C, icariin, baohuoside Ⅰ) as indexes, static adsorption and dynamic adsorption experiments were conducted to compare the adsorption characteristics of five macroporous including HPD100, HPD600, AB-8, X-5 and D101.The adsorption kinetics of the selected resin was studied by using the pseudo-first-order, pseudo-second-order kinetic models and intraparticle diffusion model, and the thermodynamic process was analyzed by using the Langmuir and Freundlich isothermal adsorption models, which explored the adsorption mechanism of resin from the perspective of physical chemistry. Result::HPD100 macroporous resin had a better adsorption and desorption properties than the others. The adsorption process of HPD100 macroporous resin for total flavonoids in Epimedii Folium and five representative flavonoids conformed to the pseudo-second-order kinetic model. The adsorption thermodynamic process of HPD100 resin for total flavonoids of Epimedii Folium conformed to the Freundlich model, and for the sum of five representative flavonoids conformed to the Langmuir model. The adsorption process of HPD100 resin for total flavonoids in Epimedii Folium was the exothermic process dominated by physical adsorption, and the optimal adsorption temperature was 25 ℃. Conclusion::HPD100 macroporous resin has large adsorption capacity, easy desorption and clear adsorption mechanism, it is suitable for isolation and purification of total flavonoids in Epimedii Folium.
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Objective: To investigate the best technological conditions for the purification of epimedin and icariin from Epimedii Folium by macroporous resin, and preliminarily characterize the purification fraction of the best technological conditions. Methods: Five kinds of macroporous resins were screened by static adsorption experiment with the content of epimedin A1, epimedin A, epimedin B, epimedin C and icariin as indexes. The best purification conditions were optimized by the concentration of upper column solution, the maximum sample volume, the upper column flow rate, the volume of water washing, the concentration of removing impurity ethanol and elution ethanol, the volume of removing impurity ethanol and elution ethanol, the column diameter-height ratio through dynamic adsorption experiment. Finally, UPLC-Q-TOF/MS, HPLC and ultraviolet spectrophotometry were used to characterize the purification fraction of the best technological conditions. Results: The best macroporous resin was AB-8, column diameter-height ratio was 1:7, 6 BV of upper column solution (crude drug 0.5 g/mL) was used for dynamic adsorption at a flow rate of 6 BV/h, 5 BV of water and 5 BV of 20% ethanol were used for impurity removal, and 6 BV of 50% ethanol was used for elution. The flow rate of impurity removal and elution was 6 BV/h. After purification, the total flavonoids content was 63.29%, the total content of epimedin A1, A, B, C and icariin was 40.48%, the content of epimedin A1, epimedin A, epimedin B, epimedin C and icariin was 1.63%, 2.52%, 16.36%, 5.51% and 14.46%, respectively. Conclusion: The purification process of epimedin and icariin from Epimedii Folium by AB-8 macroporous resin is stable, reasonable and feasible. The chemical characterization indicated that the purification fraction was mainly flavonoids, mainly consisting of epimedin and icariin. The optimized purification process can be used for the purification and enrichment of such ingredients.
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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.
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Objective To screen the macroporous adsorption resin suitable for the separation and purification of total flavonoids from Litchi Semen, and the purification process parameters were established to prepare the total flavonoids of Litchi Semen in accordance with the requirements of effective parts of Chinese materia medica, which laid the foundation for the development of the total flavonoids of Litchi Semen into five new Chinese medicines. Methods The macroporous adsorption resin for purifying the total flavonoids of Litchi Semen by static adsorption-elution test was used. Based on the single factor test, the comprehensive score of adsorption rate was used as the index to investigate the volume fraction of ethanol, the mass concentration of the sample, and the sample solution pH, diameter to height ratio, upper column volume, upper column flow rate, eluent concentration, eluent volume and elution flow rate on the purification process, and determine the optimal purification process parameters. Results The best process condition for separating the total flavonoids of Litchi Semen by AB-8 macroporous adsorption resin were as follows: the mass ratio of resin to medicinal material was 3:1, the concentration of the upper column sample solution was 4—6 mg/mL, sample flow rate was 1 mL/min, and the upper column volume was 2 BV, diameter to height ratio was 1∶12, pH of the sample solution was 2, first impurity removal by 20% ethanol 3 BV, and using 60% ethanol 3 BV for elution, elution flow rate was 4 mL/min. Conclusion AB-8 macroporous resin can be used to purify the total flavonoids of Litchi Semen under the established technological conditions. The mass fraction of total flavonoids in Litchi Semen increased from 29.22% to an average of 67.37%, and the solid content decreased from 1.25 g to 0.40 g. It indicates that the established purification process is stable and feasible, and can be used as a purification process condition for total flavonoids of Litchi Semen.
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Objective: To investigate the adsorption kinetics and thermodynamic characteristics of phenylethanoid glycosides (PGs) in the leaves of Callicarpa nudiflora on macroporous resins and provide a reference for the separation and purification of these compounds. Methods: With adsorption and desorption ratio as indexes, optimum types of macroporous resin for purification of PGs were selected from 8 kinds of macroporous resins by static adsorption and desorption tests, and then adsorption kinetics model and adsorption isotherm model of PGs were established to investigate their adsorption processes. Results: SP-825 and SP-207 resin were selected and they have similar adsorption process for PGs. Both of them showed a fast adsorption in 0-60 min, a slow adsorption in 60-360 min, and an equilibrium adsorption stage after 360 min. Adsorption dynamic behavior was well described by quasi-second-order equation of both SP-825 and SP-207 macroporous resins, and adsorption rate was mainly controlled by liquid film diffusion and intraparticle diffusion. Equilibrium adsorption data fitted Langmuir and Freundlich isotherm equations well. Both of the two kinds of resins showed good adsorption properties for PGs, and the adsorption process belongs to favorable adsorption. Conclusions: Both of the kinetic model and thermodynamic model can well describe the adsorption process of SP-825 and SP-207 macroporous resins and the two resins were regarded as excellent adsorption resins for the purification of PGs from the leaves of Callicarpa nudiflora.
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OBJECTIVE: To investigate the separation and purification technology of total saponins from the root of Thladiantha dubia (TSTR). METHODS: The content of TSTR was determined by UV-visible spectrophotometry. By comparing static adsorption and desorption properties of different types (AB-8, D101, DM130, HPD100, HPD300, HPD450, HPD600, HPD826, NKA-9) of macroporous adsorption resin, the type of macroporous adsorption resin was screened. With the content of TSTR as the index, influential factors of macroporous adsorption resin for adsorbing (ratio of height to diameter of resin, mass concentration of medicine liquid, adsorption volume flow, saturated extent of adsorption) and desorbing (desorption solvent volume fraction, desorption solvent volume flow, volume of desorbed solvent) TSTR were investigated. The optimal technology was screened. The technology validation, purification and preparation were conducted. RESULTS: HPD100 type macroporous adsorption resin had good adsorption and desorption properties for TSTR. The optimal adsorption technology was that the ratio of the height to diameter of the resin column was 1:5; mass concentration of medicine liquid was 1 g/mL; adsorption volume flow rate was 1 BV/h; saturated adsorption capacity was 1. 25 g per 1 g HPD100 resin; the optimal desorption technology was that the volume fraction of desorption solvent ethanol was 75％; volume flow rate of desorption was 3 BV/h; the volume of desorption solvent was 5 BV. The average desorption retention rate of TSTR was 77. 96％ in technology validation (RSD=0. 46％, n=3) and the purity of prepared TSTR in TSTR dry cream was 52. 47％ (RSD =1. 53％, n=3). CONCLUSIONS: The optimal purification technology is stable, feasible and suitable for the separation and purification of TSTR.
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Objective To study the separation and purification of total flavonoids from Polygonum hydropiper Linn. by macroporous adsorption resin; To investigate the effects of various factors in the process of static and dynamic adsorption on effects of adsorption and desorption to determine the optimum capability. Methods The total flavonoids from Polygonum hydropiper Linn. was extracted; the contents of flavonoids of ethyl acetate part (FEA) and flavonoids of n-butanol part (FNB) were detected; the adsorption experiment of FEA and FNB was conducted by macroporous adsorption resin. D101, AB-8, DM130, and XDA-8 macroporous resin were used to optimize the separation and purification process. Results The XDA-8 macroporous resin was selected to enrich total flavonoids from Polygonum hydropiper Linn. The optimum process was: adjusting the pH value of FEA flavonoids to 6, the concentration of sample was 750 g/mL, eluting with 75% ethanol to elute 5 bed volumes at a flow rate of 1 bed per hour; adjusting the pH value of FNB flavonoids to 6, the concentration of sample was 1 mg/mL, eluting with 60% ethanol to elute 5 bed volumes at a flow rate of 1 bed per hour. Conclusion XDA-8 macroporous adsorption resin is helpful to separate and purify the total flavonoids of Polygonum hydropiper Linn.by the best process.
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Objective: To optimize the purification technology of total flavonoids from Astragali Companati Semen (ACS) by macroporous adsorption resin. Methods: The process parameters of water decoction extraction of ACS and purification of total flavonoids extracted from ACS by D-101 macroporous adsorption resin were optimized by orthogonal experiment design method. Results: The optimal extraction process were as follows: water decoction extract for three times, each time 0.5 h, water addition of 10, 6, and 6 times amount of the medicine respectively. The optimized technology conditions of D-101 macroporous adsorption resin were as follows: The flavonoids concentration of sample liquid of ACS was about 1.0 mg/mL, the diameter ratio was 1∶5, the sample flow rate was 1 BV/h, the rate of sample weight was 0.6 g/mL (herbs/resin); The velocity of water elution was 1 BV/h and its elution volume was 4 BV; The elution concentration, elution velocity, and elution volume were 70%, 1 BV/h, and 5 BV, respectively. The content paste rate of made ACS of total flavonoids was 2.65%, the mass fraction of total flavonoids was 56.24%, and the process transfer rate was 68.37%. Conclusion: The method is simple and feasible for purification of total flavonoids extracted from ACS.
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Objective: To evaluate the optimal separation and purification processes of water extract, the analytic techniques of particle size analysis, powder fluidity testing, and scanning electronic microscope were adopted to compare the influence factor of different separation and purification techniques on microscopic preparation characteristic of intermediate product prepared from water extract of traditional Chinese medicine (TCM) formula purification. Methods: Taking Gubi Granules (GG) which have established the production technology and quality standards in the previous study as an example, three common techniques used for water extract of TCM formula purification, including ethanol precipitation, column chromatogram of macroporous resin, and membrane separation, were applied to preparing the intermediate of GG. Results: Through the comprehensive analysis of fluidity, adhesive property, compressibility, permeability, particle microstructure and particle size distribution, it was found that membrane separation could obtain intermediates with better performance, which was conducive to the subsequent granulation, tabletting, and other process smoothly. The operating conditions for liquid concentration were 0.05 g crude drug/mL, 30 ℃ liquid temperature, 0.15 MPa pressure and 5 m/s flow rate. Conclusion: The different spray dried powders varied greatly. The membrane separation method of 0.2 μm Al2O3 ceramic was selected as the optimal process for separating and purifying of water extract of GG by analyzing the influencing factors of the pharmaceutical properties.
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Objective To optimize purification technology of total lignans in Myristicae Semen; To study its anti-inflammatory effects. Methods Macroporous adsorption resin was used for enrichment and purification of total lignans in Myristicae Semen, with adsorption rate, desorption rate and content of total lignans as indexes. The resin type, concentration of eluent, sample weight and dosage of eluen were investigated. Anti-inflammatory effects were studied by determining swelling degree and inhibition rate of mice with ear swelling induced by xylene. Results Purification technology of total lignans was processed on type of AB-8 resin. 1 g crude extract was dissolved as sample; 40 mL preprocessed resin including 16 g resin was added and static adsorpted for 12 hours; 30% ethanol was used firstly to elute to colorless and then 300 mL 70% ethanol was used to elute; the eluent of 70% ethanol was collected. The purity of total lignans was 45.8%. There was statistical significance in ear swelling degree of total lignans in Myristicae Semen high-, medium-, and low-dosage groups compared with model group (P<0.05). Conclusion The purification technology of total lignans is stable and reproducible, and total lignans in Myristicae Semen has significant anti-inflammatory activity.
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Objective: To establish the methods for extraction and isolation of punicalagin from pomegranate peel, and further study the purification and quantification of punicalagin. Methods: Using an ultrasonic-assisted extraction method, punicalagin in pomegranate peel was extracted at room temperature by 50% ethanol with 20-fold volume of raw material. The content of punicalagin in the crude extract was determined by HPLC. To optimize the purification process of punicalagin, static adsorption and desorption experi-ments were employed to study five kinds of macroporous adsorbent resins (D101, A8-8, NKA-9, HPD-100 and HPD-500) for the one with the highest purification efficacy of punicalagin. In addition, the technical parameters of the macroporous adsorbent resin were opti-mized to obtain punicalagin with higher purity. Punicalagin was further separated and purified by using a reverse phase MCI GEL CHP20P column. Results:HPD500 resin showed the best ability to absorb and separate punicalagin in among five kinds of macro-porous adsorbent resins. The best technical parameters were as follows:the mass concentration of sample solution was 15 mg·ml-1 , the loading amount was 2BV, the pH was 2 and the eluting solvent was 8BV of 30% ethanol. With the best process as described a-bove, the content of punicalagin extracted from pomegranate peel increased from 10. 3% to 30. 7%. The obtained punicalagin could be further purified to 61. 3% from 30% in ethanol eluate by the reverse phase MCI GEL CHP20P column. Conclusion:HPD500 resin is the most effective in the purification of punicalagin from pomegranate peel, and the content of punicalagin can be dramatically increased after the purification by a reverse phase MCI GEL CHP20P column. The optimized process shows good reproducibility and stability.
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Objective: Through the grey correlation analysis technology and the effect of Caco-2 colon cancer cell proliferation to evaluate the optimization of purification process in total flavonoids of Schizonepetae Herba by macroporous adsorption resin. Methods: By static adsorption and desorption rate of total flavonoids as examining indexes to screen the ratios of macroporous adsorption resin, using single factor experiment to optimize its purification process conditions of total flavonoids; The Caco-2 cell inhibition rate was determined by MTT method; At the same time, using the grey correlation degree analysis technology, the correlation between the purity of total flavonoids and proliferation inhibition rate of the tumor cell was calculated. Results: HPD-400 macroporous adsorption resin has the good adsorption separation performance of the total flavonoids from Schizonepetae Herba, Schizonepetae Herba at the concentration of 0.1 g/mL, 0.8 g/mL (medicine/wet resin) on the amount of column, using 2 BV water to remove impurity, eluting by 9 BV 70% ethanol and all of the flow rate are 4 BV/h, collecting the eluent and dry it; With the same method to do the secondary purification, the purity of total flavonoids is 92.15%, the inhibitory rate of Caco-2 cell proliferation is 86.17%, the greycorrelation coefficient of flavonoids purity and inhibition is 0.9502. Conclusion: This optimization process and the conditions are feasible and stable, the inhibitory efficacy of the in vitro Caco-2 cells is clearly. It lays the foundation of the new anti-cancer drugs based on the purification of total flavonoids in Schizonepetae Herba.
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Objective: To optimize the purification process of total coumarin from Fraxini Cortex using macroporous resin. Methods: The single factor methods have been used to investigate the choice of type, adsorption performance, and desorption performance and the purification of the total coumarin from Fraxini Cortex by macroporous resin. The adsorption rate, resolution, resolution rate, and transfer rate of the total coumarin from Fraxini Cortex, four kinds of coumarin constituents, such as aesculin, aesculetin, fraxin, and fraxetin were used as examining indexes. Results: The ADS-5 was the most suitable type for the purification of total coumarin from Fraxini Cortex among the seven kinds of macroporous resin. Adsorption parameters: Crude drug-the resin was 0.8 g/g which was the sample amount; The concentration of sample solution was 0.75 g crude drug/mL; The pH value of sample liquid was 4.0-4.3 (liquid sample); The speed of the sample through the resin column was 2-4 BV/h. Elution parameters: The volume of the water cleaning fluid impurities was 1 BV; The elution solvent was 25% ethanol; The elution speed was 2 BV/h; The elution volume was 3 BV. After the purification, the transfer rate of total coumarin from Fraxini Cortex was 74.27%, the transfer rate of four kinds of coumarin was 83.06%, the extract rate of total coumarin was 7.35%, the removal of impurities was 14.00%, among which the content of total coumarin was 54.72%, the contents of the four kinds of components were 36.01%, the total coumarin extraction yield was 4.02%. Conclusion: This method to purify the total coumarin from Fraxini Cortex using ADS-5 can get better purification effect, the purification process is also stable.
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Objective To optimize purification technology of total flavonoids in Callicarpa nudiflora Hook. et Arm. by macroporous adsorption resin. Methods Macroporous resin models including AB-8, D-101, HP-20, HP2MG, were optimized by static adsorption and desorption experiments regarding to adsorption rate and desorption rate of total flavonoids. Purification technology parameters of total flavonoids were optimized by single factor test. Results HP-20 macroporous resin presented the best purification efficiency,the optimum purification conditions were that taking 4. 46 mg·mL-1 of total flavonoidsat pH 3. 0, loading at 3 BV·h-1, washed with 3BV of water at 3 BV·h-1,then eluted with 4 BV 75% ethanol at 2 BV·h-1, finally obtaining the total flavonoids from the dry extract of Callicarpa nudiflora Hook. et Arn. with the purity of 47. 4%. Conclusion HP-20 macroporous resin is suitable for preliminary purification of total flavonoids in Callicarpa nudiflora Hook. et Arn.
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OBJECTIVE:To optimize the isolation and purification technology of active components of Senecio cannabifolius with macroporous adsorption resin. METHODS:The type of macroporous adsorption resin was selected with static adsorption using adsorption capacity and resolution rate of chlorogenic acid and hyperoside as index. The isolation and purification condition was op-timized with dynamic adsorption using the elution volume of chlorogenic acid and hyperoside as index,such as maximal sample size,rinse water quantity,volume fraction and collective volume of eluant ethanol. RESULTS:Among 7 kinds of resin,HPD100 had the best purification property;the optimal purification technology was as follows as mass concentration of sample 6 mg/ml,the speed of sample loading 2 ml/min,maximal sample size 3 times of column volume(BV), rinse water quantity of 2.5 BV,60%ethanol as eluting reagent. The contents of chlorogenic acid and hyperoside were increased from 0.90,0.18 mg/g to 7.26,1.04 mg/g after purification. RSD of each index were all ≤3.0%(n=3) in validation test. CONCLUSIONS:The isolation and purification technology of active components of S. cannabifolius with HPD100 macroporous adsorption resin is stable and effective.
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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.
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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.
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Objective: To optimize the technological parameters of separation and purification of cynarin from Cynara scolymus leaves. Methods: Seven different types of macroporous adsorption resins were evaluated on absorptive capacity, desorption rate, and adsorption rate in order to select the best resin and the conditions of the best resin to separate and purify cynarin were researched. Results: It was found that LSA-21 resin showed better comprehensive adsorption property, flow rate of sample loading was 2 BV/h, 3 BV/h 50% alcohol aqueous and 2 BV/h velocity was used to elute. In this process to obtain the product with purity of 5.63% cynarin, ash content of 0.61%, product yield 5.56%, the product quality could meet the market demand. Conclusion: The LSA-21 macroporous adsorption resin shows better comprehensive adsorption property. It could be used to isolate and purify the cynarin.
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Objective:To obtain the optimal conditions for separating catalpol from leaves of Rehmannia by selecting appropriate macroporous adsorption resins.Methods:The detection indication was the content of catalpol, which was determined by HPLC method. Twelve different kinds of macroporous adsorption resins were studied on the static capacity of adsorption and desorption, and H103 resin was selected for the research of separation and purification.Results:The H103 resin had a good capacity for adsorption and desorption.The best process of purifying catalpol by H103 resin was 1mg/ml concentration, the adsorption rate of 1-2 BV/h,the flow rate of 1-3 BV/h, and 8 BV with 10% alcohol.Conclusion:The method is simple and available, which can simplify the production process and lower costs.