大孔吸附树脂分离纯化追风伞总黄酮的研究

以总黄酮的吸附量、回收率及解吸率为考察指标,研究了大孔吸附树脂分离纯化追风伞总黄酮的工艺条件。通过静态吸附实验比较了7种不同类型大孔吸附树脂的吸附特性,确定了D101型大孔吸附树脂用于追风伞总黄酮的纯化富集。通过动态吸附实验,确定了D101型大孔吸附树脂分离纯化追风伞总黄酮的最佳工艺条件为:上样液浓度1.839 mg.mL-1,上样流速为2.0 mL.min-1,洗脱剂为70%乙醇,洗脱剂用量为6 BV。在此条件下,D101型大孔吸附树脂对追风伞总黄酮的动态饱和吸附量为80.05 mg.g-1,纯化后追风伞总黄酮的纯度达到86.2%。D101型大孔吸附树脂可以较好地分离纯化追风伞总黄酮。     

大孔树脂对喹乐霉素的静态吸附

考察了9种不同极性的大孔树脂对喹乐霉素的静态吸附解吸效果,探讨了吸附过程中树脂静态吸附动力学和25℃时的等温吸附过程,并用Langmuir与Freundlich方程分别对吸附过程进行了拟合。结果表明,XAD-16和D101树脂对喹乐霉素的吸附解吸效果较好,比较两种树脂等温吸附的Langmuir和Freundlich参数,D101树脂对喹乐霉素的吸附解吸作用最好,吸附量最大,达到0.976 mg/g干树脂,吸附过程更易发生。因此,D101树脂更适用于从标桩菌WXNXJ-B发酵液中吸附并解吸喹乐霉素。     

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)。     

离子交换树脂对白扦中莽草酸的分离纯化

建立了离子交换树脂分离纯化白扦中莽草酸的工艺条件和参数。通过研究D261、D296、D301-R、D301-G、D290、201*7(717)、D201和D280共8种离子交换树脂对莽草酸的吸附和解吸附能力,筛选出最佳树脂为D290,确定了最佳的吸附与解吸附工艺参数,吸附条件为pH=6、25 ℃、流速为3 mL/min;脱附条件为：洗脱液为2.5%NaOH水溶液,洗脱流速为3 mL/min。莽草酸样品溶液经D290树脂吸附与脱附后回收率为92.53%,纯度由2.97%提高到46.76%,提高了15.74倍。实验结果表明,D290树脂对莽草酸的吸附量大,脱附容易,可以应用于莽草酸的分离纯化。     

大孔树脂纯化栾树叶多酚工艺研究

以栾树叶多酚提取物为原料,比较了7种大孔树脂对栾树叶多酚的静态吸附与解吸效果,结果表明AB-8树脂性能最佳,其24h静态吸附量为13.74mg/g,解吸率为98.35%,3h内达到吸附平衡与解吸平衡。AB-8树脂动态吸附较佳条件为上样液质量浓度为4g/L,上样液pH值为6,在此条件下吸附率为88.21%,动态洗脱较佳条件为洗脱剂乙醇体积分数为60%,洗脱速度为1mL/min,解吸率达到89.91%,在该条件下栾树叶总多酚经AB-8树脂纯化后,质量分数由50.36%增加到72.37%,回收率为86.83%。     

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.     

Separation of sinigrin from Indian mustard (<Emphasis Type="Italic">Brassica juncea</Emphasis> L.) seed using macroporous ion-exchange resin

Sinigrin is a major glucosinolate present in Indian mustard (Brassica juncea L.) seeds as the precursor of the anticancer compound allyl isothiocyanate. In the present study, the adsorption and desorption characteristics of six macroporous ion-exchange resins for the separation of sinigrin from crude aqueous extracts have been compared. The results indicated that D261 resin showed the best adsorption and desorption capacity to sinigrin, and its adsorption data fit best to the Freundlich isotherm. The dynamic adsorption/desorption experiments were carried out to optimize the separation process. After treatment with D261 resin in one run, the purity of sinigrin in the product was increased 15.57-fold from 3.75% to 58.37% with the recovery of 79.82%. Meanwhile, the separation effect of D261 resin was also supported by UV and IR. The separation process using macroporous ion-exchange resin in our paper provides a novel, rapid and economical method for separation of sinigrin.     

大孔吸附树脂纯化石榴皮多酚

从D3520、D4020、AB-8、D140、D141、D160、DM-301、DA-201、SAD-7和D101大孔吸附树脂中筛选出D141树脂,研究了其对石榴皮多酚的静态与动态吸附和解吸性能。结果表明,D141树脂对石榴皮多酚的饱和吸附量为19.86 mg/g(干树脂),吸附等温线符合Langmuir方程,饱和吸附时间为5 h,适宜解吸剂为体积分数70%的乙醇溶液;以质量浓度9 mg/mL的石榴皮提取液上柱,流速为1.8~2.0 BV/h时,树脂的多酚穿透吸附容量为39.42 mg/g(干树脂),2.5 BV体积分数70%的乙醇溶液可将吸附于柱上的石榴皮多酚完全洗脱。以该条件纯化石榴皮多酚提取物时,纯化样的收率为15.4 g/100 g(石榴皮),多酚质量分数从34%提高到76.34%。     

大孔树脂吸附纯化葡萄籽原花青素的研究

采用大孔树脂对葡萄籽原花青素进行吸附纯化,以吸附率和解吸率及纯化效果为指标,比较了7种大孔树脂对原花青素的吸附解吸性能。研究了上样量、洗脱剂浓度、上样流速、洗脱剂用量对原花青素纯化效果的影响。结果表明,AB-8大孔树脂对葡萄籽中原花青素的吸附效果最好,树脂体积为20 mL,上样量为80 mL,上样流速为40 mL/h,用40%的乙醇洗脱,洗脱剂用量为100 mL,洗脱流速为80 mL/h时的纯化效果最好,该条件下原花青素洗脱率为94.37%,所得溶质纯度可达89.63%。     

大孔吸附树脂分离纯化杜仲中京尼平甙酸

比较了NKA-9、D311、S-8、HPD600、NKA-2、A型、D140、聚酰胺8种树脂对杜仲中的降血压活性成分京尼平甙酸(GPA)的吸附及脱附性能,从中筛选出吸附率(88.17%)及脱附率(97.71%)均较高的A型树脂进行实验。最佳工艺条件为:杜仲皮粉末用φ(乙醇)=50%的水溶液提取后,乙醇沉淀,上清液调节pH=6~9后,用A型树脂吸附220 m in,装柱,用φ(乙醇)=15%的水溶液洗脱,流速为1.5 mL/m in,洗脱液浓缩后,冷冻干燥得产品。京尼平甙酸的收率为84.03%,w(GPA)=84.06%。     

不同大孔树脂吸附-解吸附喜树黄酮性能的研究

采用静态吸附和解吸方法研究了AB-8、D-101、X-5、H-103、YWD-03五种大孔树脂对喜树叶黄酮的吸附与解吸性能,结果表明,AB-8树脂对喜树叶黄酮的吸附分离综合性能最佳,中性条件下其静态吸附率为85.54%,最大解吸率高达98.75%以上。     

双官能基修饰的超高交联吸附树脂对2,4-二氯苯酚的吸附性能研究

合成了用2-氨基酚修饰的新型双官能基聚苯乙烯-二乙烯苯吸附树脂MOAPR-1和MOAPR-2,研究了其在288~318 K下对水溶液中2,4-二氯苯酚的静态吸附和静态脱附特征。结果表明,2,4-二氯苯酚在两种树脂上存在化学吸附现象,符合Freundlich等温吸附方程。利用半经验分子轨道法计算了几种吸附剂的近似结构和2,4-二氯苯酚的前线轨道能级,并对吸附过程进行了合理的解释。     

大孔吸附树脂精制鱼腥草黄酮类化合物

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.     

大孔树脂对甘草酸的吸附纯化

从3种树脂中选择了D-101树脂为纯化甘草酸的最佳树脂。考察了各种因素对D-101树脂吸附和洗脱甘草酸的影响。实验结果获得吸附最佳条件为：上样液pH值6-8,甘草酸浓度5．710mg／mL,流速为1mL／min;洗脱最佳条件为：乙醇洗脱剂浓度50％和洗脱液流速1mL／min。洗脱产物甘草酸纯度最高达82．38％。     

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%。     

Preparative enrichment and purification of nevadensin from Lysionotus pauciflorus using macroporous resins

An efficient method using macroporous adsorption resins for preparative enrichment and purification of nevadensin from Lysionotus pauciflorus Maxim was developed. The results indicated that non-polar HPD-100 resin offered the best adsorption and desorption performance, its adsorption data were well-fitted to the Freundlich isotherm and the pseudo-second-order kinetics model. Dynamic adsorption and desorption experiments have been investigated for optimization of chromatographic parameters. Through one cycle of dynamic adsorption/desorption, the purity of nevadensin in the extract, increased about 8.82-fold from 8.58% to 75.70%, with a recovery yield of 69.90%. The results suggested that HPD-100 resin can separate nevadensin effectively from plant material.     

大孔树脂富集多舌飞蓬总咖啡酸酯的工艺研究

摘要：考察了13种不同极性的大孔树脂对多舌飞蓬中总咖啡酸酯的富集纯化能力,发现极性树脂NKA-2的静态吸附率为92.51%、解吸率为98.51%,明显优于其他树脂。进一步以NKA-2极性树脂对多舌飞蓬总咖啡酸酯进行静态吸附与动态吸附实验,结果表明,最佳上样质量浓度为300 g/L,最佳上样流速为2 BV/h,树脂吸附容量为6 mL/g,即单位NKA-2树脂可以处理1.8 g生药。解吸实验结果表明,体积分数为60 %的乙醇溶液更有利于多舌飞蓬总咖啡酸酯的洗脱,用量为8 BV。用上述条件对多舌飞蓬总咖啡酸酯富集纯化,使总咖啡酸酯的纯度由18.09 %提高到58.06 %,回收率高达94.78 %。说明NKA-2型大孔吸附树脂综合性能良好,可用于多舌飞蓬中总咖啡酸酯成分的富集和纯化。     

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 from 3-5 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 of 80% 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.     

大孔树脂纯化废次烟叶中烟草多酚的工艺

通过吸附和解吸附实验,从6种大孔树脂中筛选出适于分离纯化废次烟叶中烟草多酚的大孔树脂,并确定该大孔树脂纯化工艺参数。结果显示,D101大孔树脂能够较好的富集纯化废次烟叶中的烟草多酚,当提取液浓度为2.5 mg/mL,pH值为4.0,上样液流速为2.0 mL/min,洗脱液为80%乙醇溶液,洗脱液流速为2.0 mL/min时,纯化效果最好,烟草多酚的动态回收率为70.37%。     

Adsorption of anionic textile dye Acid Green 9 from aqueous solution onto weak or strong base anion exchangers

The aim of this work is to study the thermodynamic and kinetic studies with regard to the adsorption of Acid Green 9 (AG9) on the most efficient resin, namely, acrylic weak base anion exchange resin with ethylenediamine‐functional groups (A1) selected from several anion exchange resins. The influence of the various experimental parameters such as, pH, initial dye concentration, contact time, temperature, and adsorbent dose was investigated by batch experiments. The extent of the dye adsorption increased with the decrease of the initial dye concentration and the increase of the contact time, temperature, and amount of the adsorbent. Adsorption process was quantitative and very fast at low concentrations of the dye. To investigate the mechanism of the adsorption and potential rate‐controlling steps, pseudo first‐ and second‐order, as well as intraparticle diffusion kinetic equations have been used. The adsorption kinetic of AG9 dye from aqueous solution onto A1 could be described by the pseudo second‐order reaction model. The obtained results are in agreement with the Langmuir and Freundlich models. In the optimum conditions established, an adsorption capacity of 500 mg textile dye (72% purity) g^?1 adsorbent (at 293 K) was reached. Desorption experiments by batch and dynamic methods were performed using a solution of 0.05 mol L^?1 NaOH. A series of 13 adsorption–desorption cycles were carried out by the dynamic method with a quantitative adsorption and the desorption efficiency higher than 95%. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009