大孔吸附树脂分离纯化昆仑雪菊总黄酮工艺的研究

筛选分离纯化昆仑雪菊总黄酮的大孔吸附树脂并建立纯化工艺条件。以大孔吸附树脂对昆仑雪菊总黄酮的吸附量、吸附率和解吸率等为指标,考察了11种型号的大孔吸附树脂进行分离纯化,并确定了该树脂分离纯化最佳工艺参数。结果显示NKA-9型大孔吸附树脂对昆仑雪菊总黄酮分离纯化效果好,其工艺条件为:以pH值为5.0的原料液上柱吸附,70%浓度的乙醇洗脱、洗脱速度3mL·min-1,在此条件下总黄酮的的静态吸附率为95.74%,解吸率为98.9%。     

大孔吸附树脂分离纯化迷迭香酸的研究

采用大孔吸附树脂法研究迷迭香酸的精制工艺。筛选出适合的大孔吸附树脂,并对其分离纯化的条件进行考察。使用静态吸附法确定大孔吸附树脂NK109最适于迷迭香酸的精制。通过动态吸附性能的考察,确定最佳迷迭香酸上柱浓度838.6mg/L,流速为2.0BV/h上柱。通过动态解吸性能的考察,使用乙酸乙酯作为洗脱液,确定洗脱速度为1.0BV/h。利用大孔吸附树脂,迷迭香酸得到了较好的富集和纯化。纯化后的迷迭香酸纯度可以达到90%以上。     

大孔树脂分离纯化丹酚酸的研究

比较了D301R、D392、D380大孔阴离子交换树脂和X-5.AB-8、NKA-9、SP825大孔吸附树脂对丹参水溶性成分的吸附和解吸能力,筛选出效果较好的SP825进行分离纯化丹酚酸的研究.实验表明,大孔吸附树脂SP825能分离出纯度为95.32%的丹参素,在梯度洗脱条件下可得到以丹参素(水洗脱)和丹酚酸B(乙醇洗脱)为主的产品.在最佳吸附与解吸工艺参数下,丹参素、紫草酸、迷迭香酸、丹酚酸A和丹酚酸B的收率分别为:36.92%、80.39%、82.45%、43.07%和41.03%.     

大孔吸附树脂分离纯化异甘草素的研究

研究大孔吸附树脂分离纯化异甘草素的工艺条件及参数。通过研究HPD-600、D4020、D101、AB-8、NKA-II、AL-2和NKA-9树脂对异甘草素的吸附和解吸附能力,筛选最佳树脂为AB-8,并研究了其对异甘草素的吸附和解吸附性能,确定了最佳的吸附与解吸附工艺参数,吸附:pH=5,室温,流速1.5BV/h,溶液处理量为5BV;脱附:洗脱剂为70%的乙醇溶液,流速1BV/h,洗脱剂用量4.5BV。异甘草素样品溶液经AB-8树脂吸附与脱附后回收率为76.7%,纯度由2.02%提高到29.1%,提高了14.4倍。实验结果表明,AB-8树脂对异甘草素的吸附量大,脱附容易,可以应用于异甘草素的分离纯化。     

大孔阴离子树脂分离纯化微生物转化液中5-氟尿苷的研究

探寻从微生物转化液中分离纯化5-氟尿苷(5-FUR)的工艺条件。先后尝试了大孔吸附树脂、大孔弱碱性阴离子交换树脂以及硅胶柱色谱的分离方法,首先利用大孔弱碱性阴离子交换树脂吸附,然后用1mol/L NaCl动态洗脱得到含量较高的两种含氟化合物,最终通过硅胶柱色谱,采用正己烷-乙酸乙酯(含10%醋酸)为流动相进行洗脱,得到了纯度为100%的纯品。在目标化合物和杂质理化性质极其相似,含量极其悬殊的条件下,成功去除含量极高的杂质,实现了5-FUR的分离纯化,圆满地达到了预期的目的。     

Diaion HP–20大孔吸附树脂分离纯化含羞草种子中的黄酮类物质

研究Diaion HP–20大孔吸附树脂分离纯化含羞草种子中黄酮类物质的工艺条件。用海南含羞草种子为原料,以含羞草种子中总黄酮吸附量和解吸率为评价指标,考察上样流量、洗脱液种类、柱径比、洗脱液流量等影响因素。Diaion HP–20大孔吸附树脂分离纯化含羞草种子中黄酮类物质的最佳工艺条件:上样流量3 m L/min,洗脱液为40%乙醇溶液,柱径比为1∶10,洗脱液流量为4 m L/min。该方法简单,可行,能够有效分离纯化含羞草种子中黄酮类物质,且大孔吸附树脂可重生,利用率高。     

大孔吸附树脂对天麻素的吸附与分离特性的研究

研究了AB 8、NKA 9和S 83种大孔吸附树脂对中药天麻提取液中有效成分天麻素的吸附与分离特性。结果表明,NKA 9和S 8树脂对天麻素具有较好的吸附和解吸特性。其中经NKA-9树脂纯化的天麻素纯度为16.4%,比粗提物的天麻素纯度提高了1倍多。     

火棘果总黄酮的提取和纯化研究

采用溶剂提取法、索氏提取法、循环超声提取法提取火棘果总黄酮,利用静态吸附方法筛选分离火棘果总黄酮的最适大孔树脂,利用动态吸附方法研究最适大孔树脂纯化火棘果总黄酮的条件,并用紫外分光光度法测定其含量。得出结果为循环超声提取时间短、效率高;D101大孔吸附树脂纯化效果最好,最佳工艺为上样浓度为0.899 8g·L-1,上样液pH为4,上样体积5BV,上样速率2.5mL·min-1,用5BV70%乙醇以2.0 mL·min-1速率洗脱,经树脂纯化后总黄酮的纯度由原来的9.00%提高至28.11%。     

阶段洗脱吸附层析法分离茶多酚咖啡碱

茶叶提取液经大孔吸附树脂二级阶段洗脱层析分离茶多酚咖啡碱.研究了α酸作咖啡碱洗脱剂的可行性及洗脱效果,解决了酸性溶液中茶多酚及咖啡碱的分析方法问题.确定XDA-1树脂为吸附剂,α酸及85%乙醇二级阶段洗脱层析分离茶多酚咖啡碱的优惠工艺.研究了XAD-7树脂再生α酸回收咖啡碱的工艺条件,形成了全树脂法生产茶多酚咖啡碱的新工艺.所得茶多酚产品纯度可达93.83%,咖啡碱含量为2.78%,收率可达13%.本工艺过程简单,避免使用有毒溶剂,安全无污染.     

大孔树脂分离纯化楮果总黄酮优化工艺研究

筛选适合分离纯化楮果总黄酮的大孔树脂并确定最优工艺条件。以静态吸附率和解吸率为指标对8种大孔树脂进行筛选,确定D101树脂的分离纯化效果最佳。通过动态吸附实验考察上样流速、上样溶液pH值、上样溶液浓度、乙醇浓度、洗脱流速、洗脱剂用量等工艺条件对分离纯化效果的影响,确定最优工艺条件如下:上样流速为2BV/h,pH值为6,上样溶液浓度为0.05mg/mL,80%乙醇作洗脱剂,洗脱流速为5BV/h,洗脱剂用量为7.5BV。采用最优工艺条件,楮果总黄酮含量提高至22.26%,产品精制倍数为4.79,表明D101树脂能有效纯化楮果总黄酮。     

Enrichment and purification of madecassoside and asiaticoside from Centella asiatica extracts with macroporous resins

In present study, the performance and separation characteristics of five macroporous resins for the enrichment and purification of asiaticoside and madecassoside from Centella asiatica extracts have been evaluated. The adsorption and desorption properties of total triterpene saponins (80% purity) on macroporous resins including HPD100, HPD300, X-5, AB-8 and D101 have been compared. According to our results, HPD100 offered higher adsorption and desorption capacities and higher adsorption speed for asiaticoside and madecassoside than other resins. Column packed with HPD100 resin was used to perform dynamic adsorption and desorption tests to optimize the separation process of asiaticoside and madecassoside from C. asiatica extracts. After the treatment with gradient elution on HPD100 resin, the content of madecassoside in the product increased from 3.9 to 39.7%, and the recovery yield was 70.4%; for asiaticoside the content increased from 2.0 to 21.5%, and the recovery yield was 72.0%. The results showed that HPD100 resin revealed a good ability to separate madecassoside and asiaticoside, and the method can be referenced for the separation of other triterpene saponins from herbal raw materials.     

Highly selective separation and purification of chicoric acid from Echinacea purpurea by quality control methods in macroporous adsorption resin column chromatography

Chicoric acid is the main phenolic active ingredient in Echinacea purpurea (Asteraceae), best known for its immune‐enhancing ability, as well as used as a herbal medicine. To achieve further utilization of medicinal ingredients from E. purpurea, an efficient preparative separation of chicoric acid was developed based on macroporous adsorption resin chromatography. The separation characteristics of several different typical macroporous adsorption resins were evaluated by adsorption/desorption column experiments, and HPD100 was revealed as the optimal one, which exhibited that the adsorbents fitted well to the pseudo‐second‐order kinetics model and Langmuir isotherm model, and the optimal process parameters were obtained. The breakthrough curves could be predicted and end‐point could be determined early. Besides, the optimal elution conditions of chicoric acid can be achieved using the quality control methods. As a result, the purity of chicoric acid was increased 15.8‐fold (from 4 to 63%) after the treatment with HPD100. The process of the enrichment and separation of chicoric acid is considerate, because of its high efficiency and simple operation. The established separation and purification method of chicoric acid is expected to be valuable for further utilization of E. purpurea according to product application in pharmaceutical fields in the future.     

中药复方溶液环境对黄连生物碱大孔树脂吸附的动力学比较研究

研究含黄连的不同中药复方水提液溶液环境对大孔树脂吸附率的影响,为大孔树脂在中药生产中的优选和在中药复方精制分离技术中的推广应用提供实验依据。采用pH、电导率、盐度、浊度、黏度5项物理化学指标性参数表征6种复方水提液体系,通过比较黄连生物碱于不同溶液环境中对相同AB-8树脂的吸附动力学变化,考察溶液环境对复方中指标性成分分离纯化的影响。实验结果表明,黄连在不同中药复方配伍中,虽然溶液环境差异较大,但黄连中生物碱类成分均可以在树脂上被选择性吸附,复方1~6指标性生物碱成分达到吸附平衡的时间均有差异;复方2的电导率和盐度较大,生物碱与大孔树脂的吸附作用显著降低,复方6的电导率小而黏度较大,生物碱达到吸附平衡的时间较其他复方长,吸附作用大于复方2而较其他复方较小。上述研究结果表明,复方水溶液的电导率、盐度为影响生物碱在大孔树脂选择性吸附的主要因素,黏度影响生物碱达到吸附平衡的时间。     

PURIFICATION OF L-METHIONINE AND N-ACETYL-D-METHIONINE FROM THE MIXTURE OF ENZYMATICALLY DEACYLATED N-ACETYL-DL-METHIONINE

1. INTRODUCTION Methionine, namely 2-amido-4-thiomethyl butyric acid with a structure of CH3SCH2CH2CHCOOH, is one of the essential amino acids and has two natural enantionmers, D and L-methionine. The mixture of L- and D-isomers can be used as analeptics or nutritive additives to maintain the equilibrium of amino acids of feed [1,2]. L-methionine can release active methyl and accelerate the synthesis of choline, which further speeds up the conversion of the lipid accumulated in liv…     

PURIFICATION OF L-METHIONINE AND N-ACETYL-D-METHIONINE FROM THE MIXTURE OF ENZYMATICALLY DEACYLATED N-ACETYL-DL-METHIONINE

N-acetyl-D-methionine, AaAc and the remams of N-acetyl-L-methionme dramatically.affect the purification of L-methionine when purified from the mixture of en.“ymatically deacylated N-acetyl-DL-methionine, leading to a low yield conventionally. Here, this paper reports a successful separation and purification of both L-methionine and N-acetyl-D-methionine by an H ion-exchange column. The pH, L-Met concentration and tile ratio between the content of sodium cation and the ion-exchange capacity were optimized to obtain the maximum yield. Experimental results indicate that, under the optimized conditions, the yields of L-methionine and N-acetyl-D-methionine can reach as high as 85% and 75%, respectively.     

Preparative purification of salidroside from Rhodiola rosea by two‐step adsorption chromatography on resins

Salidroside is an effective adaptogenic drug extracted from Rhodiola species. In the present study, a simple and efficient method for preparative separation and purification of salidroside from the Chinese medicinal plant Rhodiola rosesa was developed by adsorption chromatography on macroporous resins. The static adsorption isotherms and kinetics of some resins have been determined and compared for preparative separation of salidroside. According to our results, HPD‐200 resin is the most appropriate medium for the separation of salidroside and its adsorption data fit the Langmuir isotherm well. Dynamic adsorption and desorption were carried out in glass columns packed with HPD‐200 to optimize the separation process. After two adsorption and desorption runs, a product with a salidroside content of 92.21% and an overall recovery of 48.82% was achieved. In addition, pure lamellar crystals of salidroside with a purity of 99.00% could be obtained from this product. Its molecular weight was determined by an ESI‐MS method. The simple purification scheme avoids toxic organic solvents used in silica gel and high‐speed counter‐current chromatographic separation processes and thus increases the safety of the process and can be helpful for large‐scale salidroside production from Rhodiola rosea or other plant extracts.     

DNA adsorption via Co(II) immobilized cryogels

The separation and purification of important biomolecule deoxyribonucleic acid (DNA) molecules are extremely important. The adsorption technique among these methods is highly preferred as the adsorbent cryogels are pretty much used due to large pores and the associated flow channels. In this study, the adsorption of DNA via Co(II) immobilized poly(2-hydroxyethyl methacrylate-glycidyl methacrylate) [poly(HEMA-GMA)] cryogels was performed under varying conditions of pH, interaction time, initial DNA concentration, temperature, and ionic strength. For the characterization of cryogels; swelling test, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), surface area (BET), elemental and ICP-OES analysis were performed. L-lysine amino acid was chosen as Co(II)-chelating agent and the adsorption capacity of cryogels was determined as 33.81 mg DNA/g cryogel. Adsorption of pea DNA was studied under the optimum adsorption conditions and DNA adsorption capacity of cryogels was found as 10.14 mg DNA/g cryogel. The adsorption process was examined via Langmuir and Freundlich isotherm models and the Langmuir adsorption model was determined to be more appropriate for the DNA adsorption onto cryogels.     

New Thiophilic Adsorbent for the Purification of Insulin and Immunoglobulins G

We have synthesized new supports for the purification of insulin and IgG by affinity chromatography. These supports combine the advantages of biospecific ligands with the excellent separation properties of thiophilic sorbents. The existence of N-acetyl-neuraminic acid in insulin receptor and in the antigenic determinant of IgG suggests that such an acid may develop specific interactions usable in affinity chromatography. Therefore, N-acetylneuraminic acid was used as an active ligand in comparison with the β-mercaptoethanol. The performances of these supports were tested under static and dynamic (LC) conditions. The support functionalized by sialic acid appears significantly more selective than the support grafted by β-mercaptoethanol; and its purification yield is better. This new support showed similar adsorption characteristics with thiophilic adsorbent. These affinity supports allowed a one-step separation of the insulin and IgG subclasses from a pancreatic extract and mouse ascitic fluids, respectively, by LC.