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.

Macroporous Resin Adsorption for Purification of Flavonoids in Houttuynia cordata Thunb

Flavonoids 是在 Houttuynia 英国管数据 Thunb 的一个主要有点有效的部件，它显示大量药理学活动。在这研究，有二氧化碳的超级批评液体抽取(SFE ) 首先被用作移开不稳定的部件的准备步，它也是活跃部件，从 Houttuynia 英国管数据 Thunb。然后帮助超声的抽取被用来获得粗略的 flavonoids 和宏多孔的树脂吸附技术进一步被采用净化 flavonoids。九种宏有不同性质的多孔的树脂通过静态的吸附，和一个宏被测试作为 D101 标记的多孔的树脂被选择。几个因素的效果例如到直径，起始的集中和 pH 的列高度的比率，被动态吸附在 flavonoids 产量和内容上探索获得吸附和解吸附作用的合理条件。试验性的结果证明 flavonoids 的内容能与在纯化的最佳条件下面的 93.3 % 的 flavonoids 恢复超过 60% 。最后的 flavonoids 产品的 HPLC 分析证明它包含橡素，在亢奋，卢丁和橡黄素。

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 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 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 Pb2+ were investigated with chemical methods. The optimal adsorption condition of D152 resin for Pb2+ is at pH 6.00 in HAc-NaAc medium. The statically saturated adsorption capacity is 527 mg/g at 298 K. Pb2+ adsorbed on D152 resin can be eluted with 0.05 mol/L HCl quantitatively. The adsorption rate constants determined under various temperatures are k288 K=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 -HΘ=13.3 kJ/mol, -SΘ=119 J/(mol·K), and -GΘ298 K =-22.2 kJ/mol, respectively. The adsorption behavior of D152 resin for Pb2+ follows Langmuir model.

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.

Separation and Purification of Glufosinate Through Combination of an Electrodialysis Membrane and a Macroporous Adsorption Resin

Glufosinate is a nonselective organophosphorus herbicide with low toxicity and high efficiency that is widely used in forestry, agriculture and other industries. In the process of manufacturing glufosinate, large amounts of ammonium chloride and coloured organic impurities are generated. Because of its high solubility in water, separation of glufosinate from inorganic salts is extremely difficult. Hence, a co-separation method combining an electrodialysis membrane and a macroporous adsorption resin was developed to obtain glufosinate with higlier purity. For the electrodialysis process, a glufosinate reaction solution was placed in a dilute chamber and desalinated. The concentration of inorganic salts in the resultant glufosinate aqueous solution was only 0.99 g/L under the optimal conditions of an operating voltage and a volume ratio of 9 V and 1:1, respectively. For the macroporous resin adsorption/desorption process, the sample solution treated by electrodialysis was pumped into the resin-filled column, which was eluted to obtain the eluent when the adsorption reached equilibrium. Consequently, nearly all the coloured organic impurities were removed under the optimal conditions, in which the resin type, pH value, flow rate, glufosinate concentration, temperature, ratio of ethanol and volume of eluent were LX-300C,3,0.5 mL·cm^2·min^-1,20 mg/mL,25℃, 50% and 400 mL, respectively. After the electrodialysis and adsorption/desorption process, the purity of the glufosinate was increased to 95.14%, and its recovery rate was as high as 98%. The advantages of this process included its ease of operation, environmental friendliness and low cost, which provided strong potential for its use in industrial applications.

Separation of gibberellic acid (GA3) by macroporous adsorption resins

The adsorption effects of several macroporousadsorption resins for gibberellic acid (GA3) were investigated.The dynamic adsorption capacity is 58.38 mg/g drybeads for resin R4 and 96.46 mg/g dry beads for resin R5which is consistent with the surface area. Aqueous methanol(50%, V/V) is a good eluent and the yield of GA3 isabove 95%. The concentration of GA3 could increase fivefoldafter an adsorption-elution cycle and this is importantwhen considering further crystallization of GA3 in anindustrial process.

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.

两面针粗生物碱的富集

目的探索两面针对体外人红系白血病细胞(HEL细胞)增殖活性有抑制作用的粗生物碱富集方法,为两面针药材抗肿瘤活性研究提供参考。方法以不同浓度(60%、70%、80%、90%、100%)乙醇对两面针药材的干燥根进行提取,以最高提取率确定最佳提取条件;通过静态、动态吸附实验考察不同类型(HPD 100、XDA-5、D101、HPD 722、HPD 400)大孔树脂对两面针药材的吸附量确定上样量,富集两面针粗生物碱;采用噻唑蓝(MTT)法研究各组粗生物碱对HEL细胞增殖活性的影响。结果两面针药材经5种浓度乙醇提取,其中60%乙醇提取浸膏的得率最高[(11.937±0.002)%];静态、动态吸附实验表明,5种大孔树脂对两面针药材吸附量为1:500(两面针浸膏:大孔树脂);不同型号大孔树脂富集得到的粗生物碱对HEL细胞的增殖活性影响不同,两面针粗生物碱样品浓度为80μg·mL-1时,抑制率分别为(59.62±3.46)%(XDA-5)、(55.81±5.16)%(HPD 100)、(59.33±1.33)%(D101)、(79.63±1.02)%(HPD 722)、(83.97±0.38)%(HPD 400),HPD 400型大孔树脂富集的两面针粗生物碱抑制HEL细胞增殖作用最显著(P<0.01)。结论大孔树脂富集两面针粗生物碱工艺简单、可行,HPD 400型大孔树脂富集的两面针粗生物碱对HEL细胞抑制作用显著。

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。

白术多糖提取分离工艺研究

目的优选白术多糖的提取分离工艺。方法比较氯仿-正丁醇Sevage法去蛋白与不去蛋白白术多糖含量。以吸附率和解吸率为考察指标,优选AB-8型、D101型、LX-38型3种大孔吸附树脂。通过吸附时间、解吸时间、上样流速、上样浓度、洗脱剂用量、洗脱剂浓度和洗脱流速研究AB-8型大孔树脂纯化白术多糖工艺。结果未去蛋白的多糖含量为(5.582±1.4480)%、(5.407±0.7668)%、(5.155±0.7214)%,Sevage法去蛋白后的多糖含量为(4.658±0.1558)%、(4.247±0.0742)%、(4.610±0.1734)%。AB-8型大孔树脂较其他两种树脂,其吸附率及解吸率可达(18.40±0.0300)%,(91.73±0.0781)%,纯化工艺为吸附时间3 h、解吸时间3 h、上样流速1 BV/h、上样浓度0.75 mg/mL、洗脱剂用量4 BV、洗脱剂浓度15%乙醇、洗脱流速3 BV/h。结论本试验为白术多糖的提取分离提供了试验依据,为白术多糖的工业化生产提供了参考。

大孔树脂对砷还原后液中铼的吸附研究

研究了MTA1701型和RCX5143型大孔弱碱性阴离子树脂对砷还原后液中铼的吸附和解吸性能。通过静态吸附,考察了预处理方式、时间、温度、酸度、平衡浓度对树脂吸附铼的影响;采用氨水静态解吸,考察了氨水浓度、解吸体积比、解吸时间、解吸次数对负载树脂解吸率的影响。结果表明:2种树脂性能相近,树脂经过硫酸浸泡预处理后吸附砷还原后液,吸附反应符合准二级反应动力学模型;热力学研究结果表明,降低温度对吸附铼有利,静态平衡吸附量随酸度增大而降低,随平衡浓度增大而提高;在氨水浓度10%、解吸液固体积比V(氨水)∶V(树脂)=2∶1、解吸时间20 min条件下解吸2次,2种树脂的解吸率均大于99.5%。

大孔吸附树脂分离纯化甘草废渣中总黄酮的工艺研究

[目的]开发大孔吸附树脂分离纯化甘草废渣中总黄酮的工艺。[方法]以静态吸附试验比较D101B、AB-8、DM-130这3种大孔吸附树脂对甘草废渣中总黄酮的吸附量和解吸率,筛选最优树脂。采用单因素试验筛选动态吸附过程中样液浓度、上样速度、上样体积、20%乙醇洗脱体积、洗脱剂浓度、洗脱剂体积。[结果]AB-8大孔树脂用于分离纯化甘草废渣中总黄酮效果最佳,样液浓度为2.345~3.126 mg/mL,上样速度为1.0~1.5 mL/min,上样体积为64 mL,20%乙醇洗脱体积为5 BV,80%乙醇洗脱体积为4 BV。经过该纯化工艺总黄酮浓度从15.63%提升至65.68%。[结论]该方法适用于甘草废渣中总黄酮的初步分离纯化。