大孔树脂吸附法富集保和丸中橙皮苷的工艺研究

目的 :研究大孔树脂吸附法富集保和丸中有效成分的工艺条件及参数。方法 :以保和丸中主要药味陈皮中的主要成分橙皮苷富集程度为考察指标 ,考察大孔树脂富集保和丸有效成分的最佳工艺条件。结果 :保和丸提取液 (5 0 0mg/ml) 5mL上大孔树脂柱 (R15mm×H10 0mm) ,吸附 30min后 ,先用 10 0mL蒸馏水洗脱除去杂质 ,然后 ,采用 10 0mL 5 0 %乙醇洗脱橙皮苷为最佳工艺。结论 :通过大孔树脂富集橙皮苷洗脱率在 95 %以上 ,5 0 %乙醇洗脱液干燥后总固物约为处方量的 4%。

大孔吸附树脂在药用植物有效成分分离中的应用

对大孔吸附树脂的性能、分离原理、吸附作用的影响因素、树脂的预处理和再生方法进行了评述。

氨基酸修饰大孔吸附树脂NK-110对肿瘤坏死因子吸附性能的研究

应用医用吸附剂直接吸附血浆中的TNFα是一种高效的分离方法。选用 8种不同结构和性质的氨基酸修饰大孔吸附树脂NK 110 ,通过对TNFα吸附量的测定 ,吸附动力学曲线和吸附等温线的描述等方法 ,研究了经修饰后大孔吸附树脂对血浆中TNFα的吸附性能 ,结果表明 :1.半胱氨酸修饰的NK 110对TNFα的吸附量高 ,静态吸附12 0min时达 76 83 80u mL。 2 .其吸附动力学曲线表明 ,经半胱氨酸修饰后 ,相同时间内吸附量更高 ,且二者吸附量有差别 (P <0 0 1)。 3.由吸附等温线可见NK 110对血浆中TNFα的吸附量随着溶液浓度的升高而升高 ,但其吸附率随之呈降低趋势。经半胱氨酸修饰后 ,其吸附量随着TNFα浓度的升高而升高 ,吸附率基本不变。

功能基团密度对离子交换过程的影响 Ⅰ.水解程度对羧酸树脂吸附庆大霉素的影响

以丙烯酸甲酯与二乙烯基苯为单体，悬浮共聚合成了大孔白球，通过改变树脂上酯基水解反应时间，合成了一系列不同功能基团密度的树脂。从树脂的滴定曲线和静态。动态吸附实验中，得到了它们的总交换容量和对庆大霉素的交换容量，因此也得到了相对交换容量。最后通过含钙离子庆大霉素溶液的静态吸附实验，比较了树脂的选择性。结果表明，水解时间2h的树脂效果最好，其庆大霉素的相对交换容量达到96．57％，且对庆大霉素吸附量最大，而钙离子吸得最少。

Optimization of Preparative Separation and Purification of Total Flavonoids from Radix Puerariae by Macroporous Resin Method

Aim To screen the optimum macroporous resin and conditions for the isolation and purification of flavonoids from Radix Puerariae. Methods The static and dynamic adsorption/desorption methods were used, and the separation and purification process was evaluated by measuring the concentration of total flavonoid in the fractions with UV spectrophotometer. Results The SP70 macroporous resin was the most effective compared with other macroporous resins. The optimum conditions were screened, which were 0.5 g· mL^- 1 corresponding to crude drug for concentration of extract, pH 5 - 6, and appended 60 times the volume of the resin bed （BV） with the adsorption speed 2 BV·h^-1, and the volume of aq. 70% （V/V） ethanol as eluant was 5 BV with desorption speed 2 BV·h^-1. By this method, the final contents of total flavonoids exceeded 80%. Conclusion The SP70 macroporous resin is the most effective one for large-scale isolation and purification of flavonoids from Radix Pueraria, which meets industrial needs.

Optimization for Purification and Characterization of Recombinant Hirudin Ⅲ from E. coli

Aim To optimize purification conditions of recombinant hirudin 3 in thefermentation broth and characterize the product. Methods Reambinant hirudin 3 was isolated andpurified from the fermentation broth by three column chromatography steps with macroporous resin,DEAE cellulose DES2 and preparative RP-HPLC, respectively, and the optimal conditions were obtained.Purity of the product was determined by SDS-PAGE and analytical RP-HPLC. The molecular weight wasdetermined by mass spec-trometry. The structure of the product was analyzed by peptide map.ResultsThe product with purity of 95.4786% was obtained after three purification steps in the optimumconditions with a total yield of 39%. The molecular weight of the product was 6 913.32 ± 6.55 Da,coincident to the theoretical molecular weight of r-hirudin 3. The structure of the product wascoincident to r-hirudin 3 either. Conclusion The optimized purification steps can be successfullyemployed for purification of r-hirudin 3 from E. coli using batch-type approaches. The productobtained with high purity was confirmed to be r-hirudin 3.

蜂疗治疗鼻炎效果好

郑某患鼻炎十几年,多种治疗方法都无效,白天和晚上睡觉都是用嘴巴呼吸,非常难受。笔者对其用蜂疗2周后便可以用鼻子呼吸,晚上睡觉时呼吸也非常畅通。过敏性鼻炎和萎缩性鼻炎是由副交感神经和交感神经过度兴奋,刺激或抑制鼻腔腺体分泌,使鼻黏膜血管扩张和收缩,引起分泌物的增多或减少导致的。

Separation and Purification of Macranthoidin B and Dipsacoside B from Flos Lonicerae by HP-20 and HP-SS Macroporous Resin

[Objective] This study was conducted to develop a method for rapidly separating macranthoidin B and dipsacoside B from Flos Lonicerae. [Method] HP-20 and HP-SS macroporous resin were applied to separate and purify macranthoidin B and dipsacoside B from Flos Lonicerae. The extract of Flos Lonicerae was first loaded onto an HP-20 column to enrich saponins, which were then separated by an HP-SS macroporous resin column to get pure macranthoidin B and dipsacoside B.[Result] The optimal HP-20 purification conditions included： a concentration of sample liquid at 4.8 mg/ml, a sample volume of 2 BV, an adsorption flow rate at 1.5BV/h, an ethanol concentration for desorption at 60%, a desorption volume of 3 BV,and a desorption flow rate at 1.5 BV/h. Total saponins were then separated by an HP-SS macroporous resin column which was eluted sequentially by water, 20%ethanol, 30% ethanol, 40% ethanol and 50% ethanol. Two purified compounds were obtained in fractions eluted by 40% ethanol and 50% ethanol, respectively. The two compounds were identified as macranthoidin B and dipsacoside B by13 C and1H nuclear magnetic resonance spectroscopy. [Conclusion] The combination of HP-20 and HP-SS macroporous resin could efficiently separate macranthoidin B and dipsacoside B from Flos Lonicerae.

Macroporous Resin Adsorption for Purification of Flavonoids in Houttuynia cordata Thunb

Flavonoids are one main kind of effective components in Houttuynia cordata Thunb., which display a wide range of pharmacological activity. In this study supercritical fluid extraction （SFE） with carbon dioxide was first used as preparat ion step to remove the volatile components, which are also active components, from Hout-tuynia cordata Thunb. Then ultrasound-assisted extraction was used to obtain the crude flavonoids and the macro-porous resin adsorption technology was further employed to purify the flavonoids. Nine kinds of macroporous resins with different properties were tested through static adsorption, and one macroporous resin labeled as D101 was selected. The effect of several factors, such as the ratio of column height to diameter, initial concentration and pH, on both flavonoids yield and content were explored by dynamic adsorption to obtain reasonable conditions of adsorption and desorption. The experimental results show that the content of fiavonoids can be above 60% with fia- vonoids recovery of 93.3 % under the optimum conditions of purification. HPLC analysis of the final flavonoids product shows it contains quercitrin, hypefin, rutin and quercetin.

Optimization of Preparative Separation and Purification of Total Polyphenols from Sargassum tenerrimum by Column Chromatography

Polyphenols from the ethanol extracts of Sargassum tenerrimum （ST） with potent antiallergic effects were studied to optimize separation process through column chromatography. The adsorption and desorption characteristics of three widely used adsorbents： macroporous resin, silica gel, and polyvinylpolypyrrolidone （PVPP）, were critically evaluated respectively and studied for the optimization of preparative separation of polyphenols. Static operations on these adsorbents showed that macroporous resin had the best adsorption and desorption capability among the three adsorbents. Dynamic adsorption and desorption with macroporous resin packed column were also conducted to optimize the parameters such as： with the optimal values shown in brackets, the concen- tration of extract solution （4 times diluted）, pH value （6-7）, adsorption speed （3BVh-1, bed volumes/per hour）, concentration of ethanol （80%）, elution speed （3 BV ht） and elution volume （7 BV）. The chromatographic process so optimized gave a purity of 62.43% from the crude polyphenols, providing a promising basis for large scale preparation of bioactive polyphenols upon further scaling up tests.

Comparison between Decolorization Effects of Activated Carbon and Macroporous Resin on Periplaneta americana L. Skimmed Cream

[Objective] The aim of this study was to investigate the decolorization ef- fects of activated carbon and macroporous resin on Periplaneta americana L. skimmed cream and compare the advantages and disadvantages of the two decolorization technologies. [Method] Periplaneta americana L. skimmed cream was decolored with activated carbon and macroporous resin, and freeze-dried to collect solid decolorization products. By investigating the yield, decolorization rate, protein retention rate and decolorization operation process, the advantages and disadvantages of the two decolorization technologies were compared. [Result] Both activated carbon and macroporous resin can be used for decolorization. To be specific, macroporous resin-decolorization is superior in the yield and protein retention rate, while activated carbon-decolorization is superior in decolorization rate and decolorization operation process. [Conclusion] Macroporous resin-decolorization can be used if protein is the main ingredient required in the experiment, while activated carbon-decolorization can be used if protein is not the main ingredient required.

STUDIES ON THE SORPTION OF MACROPOROUS PHOSPHONIC ACID RESIN FOR LANTHANUM

The influences of medium pH sorption temperature, sorption time, etc. on thesorption capacity of macroporous Phosphonic acid resin for La3+ were determined Thesorption rate constant was k298 = 7.64×10-5 s-1. The complex ratio of phosphonicgroups of the resin to La3+ was 3:1. The basic sorption parameters were determinedThe sorption mechanism of macroporous phosphonic acid resin for La3+ was examinedby chemical analysis and IR- spectrometry.

Adsorption of Pb^(2+) on macroporous weak acid adsorbent resin from aqueous solutions: Batch and column studies

The adsorption properties of a novel macroporous weak acid resin （D152） for Pb^2＋ were investigated with chemical methods. The optimal adsorption condition of D152 resin for Pb^2＋ is at pH 6.00 in HAc-NaAc medium. The statically saturated adsorption capacity is 527 mg/g at 298 K. Pb^2＋ adsorbed on D152 resin can be eluted with 0.05 mol/L HCI quantitatively. The adsorption rate constants determined under various temperatures are k288 n=2.22×10-5 s^-1, k298 K=2.51 × 10^-5 s^-1, and k308 K= 2.95 × 10^-5 s^-1, respectively. The apparent activation energy, Ea is 10.5 kJ/mol, and the adsorption parameters of thermodynamics are ΔH^Θ=13.3 kJ/mol, ΔS^Θ=119 J/（mol·K）, and ΔG^Θ298 K =-22.2 kJ/mol, respectively. The adsorption behavior of D152 resin for Pb^2＋ follows Langmuir model.

ADSORPTION OF MACROPOROUS PHOSPHONIC ACID RESIN FOR INDIUM

The adsorption kinetics and mechanism of a novel chelate resin, macroporous phosphonic acid resin (PAR) for In(III) were investigated. The statically saturated adsorption capacity is 216mg穏-1resin at 298K in HAc-NaAc medium. The apparent adsorption rate constant is k298=4.84?0-5 s-1. The adsorption behavior of PAR for In(III) obeys the Freundlich isotherm. The thermodynamic adsorption parameters, enthalpy change △H, free energy change △G and entropy change △S of PAR for In(III) are 11.5kJ/mol, -12.6kJ/mol and 80.8J/mol稫, respectively. The apparent activation energy is Ea=3.5kJ/mol. The molar coordination ratio of the functional group of PAR to In(III) is about 3∶1.

ADSORPTION DYNAMICS OF MACROPOROUS POLYMERIC ADSORBENT Ⅱ. The Studies on the Film Diffusion Mass-Transfer Process

The film diffusion mass-transfer process of adsorption of phenol on macroporous polystyrene resin was investigated in detail In order to revise the Boyd film diffusion kinetics equation, the out-surface structure of the macroporous resin and that of gel-type ion-exchange resin was compared and the new film diffusion equation was also suggested. These results showed that the film diffusion was influenced by porosity of the macroporous resin greatly, which differed from the film diffusion behavior of ion-exchange resin obviously.

Oxidation of Benzothiophenes Using Tert-amyl Hydroperoxide

Homogeneous oxidation using an oil-soluble oxidant, tert-amyl hydroperoxide （TAHP）, for ultra-deep desulfurization was performed under mild conditions in the presence of molybdenum oxide catalysts. Dibenzothio- phene （DBT）, benzothiophene （BT） and 4, 6-dimethyl-dibenzothiophene （DMDBT）, which are the refractory sulfur compounds for hydrodesulfurization （HDS）, were employed as model substrates for a simulated diesel fuel. Activity of molybdenum oxide supported on a macroporous weak acidic resin was investigated. The mass conversion of DBT reached near 100% at 90℃ and a TAHP/DBT molar ratio of 3 with 1% of molybdenum oxide supported on Amberlite IRC-748 resin for 1 h. It was further found that the activities of the model substrates decreased in the or- der of DMDBT 〉DBT 〉BT. In the flow oxidation using TAHP as the oxidant, mass conversion of DBT increased remarkably from 61.3% to 98.5% when dropping the weight hourly space velocity （WHSV） from 40 h^-1 to 10 h^-1. A series of experiments dealt with selectivity of this oxidation using TAHP revealed that the model unsaturated compounds, i.e. 4, 6, 8-trimethyl-2-nonylene, and 2-methylnaphthalene did not affect the oxidation of DBT. Carbazole had nearly no effect on the conversion of DBT using TAHP, but had some influence on the one using tert-butyl hydroperoxide （TBHP）. The mass conversion of DBT decreased remarkably from 75.2% to 3.6% when the content of carbazole increased from 0 to 500μg·g^-1. In the flow oxidation using TAHP as the oxidant, the concentration of DBT in model fuels was reduced from 500 μg·g^-1 to 7.2 μg·g^-1 at WHSV of 10 h^-1, and then reduced to 3.8 μg·g^-1 by adsorntion of Al2O3.

Preparation of Aminated Macroporous Polyvinyl Alcohol Resins and Evaluation for Bilirubin Adsorption

In the present study we prepared macroporous polyvinyl alcohol beads. A series of bilirubin adsorbents were generated by immobilization of eight amine agents to the beads as ligands. The adsorption of bilirubin was evaluated by in vitro static and dynamic adsorption tests. The results show that these adsorbents have excellent adsorption efficiency and capacity. Among the eight ligands, trimethylamine （TMA）, triethylamine （TEA） and 1,6- hexanediamine （HDA） showed the highest adsorption capacity. The adsorption equilibrium can be achieved in half an hour, and the adsorption percentage of bilirubin was up to 80%. Static electricity and hydrophobie interaction played the main role in bilirubin adsorption, and the adsorption was found to match the monolayer model. The excellent adsorption of these adsorbents indicates their potential in clinical treatment.

ADSORPTION AND DESORPTION OF DSD ACID MANUFACTURING WASTEWATER ON MACROPOROUS RESIN

4,4’-diaminostilbene-2, 2’-disulfonic acid (DSD acid) manufacturing wastewater was treated by a macroporous resin in a fixed-bed column. The results showed that this method was suitable for removal of chemical oxygen demands (COD) and color. About 91% COD and 99.5% color removal were obtained under the optimum adsorption conditions, i.e. temperature 20℃, flow rate 1bed volume/hour (BV/hr) and pH1-2. The resin was efficiently regenerated with aqueous sodium hydroxide and water. Furthermore, 65.5% of 4,4’-dinitrostilbene-2, 2’-disulfonic acid (DNS) could be recovered from wastewater for possible recycling to the manufacturing process. The adsorption capacity of resin remained constant during the repetition process of adsorption and desorption.

Preparation and Characterization of Macroporous Resin Immobilized Pd－Cu Bimetallic Cluster Catalysts

The Solvated Metal Atom Impregnation (SMAI) technique was employed to prepare macroporous resin immobilized Pd--Cu bimetallic cluster catalysts. The X--ray diffraction (XRD) and transmission electron micrograph (TEM) showed that Pd--Cu alloy was formed and the particle sizes of Pd--Cu clusters were very small, with average diameters <3nm. X--ray photoelectron spectroscopy indicated that both Pd and Cu were in zero--valent state. The catalytic activities of the macroporous resin immobilized Pd--Cu catalysts in hydrogenation of 4--methyl--3--penten--2--one were much greater than that of the carbon supported Pd--Cu catalysts.

Application Progress of Porous Materials in Modern Pharmaceutical

Porous materials have regular three-dimensional pore structure, which has unique advantages in the field of modern pharmaceutical. At present, porous materials commonly used in the pharmaceutical field are mainly molecular sieves, macroporous adsorbent resins, activated carbon, etc. In this paper, the application status of these porous materials in the pharmaceutical field is reviewed, and the future development is prospected.