大孔树脂分离纯化枸杞多糖的研究

本文采用大孔吸附树脂分离纯化枸杞多糖的粗提取液,其中,大孔树脂HPD300对枸杞多糖的吸附容量最大可达343.71 mg/g,吸附平衡时间为180 min,HPD300对枸杞多糖的吸附过程符合Freundlich等温吸附方程,为多分子层吸附。大孔吸附树脂HPD300吸附分离工艺可以重复利用,树脂经过分连续5轮离纯化后,其再生效率可达85.09%,多糖回收率87.47%。     

D-101大孔树脂吸附薯蓣水溶性皂苷的热力学和动力学分析

实验考察了薯蓣水溶性皂苷在D-101大孔树脂上的吸附特征,确定了等温吸附模型、热力学参数和吸附动力学模型。结论:可用Langmuir方程较好地拟合等温吸附热力学过程,吸附是一个自发、放热、快速的物理吸附过程,可用拟二级动力学方程较好地描述吸附动力学过程,在180 min左右达到吸附平衡。D-101大孔树脂廉价并且适合薯蓣水溶性皂苷的吸附生产。文章为D-101大孔树脂从薯蓣提取物及皂素生产发酵工段废水中富集纯化水溶性皂苷的扩大应用提供数据参考。     

大孔吸附树脂纯化化香树果序总黄酮工艺研究

以吸附量和解吸率为指标对9种大孔吸附树脂进行对比,H-327B是分离纯化化香树总黄酮的理想树脂;热力学、动力学研究表明,Langmuir模型描述化香树果序黄酮在大孔树脂上的吸附规律更为适宜,该吸附属单分子层吸附,提高温度有利于吸附的进行,吸附过程可自发进行;对吸附?解吸工艺条件优化研究表明:当上样质量浓度为8.9 mg/mL、流速为3 BV/h时,H-327B型树脂对化香树果序总黄酮的吸附量较大。采用体积分数90%乙醇水溶液进行洗脱时,用5 BV乙醇洗脱,解吸率达到65%。     

HPD型树脂纯化肉桂枝叶非挥发部分多酚的工艺研究

本文研究了HPD型树脂富集纯化肉桂枝叶非挥发部分多酚的最佳工艺。以提取桂油后的肉桂枝叶残渣为原料,采用比色法测定其多酚含量。以吸附率和解析率为指标,采用静态吸附实验,比较了6种HPD型树脂的吸附与解吸性能,优选出最佳树脂并进行动态吸附和解吸实验,以确定最佳工艺条件。实验结果表明,HPD100树脂对肉桂残渣多酚具有良好的吸附和解吸效果,最佳工艺条件为:上样量60 mg·g~(-1),上样浓度3.0 mg·mL~(-1),上样pH=4.0,吸附时间3h,洗脱剂为60%乙醇。动态实验中,先用6BV的水洗至挥干无固体,再以4BV的60%乙醇以3 BV·h~(-1)的流速洗脱,洗脱液中的多酚含量达46.2%。放大实验中,多酚含量达45.6%,纯化后得红棕色黏稠状固体,出膏率为79.5%。     

树莓叶片黄酮成分分离纯化研究

为纯化树莓叶片黄酮成分,比较了7种树脂静态吸附和解吸过程,筛选出合适的大孔树脂初步纯化树莓叶片总黄酮,优化了吸附和解吸条件.结果表明:AB-8大孔树脂对树莓叶片总黄酮有较好的吸附和解吸性能,其最佳工艺为上样液pH=6.0、流速2.0 mL·min-1,洗脱剂乙醇最适宜浓度为70％,流速1.5 mL·min-1,经AB-...     

大孔树脂对龙脷叶总黄酮的纯化工艺及其吸附特性研究

通过静态、动态吸附,解吸实验考察大孔吸附树脂D101、AB-8、HPD100、HPD600、DM301、NKA9对龙脷叶总黄酮的纯化效果,分析大孔树脂吸附机制。结果表明,AB-8树脂对龙脷叶总黄酮具有较强的纯化能力,吸附动力学符合准二级动力学模型,等温吸附数据符合Freundlich模型。最佳上样液pH为5,上样质量浓度为0.167 mg/mL,1.5 BV样品溶液以1 mL/min的流速上样,充分吸附后用4 BV纯净水洗去杂质后,用4 BV 50%乙醇溶液以2 mL/min的流速洗脱;总黄酮的保留率达98.42%,纯度提高了3.06倍。     

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%。     

H103大孔吸附树脂分离纯化苦参碱与氧化苦参碱

通过对比苦参总碱在9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:用体积分数30%乙醇-体积分数25%氨水(体积比115∶1),体积分数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%。     

AB-8树脂吸附富集玉屏风复方中黄芪皂苷类成分

研究了黄芪皂苷在AB-8大孔树脂上的吸附等温线(20℃,30℃,40℃)及吸附动力学(30℃),考察了操作条件对黄芪皂苷在AB-8固定床上的穿透曲线及洗脱曲线的影响,在此基础上研究了AB-8固定床对玉屏风复方中黄芪皂苷类成分的富集效果.实验结果表明,黄芪皂苷在AB-8树脂上的等温吸附可用Langmuir及Freundlich 等温吸附方程描述,吸附前期吸附动力学行为基本遵循Bangham速率方程,后期遵循Langmuir速率方程,皂苷的穿透曲线实验数据可用Bohart-Adams模型方程拟合,拟合公式可用于给定操作条件下皂苷穿透时间的计算.玉屏风复方提取物中皂苷经AB-8树脂床吸附分离后,皂苷含量由2.57%提高到39.27%,回收率为83.71%,提取物中皂苷得到有效富集.研究结果可为玉屏风复方黄芪皂苷类成分的富集提供借鉴.     

H1020树脂吸附糖精的动力学和热力学研究

研究了大孔树脂H1020对糖精（邻苯甲酰磺酰亚胺）的吸附性能。在温度为303.15、308.15、313.15和318.15 K条件下分别测定了吸附平衡数据。分别采用了拟一级动力学模型和拟二级动力学模型对实验数据进行模拟,结果表明拟二级动力学方程更适合描述H1020型大孔树脂对糖精的吸附过程。用Langmuir和Freundlich吸附等温方程对实验数据进行拟合,结果表明糖精在大孔树脂H1020上的吸附平衡符合Freundlich吸附等温方程。计算糖精吸附过程的吸附焓变、吸附自由能和吸附熵变,根据吸附热力学值可判断出H1020型大孔树脂对糖精的吸附过程是自发的、放热的物理吸附。     

Preparative Separation of Glabridin from Glycyrrhiza glabra L. Extracts with Macroporous Resins

Abstract

In the present study, the performance and adsorption characteristics of five macroporous resins for the separation of glabridin from Glycyrrhiza glabra L. have been evaluated. The adsorption and desorption properties of glabridin on macroporous resins including HPD100, HPD300, HPD800, NKA and H103 were compared. HPD100 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 resins at different initial concentrations. Dynamic adsorption and desorption experiments on HPD100 resin packed column were conducted to optimize the separation process of glabridin from licorice extracts. After the treatment with stepwise elution on HPD100 resin, the content of glabridin in the product increased from 0.21% to 32.2% which is 153-fold higher than it in G. glabra L. roots and the recovery yield was 79.7%. The results indicated the good ability of HPD100 resin for separation glabridin and the study may provide scientific references for the large-scale glabridin production from G. glabra L. or other plants extracts.     

Enrichment and Purification of Syringin, Eleutheroside E and Isofraxidin from Acanthopanax senticosus by Macroporous Resin

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol-water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively.     

5种大孔吸附树脂对沙棘叶黄酮苷元的静态吸附/解吸附性能

以槲皮素、山奈酚和异鼠李素的静态吸附率/解吸附率为评价指标,考察了HPD600、YWD01G3、YWD01F、07C、AB-8 5种大孔吸附树脂对沙棘叶黄酮苷元的吸附/解吸附性能。实验结果表明:非极性树脂YWD01G3在吸附/解吸附方面显示出最佳的综合性能,对槲皮素、山奈酚、异鼠李素的平均吸附率和解吸附率分别为90.81%和59.51%。该实验为初步确定沙棘叶黄酮纯化用大孔树脂和进一步研究其动态吸附/解吸附提供了依据。该工作经中国科学院兰州查新咨询中心2006年3月28日出具的第2006033101号《科技查新报告》证实,未见相同文献报道。     

大孔吸附树脂对沙棘叶总黄酮的吸附性能考察

以吸附值(mg/g)和解吸附率(%)为评价指标,通过静态吸附/解吸附分别考察LSA-40、LSA-21、DM-130、HPD450、D101和XDA-1六种大孔吸附树脂对沙棘叶总黄酮的吸附/解吸附性能。通过动态吸附/解吸附优选沙棘叶总黄酮最佳分离工艺条件。结果表明中极性树脂LSA-21在吸附/解吸附方面显示出最佳的综合性能,对沙棘叶总黄酮的静态吸附值/解吸附率分别为131.78mg/g和55.53%,经静态和动态吸附后得到的总黄酮纯度分别为19.4%和20.3%。     

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%。     

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.     

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.     

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。     

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.     

大孔吸附树脂对葛根总黄酮吸附性能的研究

测定分析了AB-8等6种不同极性大孔吸附树脂对葛根总黄酮的吸附特性。静态实验结果表明,树脂的极性和空间结构是影响吸附效果的重要因素。AB-8树脂孔径适当,比表面积较高,葛根黄酮吸附量达74.3 mg/g。进行了静态吸附动力学的研究,并获得总黄酮吸附量与吸附时间之间的定量关系。动态吸附研究表明,在温度为20℃时,以吸附流速4 mL/min和洗脱流速3 mL/min较合适。而重复使用约10次以后,该树脂应进行再生。