Adsorption and desorption properties of macroreticular resins for salidroside from Rhodiola sachalinensis A. Bor

Four different macroreticular resins (HZ-801, HPD500, HPD700 and DA201) were evaluated for the adsorption properties of the salidroside extracted from Rhodiola sachalinensis A. Bor. The results showed that DA-201 displayed the optimal adsorption and desorption properties. The static and dynamic adsorption capacities of DA-201 were 21.88 and 13.25 mg/ml, respectively. The purity of 13.8% for the partially purified salidroside product, which was higher than the purity of 10% for sales in the markets, was achieved by one-step separation and purification with 50% ethanol.     

Preparative Purification of Solanesol from Tobacco Leaf Extracts by Macroporous Resins

In the present study, the preparative purification of solanesol by macroporous resins was studied. The adsorption and desorption properties of solanesol on macroporous resins including SP207, SP700, SP825, SP850 and HP20 were compared. SP850 resin offered the best adsorption and desorption capacities based on the research results. Both Langmuir and Freundlich isotherms were used to describe the interactions between the solutes and resin at different temperatures, and the experimental data fits best to the Freundlich isotherms. Adsorption and desorption kinetic curves were obtained for solanesol adsorption on SP850 resin in the temperature range of 298–303 K. The results showed that the mobility of solanesol adsorption increased and the proportion of adsorbed solanesol decreased with increasing temperature. The adsorption kinetic curve can be classified into three portions, i.e., instantaneous adsorption stage, intraparticle diffusion stage and the final equilibrium stage. Dynamic adsorption and desorption experiments were carried out with the column packed by SP850 resin to optimize the separation process. The isocratic and stepwise operations were designed for the separation of solanesol. The use of stepwise elution allowed a reduction in the process time and solvent consumption, but also led to some loss in purity. The corresponding optimal parameters for adsorption and desorption were determined. According to the research results, it can be concluded that SP850 resin possesses a good ability to separate solanesol and the results in this study may provide scientific references for large‐scale solanesol production from tobacco leaf extracts.     

深共熔溶剂-水混合物同步提取红景天苷和酪醇的响应面优化及其分离回收

以深共熔溶剂-水混合物（LAEG40）作为提取溶剂，红景天苷提取率为主要指标，酪醇提取率为辅助指标，在前期单因素实验的基础上，利用响应面法考察了液料比、提取温度、提取时间三个主要因素对红景天中红景天苷和酪醇同步提取的影响。得到的最佳提取条件为: 液料比12.05:1(mL/g)，提取温度60 ℃，提取时间35 min。在此条件下LAEG40对红景天苷的提取率可达到19.3552?0.6604 mg/g，酪醇提取率可达到1.7211?0.0585 mg/g，远高于传统溶剂水、乙醇对红景天苷和酪醇的提取率。为实现LAEG40提取红景天苷和酪醇的回收，进行了大孔树脂吸附分离的研究。经过一系列优化，获得的最佳吸附分离条件为：选用SP-825树脂装柱，每10g树脂上样30 mL LAEG40提取液，洗脱剂选用80 %乙醇，洗脱体积40 mL，洗脱流速1 mL/min，在此条件下红景天苷和酪醇的回收率分别可达60.47 %和85.07 %。     

Optimization of Sulforaphane Separation from Broccoli Seeds by Macroporous Resins

Abstract

In this study, the adsorption and desorption properties of sulforaphane on macroporous resins (HP20, SP207, SP850, and HP2MGL) were investigated. Analysis revealed that SP850 resin was most effective in the separation of sulforaphane. The equilibrium experimental data obtained at different temperatures were well fitted to the Langmuir and Freundlich isotherms. To optimize the separation process, dynamic adsorption and desorption tests were performed with a column packed with SP850 resin. The results showed that the optimum parameters for adsorption were as follows: flow rate: 5 BV/h, pH 2, temperature: 25°C; for desorption: ethanol–water (40:60, v/v), 6 BV as an eluent, flow rate: 6 BV/h. The highest purity of sulforaphane product was 85.9%, i.e., 107‐fold higher than those in broccoli seeds through one run treatment on the column packed with SP850 resin under normal conditions. This indicated the high efficiency of SP850 resin in separating sulforaphane.     

Enrichment and Purification of Total Chlorogenic Acids from Tobacco Waste Extract with Macroporous Resins

In the present study, an evaluation was conducted on the performance and separation characteristics of nine macroporous resins for the enrichment and purification of total chlorogenic acids from tobacco (Nicotiana tobaccum L.) waste extracts. Based on the results, XAD-4 offered higher adsorption and desorption capacities for total chlorogenic acids than other resins. To optimize the separation process of total chlorogenic acids, a column packed with XAD-4 resin was used to perform dynamic adsorption and desorption tests. The results show that the highest purity of the total chlorogenic acids product was 89.27% when optimum parameters for the adsorption process packed with the XAD-4 resin were as follows: flow rate 3.6 BV/h, pH 3.0; for desorption: ethanol–water (40:60, v/v) used as eluent, flow rate 3.6 BV/h, respectively. Therefore, the XAD-4 resin revealed a good ability to enrich and purify total chlorogenic acids. The method developed will provide a potential approach for the large-scale separation and purification of chlorogenic acid in pharmaceutical applications as a medical intermediate or a material for traditional Chinese medicine.     

大孔树脂法分离纯化申嗪霉素的工艺研究

通过大孔吸附树脂对申嗪霉素发酵滤液静态吸附和解吸试验,从6种大孔吸附树脂中筛选出分离纯化申嗪霉素最优的树脂,考察了该树脂对申嗪霉素的静态、动态吸附与解吸性能并对吸附与洗脱的最佳条件进行了研究。结果表明:AB-8树脂对申嗪霉素有很好的吸附和解吸性能,其最优的动态吸附工艺条件为:上样液浓度3 000μg/mL,上样量4 BV,上样流速2 BV/h;最优的解吸条件为:洗脱剂为80%乙醇溶液,洗脱液用量3 BV,洗脱流速1 BV/h。在此优化条件下,申嗪霉素的吸附率、解吸率、收率、纯度的平均值分别达到(90.33±0.14)%、(90.87±0.12)%、(82.1±0.1)%和(90.74±0.14)%(n=5)。     

大孔树脂吸附法提取羟基钴胺素

比较了8种大孔树脂对费氏丙酸杆菌发酵提取液光解转化后形成的羟基钴胺素的吸附性能,考察了上柱料液pH值对吸附量的影响,分析了不同浓度和pH下乙醇溶液作为洗脱剂的解吸情况,研究了上柱速率对吸附量和解吸率的影响。结果表明,静态实验中,LX-50B型大孔树脂对羟基钴胺素的吸附性能最好,当上柱溶液pH为6时,LX-50B树脂饱和吸附量最高,为203.87 mg/g。用pH为2的60%乙醇溶液作洗脱剂时解吸效果最好,羟基钴胺素提取液以2 BV(床柱体积)/h速度上柱吸附饱和,用60%乙醇溶液以0.5 BV/h速度洗脱后,羟基钴胺素浓度提高至1863.32 mg/L,为原提取液浓度的35倍,纯度由0.38%提升至15.73%,提取纯化效果良好。     

大孔树脂吸附法吸附分离黄酮的研究

研究了D101、LD601、LS-303B、LX-28、LX-38型大孔树脂对黄酮的吸附及分离性能。结果表明,LD601型大孔树脂对黄酮的吸附效果较好,pH 2～4的盐酸溶液中,静态吸附量为5 849.312μg/g,对流速2 mL/min黄酮溶液的吸附率可达96.27%,负载1 500μg黄酮的LD601树脂,用40%乙醇50 mL以3 mL/min流速进行解吸,解吸率可达97.51%。     

大孔树脂法分离纯化阿维菌素工艺研究

研究了大孔树脂分离纯化阿维菌素的工艺。采用HPLC检测方法,从7种大孔树脂中筛选出吸附阿维菌素性能最好的树脂并优化其吸附和洗脱参数。结果表明,采用大孔树脂HZ816吸附阿维菌素的效果最佳,其动态吸附量为62mg·mL^-1,在吸附流速为1．5～2BV·h^-1、90％乙醇作为洗脱剂的优化条件下,解吸收率大于90％、阿维菌素中B1a含量大于91％、总收率大于65％。该阿维菌素分离纯化方法工艺简单。分离效果好,适于工业化生产。     

Preliminary separation and purification of rutin and quercetin from Euonymus alatus (Thunb.) Siebold extracts by macroporous resins

In this study, the performances of rutin and quercetin from Euonymus alatus (Thunb.) Siebold extracts on five macroporous resins with different physical and chemical properties were investigated. The results of static tests indicated that AB-8 resin was the most appropriate and its adsorption data were well fitted to the Langmuir and Freundlich isotherms. In order to optimize the separation process, different pH values of sample solution, different concentrations and pH values of ethanol solution also have been investigated. Column packed with AB-8 resin was used to perform dynamic adsorption and desorption experiments. After the treatment with AB-8 resin and optimal conditions, the contents of rutin and quercetin in the product were 8.45-fold and 13.14-fold increased with recovery yields of 63.1% and 72.3%, respectively. The results showed that the present method was suitable for large-scale preparation of rutin and quercetin from Euonymus alatus (Thunb.) Siebold or other herbal materials.     

氨基改性苯乙烯树脂的合成及其对铼的吸附

离子交换法因适于低浓度物质的分离富集而被广泛应用于湿法冶金行业,新型高效吸附材料的合成与应用成为该领域的发展趋势。针对铀矿中伴生铼这一稀缺资源需要同步回收的现状,根据新近研发的氨基改性苯乙烯阴离子交换树脂(LSC-Re),通过静态和动态吸附解吸试验,系统考察了溶液酸度、初始浓度、吸附时间、吸附温度等因素对吸附性能的影响,结果表明：在室温(25℃)下,铼溶液初始浓度为100 mg·L^-1,该树脂6 h达到吸附平衡,酸度对该树脂吸附铼的影响不大,树脂在pH=1.5时铀铼分离效果最佳,分离系数可达到41.68;树脂的饱和吸附容量达到129.3 mg·g^-1;从热力学和动力学角度分析,吸附过程符合Langmuir吸附等温模型和准二级动力学模型,且吸附是自发的吸热过程。动态吸附解吸试验中,控制溶液流速0.5 ml·min^-1,动态饱和吸附容量达到76.17 g·L^-1,饱穿比为2.35,用1 mol·L^-1 氨水进行解吸铼效果较好,8个树脂床体积可将其解吸完全,由此可见富集倍数接近70倍,具有良好的工业应用前景。     

蛹虫草菌深层液体发酵耦合大孔树脂吸附高效生产虫草素

虫草素是一种核苷类抗生素,具有抗癌、抗肿瘤等活性,主要由蛹虫草菌液体发酵生产,然而低产量限制了其应用。考虑到高浓度虫草素积累对其生物合成过程产生强烈反馈抑制,提出了应用发酵分离耦合技术移除部分虫草素、弱化反馈抑制作用以提高虫草素产量的策略。通过静态吸附实验,筛选出虫草素吸附和解吸性能良好的大孔树脂NKA-Ⅱ,并优化了大孔树脂使用量（60 g·L^-1）、吸附温度（37℃）和解吸剂种类（100%乙醇）。在30 g·L^-1葡萄糖的分批发酵体系中,经过两次树脂吸附,发酵21 d后虫草素产量达到644.50 mg·L^-1,较对照组提高32.07%;随后,将树脂吸附分离策略应用于补料分批发酵体系,虫草素产量达到787.50 mg·L^-1,较对照组提高35.78%。这些结果表明,将虫草素液体发酵与大孔树脂吸附分离耦合,有效弱化了虫草素反馈抑制,显著提高虫草素产量,为虫草素高效生产分离提供了新思路。     

Preparation of high purity squalene from soybean oil deodorizer distillate with the combination of macroporous resin and thin-film evaporation coupling distillation

ABSTRACT

In this study, the combination of macroporous adsorbent resins (MARs) and thin-film evaporation coupling distillation (TFECD) was studied systematically, with aim to obtain high value-added squalene from soybean oil deodorizer distillate (SODD). Five types of resins (X-5, D-101, D4020, DM301, and AB-8) were first used to evaluate the adsorption/desorption properties of squalene. D101 resin exhibited higher adsorption/desorption capacities and desorption ratios for squalene based on static adsorption results among the tested resins. We further investigated the adsorption kinetics, isotherms, and thermodynamics with D101 resin as adsorbent. The adsorption of squalene on D101 was best fitted to pseudo-second-order kinetic model and the Langmuir equation. The dynamic adsorption and desorption indicated that similar results were observed in the static adsorption test. The purity of squalene was increased from 7.5 to 82.5% with the recovery up to 88.5% after separation on D101 column. The resin-refined sample was directly subjected to TFECD purification. Under optimized process parameters, the final product with purity of 98.5% and recovery yield of 76.5% was confirmed by high-performance liquid chromatography (HPLC) analysis. The present study provided an effective method for large-scale production of high purity squalene.     

Separation of gibberellic acid (GA3) by macroporous adsorption resins

Adsorption rates of gibberellic acid (GA3) on S‐8 and X‐5 resins were measured with the results indicating that the adsorption attained equilibrium for adsorption times longer than 4 h. The adsorption isotherms of GA3 on AB‐8, X‐5, S‐8, D4020, D3520, D4006 and NKA‐9 were determined at 20 °C. S‐8 resin had the largest solid/liquid distribution coefficient of 10.5 and was selected as the adsorbent for separation of GA3 from the aqueous solution. The breakthrough curves of GA3 from the aqueous solution on S‐8 resin were determined at different flow rates. The dynamic adsorption capacity of GA3 was measured as 4.56 mgg⁻¹ wet resin at a flow rate of 0.5 cm³min⁻¹. GA3 adsorbed on S‐8 resin was eluted with several eluents with 80% (v%) acetone aqueous solution having the best desorption performance. When GA3 was adsorbed by S‐8 resin from the fermentation liquor, the dynamic adsorption capacity of GA3 was increased to 12.02 mgg⁻¹ wet resin in virtue of the salting‐out effect of the ammonium sulfate in the fermentation liquor. The yield of GA3 was above 90% after GA3 was adsorbed by S‐8 resin from the fermentation liquor at pH 2 and eluted by 80% (v%) acetone aqueous solution. The GA3 concentration was increased seven‐fold from the fermentation liquor after an adsorption and desorption cycle. © 2000 Society of Chemical Industry     

EFFECT OF pH AND IONIC STRENGTH ON COMPETITIVE ADSORPTION OF ERYTHROMYCIN A AND C ONTO MACROPOROUS RESIN SEPABEAD SP825 AT DIFFERENT TEMPERATURES

Equilibrium adsorption experiments were carried out to investigate the effect of pH and ionic strength on competitive adsorption of erythromycin A (EA) and C (EC) in aqueous solution onto macroporous resin, Sepabead SP825, at different temperatures. The equilibrium data for the binary system were analyzed using the extended Langmuir isotherm, and the characteristic parameters were determined. The maximum adsorption capacities for both EA and EC were obtained at pH 8.5, ionic strength 0.4 mol · L^?1 NaCl, and 303 K. Selectivity of Sepabead SP825 for EA and EC was also studied. The results suggested that EA was preferred over EC, and the increase of ionic strength and temperature in neutral solution was to the benefit of the separation of EA and EC.     

Separation of glycyrrhizic acid from licorice root extract using macroporous resin

Glycyrrhizic acid (GA) is the major active ingredient of licorice which has many pharmacological activities. In the present study, separation of GA from licorice root extract has been carried out by adsorption on five different macroporous resins. Static and dynamic adsorption of GA from crude licorice root extract is studied on ion exchange resins followed by desorption. Indion 810 shows the maximum adsorption as well as desorption capacity. The adsorption experiments indicate that equilibrium can be achieved in 360 min. The adsorption equilibrium data is well fitted in the Langmuir isotherm. The separation process is optimized by investigating the effect of pH on adsorption capacity and effect of concentration of ethanol on desorption capacity. The dynamic adsorption is carried out in a column packed with Indion 810 resin and effect of feed flow rate and initial concentration of GA in extract has been studied. The results showed that increase in feed flow rate as well as initial feed concentration of GA lowers the dynamic binding capacity and mass transfer coefficient while increases the HETP. The purity of GA is increased from 14.3% to 71.5% by the dynamic desorption with 60% ethanol. Indion 810 resin can efficiently separate GA from licorice root extract with the HPLC recovery of 63.6%. This study forms the basis for large scale preparation of GA by resin adsorption.     

H103大孔吸附树脂分离纯化苦参碱与氧化苦参碱的研究

通过对比苦参总碱在九种大孔树脂上的静态吸附,筛选出对苦参总碱吸附能力较强的H103树脂;研究了H103树脂对上述两种生物碱的吸附等温曲线及吸附动力学行为;考察了苦参总碱在H103树脂上的动态吸脱附过程,用薄层色谱法(TLC)对洗脱液跟踪分析,用高效液相色谱法(HPLC)检测苦参碱、氧化苦参碱含量,确定了动态吸脱附的过程参数。结果表明,H103树脂对苦参总碱的等温吸附可采用Freundlich方程描述;由吸附动力学曲线得H103树脂在100 min内达到平衡,具有较快吸附速度,吸附动力学规律可用二级速率方程表示;动态吸脱附过程的洗脱条件为：用30%乙醇-25%氨水（115:1,v/v）,80%乙醇梯度洗脱,氧化苦参碱先被洗脱,苦参碱随后,两种生物碱可达到很好的分离,经计算苦参碱收率为90.1%,氧化苦参碱收率为85.3%。     

Preparative Enrichment and Separation of Glycyrrhetinic Acid Monoglucuronide from Fermentation Broths with Macroporous Resins

Preparative enrichment and separation of Glycyrrhetinic acid monoglucuronide (GAMG) from the pretreated fermentation broth of glycyrrhizin was studied by using six macroporous resins with different physical and chemical properties. D101 resin showed the maximum effectiveness among the tested resins. The solute affinity towards D101 resin at different temperatures was described in terms of Langmuir and Freundlich isotherms, and the equilibrium experimental data were well-fitted to the two isotherms. The dynamic adsorption and desorption tests were carried out in order to optimize the operational parameters for the efficient separation of GAMG. After one run treatment with D101 resin, the contents of GAMG in the product were increased to 8.2-fold with recovery yields of 93.3%. The process achieved easy and effective enrichment and separation of GAMG with D101 resin, and it could be applied for the large-scale preparation of GAMG from the fermentation broth of glycyrrhizin.     

Dowex50W-X树脂吸附硫酸溶液中的锶

In this study,strontium adsorption from sulfuric acid solution by different Dowex 50W-X ion exchange resins was investigated.Among these resins,Dowex 50W-X8 resin showed the maximum sorption of strontium from the aqueous solutions.The effect of pH,contact time,mass of resin,temperature,and concentration of interfering ions on strontium adsorption were evaluated to determine the optimum conditions of strontium sorption process.The kinetic models of sorption were analyzed using pseudo-first and pseudo-second order models.The results indicated that the pseudo-second order kinetic model was more appropriate than the other one.Moreover,the data obtained in this study were fitted into several sorption isotherm models and it was found that the Langmuir sorption isotherm shows the best fitting to the experimental data.     

基于离子交换层析技术提取发酵液中的丙酸

用7种不同性能的阴离子交换树脂吸附发酵液中丙酸,考察了发酵液酸化方式及pH值对吸附量的影响,分析了不同浓度H2SO4的解吸情况,比较了多柱串联组合层析提高丙酸收率的可行性. 结果表明,大孔弱碱性丙烯酸系阴离子交换树脂ZGD630对发酵液中的丙酸吸附量最高,采用H型阳离子交换树脂D001酸化工艺,当pH值由6.5降至3时,ZGD630树脂对发酵液中丙酸的静态吸附量从54.34 mg/g提高至110 mg/g,动态吸附量达152.5 mg/g. 用4 mol/L H2SO4进行解吸,丙酸浓度最高达81.8 g/L,为初始发酵液的2.12倍. 采用3柱串联组合层析时丙酸收率达62.15%,较单柱层析显著提高.