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ObjectiveTo optimize the extraction and purification process of Gardeniae Fructus for industrial production， and to obtain the total iridoid and total crocin extracts. MethodOrthogonal test was used to optimize the water extraction process by taking contents of geniposide， genipin gentiobioside， gardenoside， crocin-1 and crocin-2 as indicators and the decocting time， decocting times and water amount as factors. The purification process was optimized by single factor test， and four different types of macroporous adsorption resins were screened. The process conditions such as resin type， maximum loading amount， water washing amount， ethanol concentration， ethanol dosage， and flow rate of sample loading were mainly investigated. In addition， the drying methods （vacuum drying and spray drying） of the extract were investigated， and a pilot scale-up verification test was carried out. ResultThe optimal water extraction process of Gardeniae Fructus was to add 15， 10 times the amount of water for decocting twice， 1 h each time. The optimal purification process was as follows：the water extract through SP825L macroporous resin column， the amount of crude drug-the amount of resin （1∶1.5）， the sample loading flow rate of 3 BV h-1， adding 2 BV of water to remove impurities， adding 4 BV of 30% ethanol to obtain the iridoid part， then adding 3 BV of 70% ethanol to obtain the crocin part， collecting the ethanol lotion， and drying at 70 ℃. Under these conditions， the extraction amount of total iridoids was 590.75 mg·g-1 with the transfer rate of 70.48%， and the yield of dry extract was 8.89%. The extraction amount of total crocins was 83.37 mg·g-1 with the transfer rate of 22.20%， and the dry extract yield was 2.60%. ConclusionThe optimized extraction and purification process is stable and feasible with high extraction rate of active components， which is suitable for the industrial extraction and purification of active parts of Gardeniae Fructus.
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Objective:To compare the adsorption and desorption properties of different anion exchange resins for total ginsenosides， clarify their adsorption/desorption mechanism， and establish a simple protocol for the purification of total ginsenosides. Method:The adsorption and desorption properties of five different resins （D301， D315， D312， D330， D201） on total ginsenosides were evaluated with specific adsorption capacity， specific desorption capacity， desorption rate and recovery rate as indices. The adsorption kinetics and thermodynamics of the selected resin and D101 macroporous resin were investigated by pseudo-first-order and pseudo-second-order kinetic models， as well as Langmuir and Freundlich isothermal adsorption models， and the differences of adsorption mechanism between anion exchange resin and conventional macroporous resin were elucidated. The dynamic adsorption and desorption experiments were used to determine the optimum chromatographic parameters for anion exchange resin. After verifying the purification process of total ginsenosides， nine individual ginsenosides were qualitatively and quantitatively analyzed by liquid chromatography-mass spectrometry （LC-MS）. Result:D301 anion exchange resin was obviously superior to the other four kinds of anion exchange resin， the optimum parameters were set as follows：pH 8 of loading solution， loading volume of 2 BV， loading speed of 4 BV·h<sup>-1</sup>， eluted with 3 BV of water and 20% ethanol for the impurities， eluted with 8 BV of 80% ethanol with elution speed of 4 BV·h<sup>-1</sup>. After purified by D301 resin， the enrichment coefficients of 9 monomer ginsenosides were simultaneously increased to different degrees， the overall enrichment coefficient was up to 5.3， the recovery rate for the total amount of these ginsenosides was calculated to be 80.9%， and the purity of total ginsenosides in Ginseng Radix et Rhizoma extract increased from 17.07% to 91.19%. Conclusion:D301 anion exchange resin is suitable for rapid and practical purification of total ginsenosides， hence allowing for the enrichment of high-purity total ginsenosides from Ginseng Radix et Rhizoma via one-dimensional column chromatography.
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Alkaloids is one of the most extensive natural products and one of the most important effective constituents of Chinese materia medica (CMM), most of which have complex ring structure and the effect of antidiabetics, antitumor, antibacterial, antiviral and so on. Macroporous resin is a kind of high-molecular polymer, which cannot be dissolved in acid, alkali and a variety of organic solvents, with the feature of fast adsorption and mild desorption condition, easy regeneration, and long service cycle, etc. In recent years, macroporous resin has been widely applied to the separation and purification of alkaloids and flavonoids. However, there are so many different kinds and variable quality of macroporous resin in the market, as well as multifarious factors influencing the purification effect, the experimental research has been severely affected. In this paper, the application of macroporous resin on separating and enriching alkaloids in recent years had been studied to summarize the main factors affecting the purification effect. The characteristics as well as the problems of macroporous resin were also analyzed. By studying the pretreatment and regeneration process of macroporous resin and optimizing process parameters, the adsorption and desorption performance can be strengthened and the yield or recovery rate of target alkaloids could be enhanced, promoting the further use of macroporous resin in separating and enriching alkaloids from CMM.
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Objective:To study on the material basis of Sanguisorbae Radix by column chromatography and liquid chromatography-ion trap-time-of-flight mass spectrometry (LCMS-IT-TOF), and analyze the distribution of different components in Sanguisorbae Radix water extract on D101 macroporous resin and polyamide resin. Method:Sanguisorbae Radix water extract was separated by D101 macroporous resin and polyamide resin, and LCMS-IT-TOF was used for detection, chromatography separation was achieved on an ACQUITY UPLC HSS T3 column (2.1 mm×100 mm, 1.8 μm) with the mobile phase consisted of water (A) and acetonitrile (B) for gradient elution (0-10 min, 5%-20%B; 10-18 min, 20%-35%B; 18-23 min, 35%-50%B; 23-28 min, 50%-90%B; 28-30 min, 90%B; 30-33 min, 90%-5%B; 33-35 min, 5%B), the flow rate was 0.3 mL·min-1, the column temperature was 30 ℃. Data acquisition was carried out in electrospray ionization (ESI) under the positive and negative ion modes, the scanning range was m/z 100-1 200. According to mass spectrometry data such as accurate molecular mass and fragment information, combined with literature, different chemical components in loading effluents and ethanol eluents of Sanguisorbae Radix water extract were identified. A heat map of the distribution of components in each fraction was drawn by extracting mass spectrum peak intensity data of each sample. The elution rules of various components were compared visually. Result:The enrichment and separation of D101 macroporous resin and polyamide resin were obvious. Tannins in Sanguisorbae Radix water extract was mainly concentrated in loading effluent of macroporous resin and its water eluent, triterpenoids were mainly distributed in the 90% ethanol eluent of macroporous resin. In the above effluents and eluents, a total of 63 compounds (including isomers) were identified. Among them, 6 compounds, ellagic acid-4-pyranoarabinoside or its isomer, 6-O-galloylnorbergerin, 3-O-galloylnorbergerin, (6-acetyloxy-5,7-dihydroxy-8-methoxy-4-oxochromen-2-yl) acetate, ethyl 2-methyl-5,6-bis (sulfooxy) benzofuran-3- carboxylate were first discovered in Sanguisorbae Radix. Conclusion:The method can quickly and accurately identify the distribution of components in aqueous extract of Sanguisorbae Radix after column chromatography, providing experimental basis for exploring the pharmacodynamic components and mechanism of Sanguisorbae Radix.
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Objective To study the preparation method of Morinda officinalis iridoid glycosides (MOIG) and to explore the inhibitory effect on bone resorption of osteoclasts. Methods High-performance liquid chromatography (HPLC) was applied to determine the contents of monotropein and deacetyl asperulosidic acid from MOIG. The static adsorption-desorption test was used to screen the types of macroporous resins of AB-8, ADS-17, D101, HPD400, HPD600, HP20, S-8, SP850, XDA-1 and XDA-6, and to optimize the related parameters in process of enriching MOIG using macroporous resins. Furthermore, the osteoclasts induced from mouse bone marrow monocytes were used to evaluate the inhibitory effects of MOIG on osteoclastic bone resorption. Results After optimization, XDA-1 macroporous resin had better adsorption and desorption effects on MOIG. The optimized preparation conditions were as follows: mass concentration of MOIG in the sample solutions was 19.15 mg/mL, pH value was 1.0, diameter-height ratio of resin column was 17, flow rate of loading samples was 2.0 BV/h (1 BV＝80 mL), loading volume was 0.75 BV, and adsorption time was 11 h. 7 BV water was used to remove other constituents, and 10% ethanol was used to elute MOIG in the flow rate of 3.0 BV/h. The total content of monotropein and deacetyl asperulosidic acid in the prepared MOIG was more than 54%. MOIG had no significant effect on proliferation of the osteoclasts induced by mouse bone marrow monocytes, while it could significantly inhibit the tartrate-resistant acid phosphatase activity and the bone resorption of osteoclasts (P0.05, P0.01). Conclusion XDA-1 macroporous resin can be used to enrich MOIG, with more than 54% total content of monotropein and deacetyl asperulosidic acid. The MOIG can significantly inhibit the bone resorption of osteoclasts.
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Objective: To investigate the adsorption performance and purification effect of macroporous adsorption resin on total polyphenols in Acanthopanan trifoliates leaves, and to determine the technological conditions for the purification of total polyphenols from A. trifoliates leaves. Methods: The Folin-Ciocalteu colorimetric method was used to quantify the adsorption and desorption effects of five macroporous adsorption resins on the total polyphenols in the A. trifoliates leaves. The resin suitable for separation and purification of total polyphenols in A. trifoliates leaves was screened, and the adsorption and desorption conditions were investigated and optimized. The final optimized parameters were determined by single factor experiments. Results: The best purification parameters of total polyphenols were determined as follows: the concentration of sample solution was 1.0 mg/mL (crude drug) with pH 3.0, sample flow rate was at 2 mL/min, and the sample loading was controlled to 30 mL, the elution was 50% ethanol at a flow rate of 2.0 mL/min with pH 6.0, and the elution amount was 40 mL. The polyphenol sample of the A. trifoliates leaves was purified by HPD100 resin, and the purity increased from 11.7% to 49.7%, and the purification effect was 4.25 times than before. After 30 times enlargement experiment, the purity of the A. trifoliates leaves polyphenol sample increased from 12.5% before purification to 54.5%, and the purification effect was 4.4 times than before. The amount of macroporous resin did not affect the purification efficiency, which provided reference for HPD100 macroporous resin for industrial production of total polyphenols purification of A. trifoliates leaves. Conclusion: HPD100 is the best resin for purifying total polyphenols from A. trifoliates leaves, and the process technology result in this experiment can be applied to industrial production.
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Objective: To extract and purify total flavonoids from Periploca forrestii Schltr.(P. forrestii),and test the in vitro inhibitory activity of the total flavonoids and two flvaonoidal compounds in P. forrestii,so as to provide a reference for studies on the related medicinal substances in P. forrestii. Methods: Total flavonoids were extracted from P. forrestii and then purified by the column chromatography on macroporous resin and polyamide columns. The content of total flavonoids was determined according to the Lambert-Beer’s law. The in vitro xanthine oxidase(XOD)inhibitory ac- tivity was assayed for total flavonoids and the two flavonoidal compounds by the ultraviolet spectrophotometry. Results The purified total flavonoids had a content of more than 95%. The total flavonoids and two flavonoidal compounds all showed an inhibitory effect on XOD in vitro,with the inhibitory rate enhanced with increasing concentration. The IC50 of the total flavonoids as well as the two flavonoidal compounds,quercetin-3-O-α-L-pyranoside(QP)and quercetin-7-O-β- D-glucopyranoside(QG)were 608.9,221.2 and 261.2 μg/ml,respectively. Conclusion: The total flavonoids as well as the two flvaonoidal compounds QP and QG in P. forrestii all showed the in vitro inhibitory activity on XOD.
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Objective: To establish a macroporous resin enrichment process for total triterpene sapogenins from Pfaffia glomerata,and evaluate the free radical scavenging activity of the total triterpene sapogenins. Methods: The transfer rate of triterpene sapogenins was used as the index. Static adsorption-desorption method was used to select the best macroporous resin,dynamic adsorption-desorption method was used to determine the enrichment process parame- ters,and orthogonal test was used to optimize the enrichment process. The 1,1- diphenyl- 2- trinitrophenylhydrazine (DPPH)and hydroxyl free radical scavenging tests were used to evaluate the free radical scavenging capacity of the triter- pene sapogenins. Results: The AB-8 type macroporous resin had the best enrichment effect on the triterpene sapoge-nins. The conditions for the optimum enrichment process were as follows:the concentration of triterpene sapogenins in the sample solution for resin column chromatography was 3.5 mg/ml,the ratio of diameter to height for the bed of resin column was 1:7,the amount of the raw herbs subjected to the resin column was 0.11 g/ml(herbs/resin),the flow rate for subjecting sample solution to resin column was 1 BV/h,the eluent was 95% aqueous ethanol,the eluting flow rate was 2BV/h,and the eluent volume for elution was 7 BV. After optimization,total triterpene sapogenins reached 65% in the samples prepared by the optimized process,and the transfer rate of total triterpene sapogenins reached 80.23% in the pre- paring process. The total triterpene sapogenin sample could scavenge the DPPH and hydroxyl free radicals,and the scav- enging rate for the DPPH and hydroxyl radicals reached 82.42% and 73.43% at the 1.0 mg/ml,respectively. Conclusion: The AB- 8 macroporous resin can be used for the enrichment and purification of triterpene sapogenins from P. glomerata. The optimized enrichment process was stable and feasible,and the obtained triterpene sapogenins showed a good free radical scavenging activity.
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Objective: To optimize the recovery technology for 6 kinds of toxic alkaloids in the toxic wastewater from processing of Aconiti Radix with macroporous resin. Method:With the rates of adsorption and elution of benzoylmesaconine,benzoylaconine,benzoylhypaconine,mesaconitine,hypaconitine and aconitine as indexes,static and dynamic adsorption-elution tests were used to select the best one from 15 kinds of macroporous resin,and the recovery technology parameters of six toxic alkaloids in the wastewater from processing of Aconiti Radix were optimized. Result:D101 macroporous resin had a good adsorption and elution effect on 6 kinds of toxic alkaloids in the wastewater from processing of Aconiti Radix,its optimum technology conditions were as follows:each gram of macroporous resin could be used to treat processing wastewater from 4.3 g of Aconiti Radix,the sample loading speed was not higher than 3.0 mL·min-1,the resin column was eluted with 6 BV of 70% ethanol after removing impurities with 2 BV of water.The recoveries of benzoylmesaconine,benzoylaconine,benzoylhypaconine,mesaconitine, hypaconitine and aconitine were 98.03%,94.09%,96.53%,78.15%,85.40% and 70.57%,respectively. Conclusion:D101 macroporous resin can be used for detoxification treatment of processing wastewater of Aconiti Radix,at the same time,6 kinds of alkaloids are effectively recovered,which can solve the environmental problems and create certain economic benefits,and the optimized process conditions are stable and feasible.
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Objective: To optimize purification process of total alkaloid extract of Berberis dictyophylla cortex by macroporous resin,and to establish its quality standard. Method: Acid dye colorimetry was used to investigate the purification process of total alkaloid extract of B. dictyophylla cortex,the process parameters included concentration of sample solution,speed of sampling,diameter-height ratio of resin column,water washing amount,concentration and dosage of eluent,flow rate of elution,etc.In order to determine the optimum process,HPLC was employed to determine the contents of four alkaloids(magnoflorine,jatrorrhizine hydrochloride,palmatine hydrochloride,and berberine hydrochloride) with mobile phase of acetonitrile-0.1% phosphoric acid aqueous solution for gradient elution and detection wavelength at 270 nm.After being purified,quality standard of total alkaloid extract of B. dictyophylla cortex was investigated according to the requirements in the 2015 edition of Chinese Pharmacopoeia. Result: Optimal purification conditions were as following:10 g of HPD100 macroporous adsorption resin with a column diameter-height ratio of 1:8,sampling solution concentration of 11 g·L-1,the loading flow rate of 1 mL·min-1,sampling solution volume of 50 mL,washed with 4 BV of water(1 BV=15 mL) and added 9 BV of 30% ethanol,after being purified,the transfer rate of total alkaloids was>80%,and its purity was>65%.The quality standard of total alkaloid extract of B. dictyophylla cortex was established,there were 19 common peaks in the characteristic chromatogram,and the overall similarity was>0.99. Conclusion: This optimized purification process is stable and feasible, and the established quality standard is controllable.
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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.
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In this study, taking Cistanche deserticola in Xinjiang as the experimental material, the optimal process for extracting polysaccharides from C. deserticola with water extraction was studied by using single factor and orthogonal experiment. Its effects on protein removal and polysaccharides retaining were investigated by using Sevag, enzymatic method or combination of these two methods, so as to determine the optimal method for protein removal from polysaccharides of C. deserticola; the decolorization and purification methods such as macroporous resin of AB-8 and activated Carbon were used to determine the optimal process. The results showed that the extraction rate of polysaccharides from C. deserticola was 18.40% during the optimal process of the water extraction as follows: extraction temperature 75 ℃, extraction time 165 min and solid-liquid ratio 1∶55. The protein removal rate can reach 31.40% and polysaccharide retention rate can reach 96.00% under the optimal protein removal process: temperature 50 ℃, time 2 h, and papain dosage 0.2%. The decolorization rate of activated Carbon and macroporous resin called AB-8 was 80.37% and 86.43%, and the recovery rate of polysaccharides was 77.05% and 91.93%, respectively, suggesting that macroporous resin was more suitable for decoloration. Macroporous resin named AB-8 increased the purity of the polysaccharide crude extract from 67.70% to 84.80% under the following conditions: concentration of the sample 4 g·L~(-1), concentration of the eluent 60% ethanol, and the flow rate 1 mL·min~(-1), showing significant purification effect.
Subject(s)
Cistanche , Chemistry , Plant Extracts , Chemistry , Polysaccharides , Temperature , WaterABSTRACT
bjective To optimize the optimal purification technology for total alkaloids from Longzuan Tongbi Recipe (LTR). Methods Five types of macroporous resins were used to adsorb and desorb the total alkaloids in LTR, and the adsorption capacities, adsorption ratios and desorption ratios of total alkaloids were regarded as the indexes to screen out the suitable resin. The purification technology for total alkaloids was optimized from LTR by single factor investigation and central composite design and response surface method. Results The best purification technology of total alkaloid from LTR were determined as follows: the concentration of sample solution of 0.17 g/mL (crude drug) with pH 1.7, sample flow rate at 1 mL/min, washing impurity with 9-column volume of 80% ethanol at a flow rate of 1 mL/min. The mass scores of total alkaloids was 22.23% and the yield of that was 173.27 mg/g. Conclusion HPD100 resin has good purification effect on total alkaloids from LTR, which could provide reference for the further study of pharmacodynamics.
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Objective: To optimize the purification technology of saponins in steamed Panax notoginseng with macroporous resin. Methods: The main factors affecting the purification process were screened by failure mode and effects analysis (FMEA). The purification method with macroporous resin was optimized by central combination design-response surface method (CCD-RSM) based on the recovery and purity of saponins. In this experiment, the concentration of sample solution, loading volume, washing volume, ethanol concentration, and ethanol elution volume were used to investigate the purification of saponins in steamed P. notoginseng. Results: The optimized purification process with macroporous resin was as follows: maximum recovery (82.81%) and purity (77.24%) of saponins were obtained with the concentration of saponin solution of 11.22 mg/mL, loading volume of 4.97 BV, washing volume of 2 BV, ethanol concentration of 70%, and ethanol elution volume of 3.31 BV. Conclusion: The optimized purification process based on FMEA and CCD-RSM is convenient and stable, with high recovery and purity of saponins, which has a certain practical value.
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Objective: To compare the effects of different purification processes on the content of salidroside in the extract of Herba Rhodiola to provide reference for the large-scale production. Methods: Ethanol precipitation, clarifier precipitation and AB-8 macro-porous resin separation was respectively used to purify the extract of Herba Rhodiolae, and HPLC was used to determine the content of salidroside to screen the optimum purification process. Results: After the purification by AB-8 macroporous resin, the content of sali-droside was as high as 0. 272 5 mg·ml-1followed by that by ethanol precipitation (70% alcohol), and the clarifier precipitation lost more salidroside. Conclusion: The purification of salidroside by AB-8 macroporous resin separation is with high yield, good selectivi-ty, promising reproducibility and so on, which is suitable for the large-scale production of salidroside.
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Objective: To explore the optimal extraction process by a blitzkrieg extractor and the adsorption separation by macro-porous resin for chlorogenic acid in Lonicera macranthoides. Methods: The transfer rate of chlorogenic acid was used as the main as-sessment index, the response surface test was adopted to optimize the main influencing factors in the extraction process by a blitzkrieg extractor for chlorogenic acid in Lonicera macranthoides. The transfer rate and the product purity of chlorogenic acid were used as the main assessment indices, the water extract solution of Lonicera macranthoides was used as the raw material, single factor test was adopt-ed to optimize the main influencing factors in the adsorption separation process by a macroporous resin for chlorogenic acid in Lonicera macranthoides. Results: The optimum conditions of the extraction process by a blitzkrieg extractor and the adsorption separation by a macroporous resin for chlorogenic acid in Lonicera macranthoides were as follows: the solid-liquid ratio was 1 : 23, the extraction time was 4. 7 min, the rotating speed was 6 000 r·min-1, the type of macroporous resin was ADS-7, the amount ratio of medicinal materi-als to macroporous resin was 1: 5, the flow rate of sample solution was 1 BV·h-1, the macroporous resin column was eluted by 1 BV water at the speed of 1 BV·h-1followed by 6 BV 20% ethanol solution at the speed of 2 BV·h-1, and the eluent of 20% ethanol so-lution was collected. The average transfer rate of chlorogenic acid was 90. 12% (RSD=1. 33% ) with the purity of 50. 30% (RSD=2. 19% ). Conclusion: A new route of the extraction process by a blitzkrieg extractor and the adsorption separation by a macroporous resin for chlorogenic acid in Lonicera macranthoides has established through the optimization and verification experiments. The process with high transfer rate of chlorogenic acid (the purity of chlorogenic acid product was over 50% ) is fast, and the solvent is healthy and easy to recycle.
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Objective:To explore the macroporous resin adsorption and the membrane separation technologies for the purification of saponins water extract of Anemarrhena asphodeloides. Methods:Ten-fold amount of water was used to extract twice for 120 min each time to extract saponins from Anemarrhena asphodeloides. The macroporous resin adsorption(HP-20,HPD-600,D101,AB-8) and the membrane separation technologies (ceramic microfiltration membranes 0.8 μm and 0.05 μm, and hollow fiber ultrafiltration mem-branes 50,10 and 6 kDa) were adopted to purify the saponins water extract liquid. The physicochemical parameters including electri-cal conductivity,viscosity and turbidity were measured,as well as the contents of total saponins,proteins and polysaccharides were de-termined. Results:The viscosity and turbidity decreased,the value of pH increased and the electrical conductivity of the saponins puri-fication liquid changed irregularly after the membrane filtration. The microfiltration membrane was more advantageous than the ultrafil-tration membrane in removing macromolecular substances. The smaller the pore diameter of microfiltration membrane, the smaller the intercepted molecular weigh,the higher the removal ratio of proteins and the higher the penetration rate of the total saponins,while the polysaccharides content was stable, which was consistent with the results of physicochemical parameters. The ceramic microfiltration membrane could obtain clearer extract,while the ultrafiltration membrane was more suitable for the enrichment of saponins when the in-tercepted molecular weight was 6 kDa. The macroporous resin HPD-600 was the best for the purification of timosaponin water extraction liquid.Conclusion:The selection of membrane for the separation and purification of different substances is particularly important. The change of physicochemical parameters and the content decrease of macromolecular substances have obvious corresponding relationship. Ultrafiltration membrane is better than microfiltration membrane for the purification of timosaponin water extract liquid.
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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.
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Objective To study the optimum technological conditions of macroporous resin separation and purification of polyphenol composition. Methods Fingerprint of Ilex paraguariensis was established by HPLC method. The best resin, loading conditions and elution requirements were screened with chlorogenic acid and elution rate of total active constituents served as the index. Results The optimum technological conditions were as follows:the separation carrier was D101 macroporous resin,the concentration of the sample liquid was 0.10 g?mL-1 ,the resin adsorption quantity of crude drugs was 1.5 g?g-1 ,the impurity was removed by four times of amount of water at first,and then eluted with four times the amount of 70％ ethanol in a gradient manner.After purification,the elution rate of chlorogenic acid was up to 82.83％,and the elution rate of total effective component was about 72. 48％. The resemblance of HPLC fingerprint was over 0. 98, and the components were balancedly recoveried. Conclusion The purification process of total polyphenols in Ilex paraguariensis by D101 macroporous resin was simple,reliable,and can be used for large-scale production.
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Objective:To explore the purification technology parameters for polyphenols from vitis amurensis seed extract with AB-8 macroporous resin and to establish the optimum purification process conditions,and to provide technical reference for further development and utilization of vitis amurensis seeds.Methods:The vitis amurensis seeds were regarded as raw material,the concentration of vitis amurensis seed polyphenols was detected, and the adsorption rate and desorption rate of polyphenols were calculated.The AB-8 macroporous resin was used to purify the polyphenols from vitis amurensis seed extract, and the purification technology parameters of vitis amurensis seed polyphenols were optimized by absorption-desorption experiment.The concentrations of polyphenol from vitis amurensis seed extract were compared between before and after purification, and the effect of the purification process was verified. Results: The AB-8 macroporous resin had good absorption and desorption properties to crude the extract of vitis amurensis seed polyphenols,and the adsorption rate and desorption rate were 90.48% and 71.42%.The optimum adsorption conditions and desorption conditions were as follows:the sample concentration was 10 g· L-1 ,the sample flow rate was 3 mL· min-1 ,the eluting concentration was 60%,the elution velocity was 2 mL·min-1 ,and the eluting volume was 2-fold column volume.Under this condition,the concentration of polyphenols from vitis amurensis seed extract after purification was increased from 35.02% to 88.8%.Conclusion:AB-8 macroporous resin has better purification effect,and it is worthy of popularization and application.