Q-marker prediction of resin ethanol extract of Gegen Qinlian Decoction based on characteristic spectrum and network pharmacology / 中国中药杂志

The resin ethanol extract of Gegen Qinlian Decoction(GGQLD) has been found to significantly alleviate the intestinal toxicity caused by Irinotecan, but further research is needed to establish its overall quality and clinical medication standards. This study aimed to establish an HPLC characteristic fingerprint of the resin ethanol extract of GGQLD, predicted the targets and signaling pathways of its pharmacological effects based on network pharmacology, identified core compounds with pharmacological relevance, and analyzed potential quality markers(Q-markers) of the resin eluate of GGQLD for relieving Irinotecan-induced toxicity. By considering the uniqueness, measurability, and traceability of Q-markers based on the "five principles" of Q-markers and combining them with network pharmacology techniques, the overall efficacy of the resin ethanol extract of GGQLD can be characterized. Preliminary predictions suggested that the four components of puerarin, berberine, baicalin, and baicalein might serve as potential Q-markers for the resin etha-nol extract of GGQLD. This study provides a basis and references for the quality control and clinical mechanism of the resin ethanol extract of GGQLD.

Optimization of Extraction and Purification Process of Total Iridoids and Total Crocins in Gardeniae Fructus / 中国实验方剂学杂志

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.

Optimization of total polyphenol purification from purple tea by macroporous resin / 药学实践杂志

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.

Investigation of Adsorption and Desorption Properties of Total Ginsenosides on Anion-exchange Resins and Its LC-MS Analysis / 中国实验方剂学杂志

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^-1， 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^-1. 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.

Purification and component identification of total proanthocyanidins in Choerospondias axillaris pericarp / 中国中药杂志

The present study determined the quantitative markers of total proanthocyanidins in the purification of the industrial waste Choerospondias axillaris pericarp based on the comparison results of high-performance liquid chromatography(HPLC) and mass spectrometry(MS) and optimized the purification process with two stable procyanidins as markers. The adsorption and desorption of five different macroporous adsorption resins, the static adsorption kinetics curve of NKA-Ⅱ resin, the maximum sample load, and the gradient elution were investigated. The UPLC-Q-TOF-MS/MS was employed for qualitative analysis of the newly-prepared total proanthocyanidins of C. axillaris pericarp. As revealed by the results, NKA-Ⅱ resin displayed strong adsorption and desorption toward total proanthocyanidins. The sample solution(50 mg·mL~(-1)) was prepared from 70% ethanol crude extract of C. axillaris pericarp dissolved in water and 7-fold BV of the sample solution was loaded, followed by static adsorption for 12 h. After 8-fold BV of distilled water and 6-fold BV of 10% ethanol were employed to remove impurities, the solution was eluted with 8-fold BV of 50% ethanol, concentrated, and dried under reduced pressure, and purified total proanthocyanidin powder was therefore obtained. Measured by vanillin-hydrochloric acid method, the purity and transfer rate of total proanthocyanidins were 47.67% and 59.92%, respectively, indicating the feasibi-lity of the optimized process. UPLC-Q-TOF-MS/MS qualitative analysis identified 16 procyanidins in C. axillaris total proanthocyanidins. The optimized purification process is simple in operation and accurate in component identification, and it can be applied to the process investigation of a class of components that are difficult to be separated and purified. It can also provide technical support and research ideas for the comprehensive utilization of industrial waste.

Investigation of Adsorption Properties of Five Macroporous Resins for Total Flavonoids in Epimedii Folium / 中国实验方剂学杂志

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.

LCMS-IT-TOF Analysis of Retention Behavior of Sanguisorbae Radix Components on D101 Macroporous Resin and Polyamide Resin / 中国实验方剂学杂志

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.

Purification process of epimedin and icariin from Epimedii Folium by macroporous resin / 中草药

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.

Review on factors influencing separation and purification of Chinese materia medica components by macroporous adsorption resin / 中草药

In recent years, macroporous adsorption resin has been widely used in the purification and separation of natural medicine and effective components of Chinese materia medica, the purification of compound Chinese medicine preparations, the removal of harmful impurities due to the advantages of stable physical and chemical properties, high selectivity, strong adsorption capacity and easy elution, recyclable use and regeneration treatment, economic and environmental protection, convenient preparation molding and so on. By summarizing the preparation, properties, classification and working principle of macroporous adsorption resin, the influencing factors and purification process of Chinese materia medica components were reviewed. The purpose of this paper is to explore the important factors affecting the purification of Chinese materia medica components by macroporous adsorption resin, and provide reference for improving the purification effect of Chinese materia medica components.

Research progress on macroporous resin application in enriching and separating alkaloids / 中草药

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.

Application and significance of nanofibrous macroporous scaffold preparation technology for bone tissue engineering / 中国组织工程研究

BACKGROUND: Bionic porous scaffolds used in bone tissue engineering requires extracellular matrix-like nanofibrous and connected macroporous structure to effectively support cell implantation, adhesion, proliferation and other behaviors, and promote tissue regeneration. OBJECTIVE: To summarize the research progress in nanorfibrous macroporous scaffold preparation technology for tissue engineering based on the latest relevant research trends. METHODS: The first author searched Web of Science, CNKI and Baidu academic databases to retrieve papers published from 2000 to 2019 with the search terms “bone tissue engineering, nanofibrous, macroporous, scaffolds” in English and Chinese, respectively. Finally, 58 articles were included in result analysis. RESULTS AND CONCLUSION: The scaffolds with nanofibrous structures are fabricated using three strategies, including electrospinning, thermally induced phase separation, and self-assembly process. However, bone scaffold fabricated by a single strategy failed to provide interconnected macropores to simulate the microenvironment in the body, which was necessary for cell migration, growth, differentiation, proliferation, and tissue and organ regeneration. Therefore, it is now of great practical and scientific significance to develop macroporous nanofibrous scaffold using a combination of several strategies. Three-dimensional printing technique can provide precise structure and enables the customization of the internal structure and external shape of the scaffold, which promotes the development of bone tissue engineering technique.

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 .

Development of Macroporous Chitosan Scaffolds for Eyelid Tarsus Tissue Engineering

BACKGROUND: Reconstruction of large eyelid defects remains challenging due to the lack of suitable eyelid tarsus tissue substitutes. We aimed to evaluate a novel bioengineered chitosan scaffold for use as an eyelid tarsus substitute.METHODS: Three-dimensional macroporous chitosan hydrogel scaffold were produced via cryogelation with specific biomechanical properties designed to directly match characteristics of native eyelid tarsus tissue. Scaffolds were characterized by confocal microscopy and tensile mechanical testing. To optimise biocompatibility, human eyelid skin fibroblasts were cultured from biopsy-sized samples of fresh eyelid skin. Immunological and gene expression analysis including specific fibroblast-specific markers were used to determine the rate of fibroblast de-differentiation in vitro and characterize cells cultured. Eyelid skin fibroblasts were then cultured over the chitosan scaffolds and the resultant adhesion and growth of cells were characterized using immunocytochemical staining.RESULTS: The chitosan scaffolds were shown to support the attachment and proliferation of NIH 3T3 mouse fibroblasts and human orbital skin fibroblasts in vitro. Our novel bioengineered chitosan scaffold has demonstrated biomechanical compatibility and has the ability to support human eyelid skin fibroblast growth and proliferation.CONCLUSIONS: This bioengineered tissue has the potential to be used as a tarsus substitute during eyelid reconstruction, offering the opportunity to pre-seed the patient's own cells and represents a truly personalised approach to tissue engineering.

Process optimization for extraction and purification of polysaccharides from Cistanche deserticola / 中国中药杂志

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.

Optimization of Purification Process of Total Alkaloid Extract of Berberis dictyophylla Cortex by Macroporous Resin and Investigation of Its Quality Standard / 中国实验方剂学杂志

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.

Recovery and Utilization of Alkaloids in Processing Wastewater of Aconiti Radix / 中国实验方剂学杂志

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.

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.

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.

Preparation of morinda officinalis iridoid glycosides and the inhibitory effect on bone resorption of osteoclasts / 第二军医大学学报

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.

Optimization of the extraction and enrichment process and evatuation of the free radical scavenging activity of triterpene sapogenins from Pfaffia glomerata / 国际药学研究杂志

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.