Separation of chlorogenic acid from honeysuckle crude extracts by macroporous resins

Chlorogenic acid, one of the most bioactive compounds rich in the Chinese medicinal herb honeysuckle, is a natural antioxidant and serves as anti-inflammatory, anti-tumor, anti-mutagenic and anti-carcinogenic agent. An efficient preparative separation process of chlorogenic acid from honeysuckle crude extracts has been developed in the present study. HPD-850 resin offers the best adsorption capacity, and adsorption and desorption ratios for chlorogenic acid among the nine macroporous resins tested, and its adsorption rate at 25 degrees C fit best to the Langmuir isotherm. The adsorption capacity of HPD-850 resin was found to depend strongly on the pH value of the initial adsorption solution. The dynamic adsorption and desorption experiments have been carried out on a HPD-850 resin packed column to optimize the separation process of chlorogenic acid from honeysuckle crude extracts. After one run treatment with HPD-850 resin, the chlorogenic acid content in the final product was increased 4.46-fold from 11.2% to 50.0%, with a recovery yield of 87.9%. The preparative separation of chlorogenic acid can be easily and efficiently achieved via adsorption and desorption on HPD-850 resin, and the method developed will provide a potential approach for large-scale separation and purification of chlorogenic acid for its wide pharmaceutical use.     

大孔吸附树脂分离虎杖中白藜芦醇的研究

目的:采用大孔吸附树脂对虎杖粗提物中白藜芦醇进行初步富集、分离和纯化.方法:考察18种树脂对白藜芦醇的吸附量和解吸率,选择吸附量大、解吸率高的数种树脂进行吸附动力学研究,确定最佳的脱附工艺.结论:HPD-500树脂对白藜芦醇的吸附量可达58.67mg/g,解吸率为92.6%,经大孔吸附树脂的吸附与解吸,白藜芦醇的含量由粗提物中9.25%提高至39.5%.     

大孔吸附树脂纯化海红果黄酮工艺的研究

通过采用大孔吸附树脂对海红果黄酮粗提液的静态吸附和解吸试验,从10种大孔吸附树脂中筛选出海红果黄酮纯化的最优树脂,考察了该树脂对诲红果黄酮的静态、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:NKA-9树脂对海红果黄酮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pH值为4.0,浓度5.15 mg/mL,上样量为4 BV,流速控制在2 BV/h.最优的解吸工艺条件为:洗脱剂为80％乙醇溶液,洗脱液用量为3 BV,洗脱流速控制在1 BV/h.在此优化条件下,海红果黄酮的吸附率、解析率、收率、纯度的平均值分别达到为(79.39±0.13)％,(84.14±0.11)％,(68.20±0.15)％和(28.81 ±0.06)％ (n=5).     

大孔树脂纯化岩高兰多酚的工艺研究

为获得大孔树脂纯化岩高兰多酚的最佳工艺,以岩高兰的地上部分为原料,通过考察6种不同类型树脂(HPD-100、X-5、AB-8、D101、HPD-600、NKA-II)的含水率、吸附率和解吸率的大小,筛选出一种最适合纯化岩高兰多酚的树脂。在此基础上,选择对纯化工艺影响较大的4种因素(上样浓度、乙醇浓度、洗脱流速、洗脱体积),进行响应面法分析得到最佳工艺。结果表明:HPD-600型大孔树脂对岩高兰多酚的纯化效果最佳,其最优工艺参数为:上样浓度0.84 mg·mL^-1;乙醇浓度62.15%;洗脱流速0.67 mL·min^-1;洗脱体积2.71 BV。该条件下,岩高兰多酚的提取率为229.18 mg·g^-1,岩高兰多酚的纯度由8.11%提高到22.56%,回收率为67.78%。本研究为岩高兰多酚的纯化工艺提供了新的技术路线,也可为岩高兰提取物的研究和应用提供参考。     

Enhancement of the isolation selectivity of isoflavonoid puerarin using oligo-β-cyclodextrin coupled polystyrene-based media

The isolation selectivity of the isoflavonoid puerarin, a well-known traditional Chinese medicine, was studied when native and oligo-β-cyclodextrin (CDP) coupled polystyrene-based macroporous resins were used as adsorbents by static tests. The research results indicated that the CDP coupled resin HPD-100-CDP offered the best adsorption and desorption capacity for puerarin than others and its equilibrium adsorption data at 25 °C fit best to the Freundlich isotherm. The performance of separation of puerarin on HPD-100-CDP column in one step was evaluated. Based on the above experimental data, a novel medium PS-CDP was synthesized and its chromatographic retention behaviors were also explored. ESI-MS/MS, ¹H NMR spectroscopy and UV absorption spectrum were used for the detection and characterization of puerarin in isolated fraction. Under the optimum mobile phase, methanol/acetic acid/water = 5.0/6.6/88.4 (v/v/v), the purity and recovery of puerarin were 95.3% and 86.7%, respectively, by HPLC analysis. In conclusion, the PS-CDP medium can enhance the isolated selectivity of puerarin and it can be applied in preparative scale operations.     

油橄榄叶中橄榄苦苷的分离纯化

考察了6种不同大孔树脂对橄榄苦苷的吸附,筛选出吸附选择性好的D101大孔吸附树脂为实验材料.得到的D101大孔树脂的最佳吸附条件:试样上样质量浓度41.06[J].,流速5 mL/min,50％乙醇溶液洗脱,洗脱液用量260mL,树脂可以反复使用.经大孔树脂富集后,橄榄苦苷的纯度可达55％以上,再经葡聚糖凝胶精纯化后,可达76％以上.     

大孔吸附树脂分离纯化地黄中梓醇工艺的研究

利用大孔吸附树脂分离提取地黄中梓醇。以地黄粗提液中梓醇含量为指标,高效液相色谱(HPLC)为含量测定方法,考察九种不同极性大孔吸附树脂对梓醇的吸附和解吸附性能,筛选出最佳树脂D101进行分离实验。结果表明,D101大孔吸附树脂的静态吸附容量为69.2mg/g干树脂,其吸附等温线符合Langmuir和Freundlich吸附等温式。采用5%乙醇作为洗脱剂,洗脱液减压浓缩后进行硅胶柱层析分离,氯仿：甲醇（8：2）梯度洗脱得到梓醇单体,纯度达90%以上,梓醇得率为6%。     

Recovery of ganoderic acids from <Emphasis Type="Italic">Ganoderma lucidum</Emphasis> mycelia by macroporous adsorption resins

In this work, the performance and adsorption characteristics of macroporous resins for the recovery and enrichment of ganoderic acid (GA)-Mk and GA-T from Ganoderma lucidum mycelia were systematically evaluated. ADS-8 resin displayed the best adsorption and desorption capacities among the tested resins based on batch experiments. The interaction between solute and ADS-8 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. Thermodynamic analysis indicated the exothermic and spontaneous nature of the adsorption process. The adsorption capacity of ADS-8 resin was found to depend strongly on the pH value of the initial solution. Dynamic adsorption and desorption tests were performed on an ADS-8 resin-packed column to obtain optimal parameters for recovering GA-Mk and GAT from G. lucidum extract. Under optimized conditions, a laboratory scale-up preparation of GA-Mk and GA-T was carried out. The contents of GA-Mk and GA-T were increased from 45 to 22 mg/g in the crude extract to 352 and 141 mg/g in the final product with recovery yields of 90.1 and 72.2%, respectively. These results demonstrated that ADS-8 resin chromatography could act as a useful approach for obtaining ganoderic acids from G. lucidum mycelia.     

大孔树脂分离纯化“黑金刚”紫马铃薯花青苷工艺研究

以紫色马铃薯"黑金刚"花青苷为原料,采用D101、HDP100A、HDP450A、NK-9、AB-8五种大孔吸附树脂对花青苷的吸附与解析特性进行了比较研究,并在此基础上,采用最佳大孔树脂对花青苷纯化过程中的静态、动态吸附和解析附条件进行了优化研究。结果表明AB-8大孔树脂具有较好的吸附和解析能力,是纯化紫色马铃薯花青苷的最佳树脂,较优纯化条件为:上样液花青苷浓度为0.028mg.g-1,上样液pH=2,洗脱液乙醇浓度为50%,洗脱液pH=1,吸附流速为1mL.min-1,洗脱流速为1mL.min-1。经大孔树脂纯化后,色价值比纯化前提高了7.55倍。     

大孔树脂分离纯化辣椒叶总黄酮的工艺研究

目的:筛选适合分离纯化辣椒叶总黄酮的一种大孔树脂,同时用响应面法进行优化得到最佳纯化工艺。方法:采用热回流法提取辣椒叶总黄酮,以吸附率和解吸率为考察指标,考察6种不同型号的大孔树脂(HPD100、HPD450、HPD600、HPD826、D101、AB-8)对辣椒叶总黄酮的吸附能力与解吸能力,确定最佳树脂。通过动态吸附解吸实验考察此树脂对辣椒叶总黄酮的最佳分离纯化工艺。结果:通过对辣椒叶总黄酮吸附分离性能的分析显示HPD600为最佳树脂,最优工艺为:上样浓度为10 mg/mL,上样量为10 mL,洗脱体积为4 BV,洗脱液流速为4 mL/min,洗脱液pH为7,依次用水、10%、30%乙醇冲洗树脂柱,50%乙醇为洗脱液。纯化后的黄酮纯度435.4 mg/g。结论:该方法简便,操作简单,对辣椒叶总黄酮的纯化效果较好。     

大孔吸附树脂对苜蓿皂苷的吸附和解吸附作用(英文)

采用5种不同极性的树脂(AB-8、S-8、NKA-9、D-101和X-5)来评价对苜蓿皂苷的吸附和解吸附作用,其中中等极性的AB-8树脂对苜蓿皂苷具有最大的吸附量,用55%~65%的乙醇溶液能有效地将吸附的皂苷洗脱下来。当苜蓿粗提物量和AB-8树脂量为1∶1时,树脂的吸附量达到饱和。采用AB-8树脂,用90%乙醇洗脱,苜蓿提取物的最大解吸附量为108.4 mg/g干重树脂。通过大孔树脂吸附和解吸附,将90%乙醇洗脱液浓缩,皂苷含量(53%)是苜蓿粗提物含量(5.68%)的9倍。结果表明,AB-8大孔吸附树脂可用于苜蓿皂苷的大规模制备。     

战骨黄酮碳苷类化合物的大孔树脂富集工艺研究

黄酮碳苷,作为战骨植物中的有效成分之一,具有抗骨关节炎的功效.为优化植物战骨茎中总黄酮碳苷的富集纯化工艺,该研究以战骨中5个黄酮碳苷为考察指标,通过对13种大孔树脂的静态吸附与解吸实验,优选出合适的大孔树脂,利用高效液相色谱对结果进行检测,然后利用正交工艺优化富集纯化条件.结果表明:(1)XAD-16N型大孔树脂对植物...     

Preparation of high purity biphenyl cyclooctene lignans from Schisandra extract by ion exchange resin catalytic transformation combined with macroporous resin separation

In this study, ester-bond biphenyl cyclooctene lignans were efficiently hydrolytically degraded into free biphenyl cyclooctene lignans by ion exchange resin transformation and simultaneous removal of impurities by macroporous resin. The OH-type strongly basic anion exchange resin 201×7 was the best one, and the dynamic hydrolysis efficiency was 146.7±5.0%. HPD5000 macroporous resin, which offered higher adsorption and desorption capacities and faster adsorption than other resins. The purity of free biphenyl cyclooctene lignans in the product increased from 5.14±0.24% to 79.67±0.0.67%. After dynamic catalytic transformation by 201×7 resin combined with purification of HPD5000 resin, the yield and the purity of free biphenyl cyclooctene lignans in the product were 132.1±4.7% and 80.91±3.53%, respectively.     

爬山虎红色素的大孔树脂吸附和分离及理化性质研究

本文比较了六种不同型号的大孔树脂对爬山虎红色素的吸附能力,筛选其中最佳的HPD600树脂作为爬山虎红色素的吸附和分离的树脂;用甲醇作为洗脱剂,洗脱效果好;研究了食品中几种常见的共存物、几种金属离子、氧化剂、温度及光等对爬山虎红色素稳定性的影响。     

大孔吸附树脂分离纯化香叶木苷

比较了D-101、D-140、AB-8、XAB-8、D312、聚酰胺等6种吸附树脂对蓬子菜中活性成分香叶木苷diosmin的吸附和洗脱条件,在静态吸附研究的基础上,进行了动态实验,并且利用二次吸附对该成分进行了纯化。结果表明AB-8树脂对diosmin的吸附量大、吸附速度快、解吸容易、富集分离效果好。利用聚酰胺进行二次纯化,得到纯度95%以上的diosmin。     

柴达木沙漠链霉菌S10T阿糖腺苷的大孔树脂分离工艺优化与结构鉴定

为了获得具有药用价值的活性天然产物,采用4种大孔吸附树脂对柴达木沙漠链霉菌（Streptomyces qaidemensis）S10^T发酵液进行静态吸附和解吸实验,优化分离工艺。结果显示,AB-8型树脂具有良好的吸附和解吸性能,该树脂对柴达木沙漠链霉菌S10^T发酵液中的活性天然产物吸附工艺为发酵液pH值9,吸附时间4 h,洗脱液70%甲醇溶液。经正向硅胶、反相硅胶和葡聚糖凝胶Sephadex LH-20分离得到了一个化合物,¹H-NMR和¹³C-NMR结合高分辨质谱（LC-HR-MS）鉴定该化合物为阿糖腺苷（vidarabine）,是一种具有抗病毒活性的核苷类抗生素,并简单探究了其在柴达木沙漠链霉菌中的生物合成过程。     

拮抗链霉菌S24抗菌物质的提取及其部分理化性质

拮抗链霉菌S24对黄曲霉、赭曲霉、黑曲霉等粮食和饲料中常见的曲霉菌具有广谱抗性,本试验通过牛津杯法测定抗菌物质的效价,研究了大孔吸附树脂对链霉菌S24产生的抗菌物质的吸附、解吸性能,筛选了解吸剂,并研究了抗菌物质的部分理化性质。结果表明,大孔吸附树脂AB-8对抗菌物质的吸附及解吸性能最好,其饱和吸附量为7.0822×104μg/g,最佳解吸剂为85%丙酮,以85%丙酮进行动态解吸,解吸率达93.82%。该抗菌物质对热稳定,对紫外线敏感,对有机溶剂不敏感,对酸敏感,对碱稳定,紫外全波长扫描发现该抗菌物质为多烯大环内酯类抗生素。     

杀线虫芽孢杆菌发酵条件优化及大孔树脂筛选

芽孢杆菌 SMrs28分离自草原毒草瑞香狼毒根际土壤,其代谢产物有明显的线虫触杀活性。为了确定该菌株的最优发酵条件及初步纯化活性成分的树脂类型,采用单因素试验对发酵条件进行优化,通过静态吸附试验对大孔树脂类型进行筛选。结果表明: SMrs28菌株的最优发酵条件为:以葡萄糖和酵母粉作为最佳碳源和氮源,发酵时间48 h,接种量10%,温度28 ℃,转速180 r·min^-1,150 mL的三角瓶装液量30 mL,初始pH 7.2。静态吸附试验表明,大孔吸附树脂D101对发酵液中活性成分的吸附和解吸效果显著优于XAD-4、HP20和AB-8,其解吸液的杀线虫活性明显提高。发酵条件的优化和大孔吸附树脂的筛选,明显提高了发酵液的杀线虫活性,为进一步分离纯化该菌株的活性成分奠定了基础,为微生物杀线虫剂的开发和应用提供了理论依据。     

非水介质大孔树脂分离纯化虾壳中虾青素

通过7种大孔树脂对虾青素的静态吸附容量和解析率等指标的考察,筛选出AB-8大孔吸附树脂,用于分离虾壳中虾青素,同时利用高效液相色谱（HPLC）法测量虾青素的含量。结果表明,AB-8树脂对虾青素的吸附量为（24．17±0．5）mg／g,解吸率为95．2％,最大上样量（每g干树脂）以虾青素计为（23．07±0．2）mg,并确定用8倍量柱床体积的乙酸乙酯为洗脱剂,纯化所得虾青素的纯度为14．73％。     

Adsorption kinetics,isotherm, and thermodynamics studies of acetyl-11-keto-β-boswellic acids (AKBA) from Boswellia serrata extract using macroporous resin

An acetyl-11-keto-β-boswellic acid (AKBA) is potent anti-inflammatory agent found in Boswellia serrata oleogum resin. Adsorption characteristics of AKBA from B. serrata were studied using macroporous adsorbent resin to understand separation and adsorption mechanism of targeted molecules. Different macroporous resins were screened for adsorption and desorption of AKBA and Indion 830 was screened as it showed higher adsorption capacity. The kinetic equations were studied and results showed that the adsorption of AKBA on Indion 830 was well fitted to the pseudo first-order kinetic model. The influence of two parameters such as temperature (298, 303, and 308?K) and pH (5–8) on the adsorption process was also studied. The experimental data was further investigated using Langmuir, Freundlich, and Temkin isotherm models. It was observed that Langmuir isotherm model was found to be the best fit for AKBA adsorption by Indion 830 and highest adsorption capacity (50.34?mg/g) was obtained at temperature of 303?K. The values of thermodynamic parameters such as the change of Gibbs free energy (ΔG*), entropy (ΔS*), and enthalpy (ΔH*), indicated that the process of adsorption was spontaneous, favourable, and exothermic.