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.

Static and dynamic studies of adsorption by four macroporous resins to enrich oridonin from Rabdosia rubescens

Oridonin,one of the active ingredients in Rabdosia rubescens(R.rubescens),has been reported to induce cell apoptosis and cell cycle arrest in many cancers.Conventional extraction methods tend to result in unsatisfied enrichment and poor quality of oridonin present in a given biomass.This paper aims to evaluate the performance and separation characteristics of four different macroporous resins to arrive at the most suitable methodology for the isolation and purification of highquality oridonin.Static absorption kinetics,thermodynamic and dynamic adsorption were evaluated.HP20 was selected for further study due to its high adsorption capacity of 32 mgg 1 and desorption ratio with 98.5%.The pseudosecondorder model was considered to be the most suitable for kinetic results,and Langmuir model was chosen to better describe the absorption thermodynamics.Under optimum conditions(flow rate of 4 ml min 1,bed depth with 6 cm and initial concentration of 2.15 mg·ml^1),the effective content of oridonin increased from 33.9%to 79.1%in the dry extract with a recovery of 81%and the purity of oridonin improved from 76%to 93%.The results confirm that HP20 provides an efficient method to purify most oridonin from R.rubescens.

Adsorption of Macroporous Phosphonic Acid Resin for Nickel

Tje adsorption bchavior and mechanism of a novel chelate resin,macroporous phosphonic acid resin（PAR）for Ni（Ⅱ）were imestigated.The stotically saturated adsorption capacity is 64.3mg·g^-1 resin at 298K in HAc-NaAc medium.The Ni（Ⅱ）adsorbed on PAR can be eluted by 0.5mal·L^-1 HCl and the elution percentage reaches 96.6%.The resin can be regenerated and reused without abvious decrease in adsorption capacity.The apparent adsorption rate constant is k298=2.6×10^-5s^-1.The adsorption behavior of PAR for Ni（Ⅱ）obeys the Freundllich isotherm.The thermodynamie adsorption parameters.enthalpy change △H,free energy change △G and entropy change △S of PAR for Ni（Ⅱ）are 3.36kJ·mol^-1,-5.47kJ·mol^-1 and 29.6J·mol^-1·K^-1,respectively.The apparent activation energy is Ea=12.2kJ·mol^-1,The molar coordination ratio of the functional group of PAR to Ni（Ⅱ）is about 4：1.The adsorption mechanism of PAR for Ni（Ⅱ）was examined by a chemical method and IR spectrometry.

Preparation and adsorption properties of macroporous tannin resins

In this paper, a new kind of adsorption resin with multi-phenolic hydroxyl was created by immobilizing black wattle bark tannins to chloromethyl polystyrene resin. Its adsorption capacity to cation dye was tested. With an orthogonal test the optimal conditions of synthesis were determined： the concentration of sodium hydroxide solution 1.0 mol.L^-1; the reaction time is one hour and the mass concentration of tannins 5%. With single factorial experiment the optimal conditions of adsorption were confirmed： a solidified pH of 5.0; an adsorption temperature of 25℃ and a cation dye concentration of 100 mg.L^-1. The adsorption for cation dye can be similar to Langmuir isotherms.

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 Behavior and Mechanism of Macroporous Phosphonic Acid Resin for Lu^(3+)

The article is based on a research on the adsorption behavior and adsorption mechanism of macroporous phosphonic acid resin (PAR) for Lu 3+ and the influence of the medium’s pH, adsorption temperature, adsorption time, etc on adsorbing Lu 3+ . The best value of medium’s pH to the adsorption of PAR for Lu 3+ was found to be 4.92. The static adsorption maximum capacity of PAR for Lu 3+ is 220?mg·g -1 . The thermodynamic adsorption parameters are respectively ΔH=11.3?kJ·mol -1 , ΔS=46.3?J·mol -1 ·K -1 , ΔG=-2.50?kJ·mol -1 and the apparent activity energy is E_a=31.4?kJ·mol -1 . The adsorption behavior of PAR for Lu 3+ obeys the Freundlich isotherm. The apparent adsorption rate constant is k_ 298 =4.68 ×10 -5 ?s -1 . The coordinate ratio of the functional radical to Lu 3+ is approximately 4∶1. The best eluant is 1.0?mol·L -1 HCl. The adsorption mechanism of PAR for Lu 3+ was separately confirmed by chemical analysis and IR spectra.

ADSORPTION OF TANNIN ACID ONTO AN AMINATED MACROPOROUS RESIN FROM AQUEOUS SOLUTIONS

A macroporous polymeric adsorbent NG-8 was synthesized with divinylbenzene using conventional suspension polymerization technique. Its aminated product NG-9 was prepared by introducing tertiary amino groups into NG-8 for removal of tannin acid from aqueous solutions. NG-9 could be used directly without a wetting process and had higher adsorption capacity than NG-8, which might be attributed to the enhanced adsorbent-adsorbate interaction due to the tertiary amino groups on the polymeric matrix. The Langmuir equation was successfully employed to describe the adsorption process. The adsorption enthalpy change further validated the uptake of tannin acid on NG-9 to be an enhanced physical adsorption because of the Lewis acid-base interaction. In addition, adsorption kinetic studies testified that the tertiary amino groups on the polymer matrix could decrease the adsorption rate maybe for the hindrance of the tertiary amino groups and water clusters built up.

Adsorption Behaviors and Mechanism of Macroporous PhosphonicAcid Resin for Gadolinium

The adsorption behaviors and mechanism of a novel chelate resin, macroporous phosphonic acid resin(PAR)for Gd(Ⅲ)were investigated. The statically and dynamically saturated adsorption capacity is respectively 308 mg·g^(-1)resin and 296 mg·g^(-1)resin at 298 K in HAc-NaAc medium at pH 5.6. Gd(Ⅲ)adsorbed on PAR can be reductively eluted by 0.5～5.0 mol·L^(-1) HCl used as eluant and the elution percentage is up to 94.7% in 1.0 mol·L^(-1) HCl. The resin can be regenerated and reused without apparent decrease in adsorption capacity. The apparent adsorption rate constant is k_(298)=3.96×10^(-5) s^(-1). The adsorption behavior of PAR for Gd(Ⅲ) conforms to the Freundlich isotherm. The thermodynamic adsorption parameter, enthalpy change △H of PAR for Gd(Ⅲ)is 22.6kJ·mol^(-1). The apparent adsorption activation energy(Ea)of PAR for Gd(Ⅲ)is 5.0 kJ·mol^(-1). The molar coordination ratio of the functional group of PAR to Gd(Ⅲ)is about 3∶1. The adsorption mechanism of PAR for Gd(Ⅲ)was examined by using chemical method and IR spectrometry.

Adsorption of copper using macroporous phosphonic acid resin

The adsorption behavior and mechanism of a novel chelate resin, macroporous phosphonic acid resin（PAR） for Cu（Ⅱ） were investigated. The statically saturated Cu（Ⅱ） adsorption capacity is 168 mg/g resin at 298K in HAc-NaAc medium. The Cu（Ⅱ） adsorbed on PAR can be eluted by 1.03.0 mol/L HCl and the elution percentage reaches 100%. The resin can be regenerated and reused without apparent decrease in adsorption capacity. The apparent adsorption rate constant is (k=1.64×10-4 s-1) at 298K. The adsorption behavior of PAR for （Cu（Ⅱ）） obeys the Freundlich isotherm. The thermodynamic adsorption parameters, enthalpy change ΔH, free energy change ΔG and entropy change ΔS of PAR for Cu（Ⅱ） are 11.8 kJ/mol, -2.0 kJ/mol and (46.4 J·mol-1·K-1) respectively. The apparent activation energy is Ea=8.0 kJ/mol. The molar coordination ratio of the functional group of PAR to Cu（Ⅱ） is about 2∶1. The adsorption mechanism of PAR for Cu（Ⅱ） was examined by chemical method and IR spectrometry.

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 behavior and mechanism of D113 resin for lanthanum

The sorption properties of macroporous weak acid resin （D113） for La^3＋ ion were studied by chemical analysis and IR spectra. Experimental results indicate that the D113 resin has a good adsorption ability for La^3＋ at pH = 6.0 in the HAc-NaAc medium. The statically saturated adsorption capacity is 273.3 mg/g. Separation coefficients of βLa^3＋/Ce^3＋, βLa^3＋/Gd^3＋, βLa^3＋/Er^3＋, and βLa^3＋/Y^3＋ are 2.29, 3.64, 4.27, and 0.627, respectively. The apparent activation energy of adsorption, Ea is 18.4 kJ/mol, the thermodynamics parameters AH, AS, and AG of sorption are 4.53 kJ/mol, 61.8 J/（mol·K）, -13.9 kJ/mol, respectively. The adsorption behavior of D113 for La^3＋ obeys the Freundlich isotherm. La^3＋adsorbed on resin can be eluted by 2.0 mol/L HCl quantitatively.

Separation of salidroside from the fermentation broth of engineered Escherichia coli using macroporous adsorbent resins

Salidroside(8-O-β-D-glucoside of tyrosol),a plant-derived natural product,is used for treatment of hypoxia,fatigue and aging diseases.The availability of salidroside is restricted since it is extracted from3-5 years old Rhodiola roots,which grow very slowly in the cold region of northern hemisphere of Earth.Our laboratory has constructed an engineered Escherichia coli and established a fermentation process to produce salidroside from glucose.In this article,nine macroporous resins from polarity to non-polarity,including NKA-9,S-8,AB-8,SP825,D101,LSA-8,LX-12,LX-18 and LX-68 resins,were tested to separate salidroside from fermentation broth.After static and dynamic experiments,the weakly polar SP825 resin had a better separation efficiency among nine resins.The adsorption kinetic and isotherm of salidroside on the SP825 resin were determined,and the pseudo-second-order kinetic model and Langmuir model could be fitted well.The effects of the pH on adsorption and ethanol concentration on desorption were investigated,and an optimal separation process was established.The adsorption for salidroside in the SP825 resin column was conducted with loading 150 ml at pH 7,and desorpted by washing 50 ml of80%ethanol solution.Under the best process conditions,the purity and yield of salidroside in the final product were 91.6%and 74.0%,respectively.The results showed that the macroporous SP825 resin would be feasible and effective to prepare salidroside and has promising application in the downstream process of microbial fermentation.

Screening of Macroporous Resin for Polysaccharide of Solanum nigrum L.

[Objectives] To screen the optimal macroporous resin for polysaccharide of Solanum nigrum L. [Methods] The polysaccharide content was taken as the indicator, and adsorption and desorption performance of 20 kinds of resin were observed and studied. [Results] Adsorption and desorption performance of 20 kinds of resin had significant difference. S-8 type macroporous resin showed the best comprehensive property. [Conclusions] S-8 type macroporous resin should be used to purify polysaccharide of S. nigrum L.

THERMODYNAMIC STUDY OF ADSORPTION OF PHENOLIC COMPOUNDS FROM AQUEOUS SOLUTION BY A WATER-COMPATIBLE HYPERCROSSLINKED POLYMERIC ADSORBENT

Equilibrium data for the adsorption of phenolic compounds, i.e., phenol, p-cresol, p-chlorophenol and p- nitrophenol from aqueous solutions by a water-compatible hypercrosslinked polymeric adsorbent (NJ-8) within temperature range of 283-323 K were obtained and correlated with a Freundlich-type of isotherm equation, so that equilibrium constants KF and n were obtained. The capacities of equilibrium adsorption for all the four phenolic compounds on the NJ-8 from aqueous solutions are around 2 times as high as those of Amberlite XAD-4, which may be attributed to the unusual micropore structure and the partial polarity on the network. The values of the enthalpy (always negative) are indicative of an exothermic process, which manifests the adsorption of all the four phenolic compounds on the two polymeric adsorbents to be a process of physical adsorption. The negative values of free energy change show that the solute is more concentrated on the adsorbent than in the bulk solution. The absolute free energy values of adsorption for NJ-8 are always higher than those for Amberlite XAD-4, which indicates that phenolic compounds are preferentially adsorbed on NJ-8. The negative values of the adsorption entropy are consistent with the restricted mobilities of adsorbed molecules of phenolic compounds as compared with the molecules in solution. The adsorption entropy values of phenolic compounds for NJ-8 are lower than those for Amberlite XAD-4, which means the micropores of NJ-8 require more orderly arranged adsorbate.

Preparation of Macroporous Poly (vinyl alcohol-co-triallyl isocyanurate) Beads Bearing Aminocarboxylic Acid as Functional Groups by Suspension Polymerization

Macroporous poly (vinyl acetate-co-triallyl isocyanurate) beads were prepared with suspension polymerization method. The copolymer beads were then transformed into poly (vinyl alcohol-co-triallyl isocyanurate) by ester exchange reaction. Aminocarboxylic acids were immobilized on the copolymer beads by the esterification of hydroxyl groups with diethyl-lenetriaminepentaacetic bisanhydride. The weak acid exchange capacities, specific surface areas and mean pore diameters of the resultant resin beads were measured.

ISOLATION AND PURIFICATION OF ALKALOIDS FROM PLUMULA NELUMBINIS BY DOUBLE-COLUMN ADSORPTION CHROMOTOGRAPHY

The performance of adsorption and separation for liensinine, isoliensinine and neferine was studied by double-column adsorption chromatography using macroporous adsorption and cation exchange resins. The alkaloid extract with 49.2% total contents by mass representing 10.6% liensinine, 10.6% isoliensinine and 28.0% neferine respectively was prepared by D72 cation exchange resins, in which most of the impurities were water-soluble alkaloids. Furthermore,the alkaloid extract with 82.6% total contents by mass containing 33.1%, 15.0% and 34.5% of the three adsorbates respectively was prepared by double-column adsorption chromatography using AKS-W macroporous adsorption and D72 cation exchange resins. As a result, the content of single and total alkaloids has been greatly increased by the double-column adsorption chromatography.

深共熔溶剂提取桑黄黄酮及体外降血糖、结合胆酸盐能力分析

从7种深共熔溶剂中筛选最适合用于桑黄黄酮化合物提取的溶剂体系,采用响应面优化深共熔溶剂提取桑黄黄酮的工艺,筛选最佳黄酮回收树脂,并分析其体外降血糖和结合胆酸盐能力。试验结果表明,乙二醇与氯化胆碱组成的深共熔溶剂体系最适合提取桑黄黄酮,最佳提取工艺为深共熔溶剂含水率30%,乙二醇与氯化胆碱的物质的量比为8.21∶1,料液比=50∶1(mg∶m L),提取温度64℃,提取时间43 min,在此条件下,桑黄黄酮得率为(8.85±0.34)%,较体积分数为60%乙醇提取的得率提高了2.02倍。9种大孔树脂中,AB-8型大孔树脂对桑黄黄酮的回收率最高,为85.25%;纯化后桑黄黄酮的纯度提高了6.12倍。桑黄黄酮抑制α-淀粉酶和α-葡萄糖苷酶活性的IC_(50)值分别为1.19 mg/m L和1.28 mg/m L,结合牛磺胆酸钠和甘氨胆酸钠的IC_(50)值分别为0.62 mg/m L和1.19 mg/m L,表明桑黄黄酮具有较强的调节血糖和血脂能力。实验表明,深共熔溶剂结合大孔吸附树脂富集回收可以绿色高效地从桑黄中提取黄酮类化合物。

贵州野生刺梨叶黄酮的纯化工艺研究

研究旨在通过超声波提取法利用60%乙醇提取贵州野生刺梨叶片中的总黄酮,通过静态吸附试验研究了5种大孔吸附树脂对总黄酮的动态吸附特性,筛选出了对刺梨叶黄酮具有良好吸附和解吸性能的大孔吸附树脂。以吸附率和解吸率作为考察指标,对大孔树脂纯化刺梨叶黄酮的提取工艺进行优化。结果显示,大孔吸附树脂AB-8具有较好的吸附以及解吸性能,当纯化工艺为径高比1∶2(2BV)、上样液浓度0.6 g/L、控制流速2 mL/min时,AB-8大孔吸附树脂可快速有效地吸附刺梨叶中的黄酮。进一步使用55%乙醇80 mL,保持洗脱流速为2 mL/min时可以快速充分地洗脱AB-8大孔吸附树脂吸附的黄酮。在该纯化条件下,刺梨叶黄酮的纯度从3.368 mg/g提高至6.679 mg/g。研究表明,该工艺条件适于刺梨叶黄酮的纯化。

大孔树脂对纺织印染废水吸附性能研究

研究XDA-11树脂对次甲基蓝纺织印染废水的吸附行为,考察吸附时间、pH值、温度、流速等对树脂吸附性能的影响。结果显示,在静态吸附条件下,调节温度48℃,pH值为11.0,吸附4.5 h,使用0.120 0 g树脂处理80.0 mL,质量浓度为50.0 mg/L的废水,废水脱色率约为99.66%。在动态吸附条件下,在常温,调pH值为11.0,吸附流速为2BV/h时,处理质量浓度为500.0 mg/L的废水,废水处理量达到126 BV,脱色率约为99.98%。用盐酸-碱性乙醇对树脂进行多次再生,再生率达70.39%以上。

葛根蛋白酶解物大孔树脂吸附工艺优化及其体外抗氧化活性研究

目的:优化大孔树脂吸附葛根蛋白酶解物工艺及其抗氧化活性研究。方法:采用Box-Behnken响应面法确定大孔树脂吸附葛根蛋白酶解物最佳工艺。以维生素C为对照,测定最佳工艺下纯化前后葛根蛋白酶解物的抗氧化活性。结果:大孔树脂的最佳吸附—解吸工艺为上样液质量浓度10.0 mg/mL,洗脱液流速2.6 mL/min,洗脱液乙醇体积分数74%,纯化后葛根蛋白酶解物含量提升至37.19%。大孔树脂纯化后的葛根蛋白酶解物对DPPH自由基、ABTS+自由基、羟自由基的清除率均强于吸附前的。结论:大孔树脂纯化后的葛根蛋白酶解物抗氧化效果良好,可以作为一种潜在的蛋白多肽应用于食品中。