离子交换法从发酵液中提取聚苹果酸

用离子交换法提取发酵液中的聚苹果酸,比较了不同型号的阴离子树脂对聚苹果酸的静态吸附量,其中以D296树脂对聚苹果酸的吸附量最大.通过静态和动态方法,考察了不同操作条件对固定床分离工艺的影响.结果表明,发酵液经预处理后,调pH至9.5,以lBV/h流速上柱吸附,上柱量为4BV;用0.5mol/L NaCl洗脱,速度为1BV/h.该工艺能够将发酵液中大部分杂质去除,PMLA样品的纯度达到 93.2%,提取收率为79.46%.     

离子交换法从发酵液中提取L-亮氨酸

用离子交换法提取发酵液中的L-亮氨酸,比较了不同型号的强酸性阳离子树脂对L-亮氨酸的静态吸附量和吸附动力学,其中以WA-2型树脂对L-亮氨酸吸附量最大、吸附速度快,适于L-亮氨酸的提取.测定了WA-2型树脂对L-亮氨酸的吸附等温线,并回归得到Freundlich方程.考察了固定床操作工艺条件,结果表明:发酵液经预处理后,以1BV/h流速上柱吸附,上柱量为2BV;再用0.3mol/L的氨水洗脱,速度为1BV/h,洗脱效果较好,L-亮氨酸回收率达到95.7%.提取过程中WA-2型树脂不会受到不可逆的污染,也没有机械损坏,其使用寿命不受影响.     

阳离子交换树脂二次纯化紫甘薯花色苷的研究

采用阳离子交换树脂二次纯化紫甘薯花色苷。以紫甘薯花色苷的吸附率,解吸率和花色苷含量等为考察指标,确定了阳离子交换树脂二次纯化紫甘薯花色苷的工艺条件。研究结果表明,D061树脂对紫甘薯花色苷的吸附量大,解吸容易,可用于二次纯化紫甘薯花色苷的工业化生产,其工艺条件为:上样液的pH值为2.6,上样液吸光度值在0.6×100左右,上样流速为1.0BV/h,50%乙醇(含2%盐酸)为洗脱液,洗脱流速为0.5BV/h,用此工艺条件D061树脂吸附花色苷的吸附量为10.5mg/g,洗脱剂用量为3.0BV,花色苷的收率为82.99%。二次纯化后,紫甘薯花色苷的花色苷含量达到29.38%,色价高达136.80。     

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。     

大孔树脂对油茶叶黄酮的吸附分离特性研究

选择6种大孔吸附树脂,比较其对油茶叶黄酮(FCOA)的吸附量和解吸率,筛选出较优的油茶叶黄酮吸附剂,并对其静态吸附动力学曲线和动态吸附性能进行了考察。实验结果表明,D101树脂适合于FCOA的吸附分离,其吸附机理符合Langmuir单分子层吸附。D101树脂吸附分离FCOA适宜的工艺参数为:上样液浓度为1.2mg/mL左右,pH值3.29,上样流速2BV/h,溶液处理量为19BV;洗脱剂为70%乙醇,洗脱流速2BV/h,洗脱剂用量约4BV。     

吸附树脂分离纯化枇杷花总黄酮的研究

比较了D-101、D-160、AB-8、NKA-9和聚酰胺等5种吸附树脂对枇杷花总黄酮的吸附及解吸附性能。在静态吸附和动态吸附实验基础上,筛选出效果较好的AB-8树脂进行动态吸附参数的研究。考察了样品液pH值、样品液浓度、洗脱液浓度、上样速度、洗脱速度等对AB-8树脂吸附和解吸效果的影响,确定了AB-8树脂动态吸附枇杷花总黄酮的最佳条件。获得的最佳纯化条件如下,样品液pH值为5.5,样品液浓度为12mg/mL,洗脱液为30%的乙醇水溶液,上样速度为2BV/h,洗脱速度为1BV/h。纯化后样品总黄酮含量达86.7%,比纯化前总黄酮含量高5~6倍。实验结果表明,AB-8树脂可用于分离纯化枇杷花总黄酮。     

大孔树脂对发酵液中松脂醇二葡萄糖苷的吸脱附性能

考察了S-8、AB-8、NKA-II、NKA-9 4种大孔吸附树脂对杜仲内生真菌拟茎点霉属XP-8发酵液中松脂醇二葡萄糖苷(Pinoresinol Diglucoside,PDG)的吸附和脱附性能,筛选出S-8树脂的吸附和脱附性能最好;探讨了S-8树脂在静态吸附条件下对发酵液中PDG的吸附平衡和吸附动力学,考察了温度和pH值对吸附效果的影响;进行了动态吸附实验,确定了最佳吸附和洗脱条件。结果表明,在静态吸附条件下,Langmuir方程可很好地描述PDG在S-8树脂上的吸附平衡,液膜扩散和颗粒内扩散分别是控制吸附初期和后期吸附速率的主要步骤;动态吸附的最佳条件是,上样浓度为0.195mg/mL、上样温度为20℃、pH 9、进样流速1BV/h,溶液处理量20BV;最佳动态洗脱条件是,洗脱液为30%的乙醇水溶液,洗脱液流速1BV/h,用量为6BV。整个动态吸附洗脱过程结束后的PDG得率为89.8%。     

大孔吸附树脂分离纯化枳实中辛弗林的研究

以辛弗林的吸附量、解吸率和所得粉末中辛弗林的含量为指标,从选用的6种大孔吸附树脂中筛选出较好的AB-8树脂。通过静态和动态实验,对辛弗林在AB-8树脂上吸附和解吸的条件进行优化,并考察其吸附等温线、吸附和解吸性能。结果表明,在环境温度约25℃下,使用AB-8树脂纯化辛弗林的较优工艺参数为:上柱液pH值7～8,流速2BV/h,溶液处理量3BV,洗脱剂为20%乙醇,洗脱速度1BV/h,收集洗脱液3BV。按此工艺条件,辛弗林的解吸率为87.2%,3BV洗脱液浓缩干燥后,所得粉末中辛弗林含量为56.6%。     

树脂吸附法分离纯化桑叶总黄酮——（Ⅱ）动态法分离桑叶总黄酮的工艺条件及数学模拟

考察了H103树脂固定床吸附分离桑叶总黄酮的工艺参数,并对吸附工艺进行了数学模拟和比较.实验结果表明,H103树脂固定床吸附分离桑叶总黄酮在上样浓度6.05mg/mL时,以9mL/min上样,吸附完全后用60%乙醇以4.5mL/min流速洗脱,桑叶总黄酮产品的回收率为90.57%,纯度为76.33%,建立的固定床吸附模型为预测固定床吸附桑叶水提液中桑叶黄酮达到穿透点时间及固定床吸附容量提供了准确、快捷的方法.     

大孔树脂分离纯化藏药白花龙胆花总黄酮的研究

考察了HPD-826、HPD-417、ADS-17、HPD-722、HPD-450、AB-8、HPD-600、D-101,共8种大孔树脂对藏药白花龙胆花总黄酮的吸附和解吸性能,通过静态吸附量和解吸附率及静态吸附曲线的绘制,筛选出AB-8树脂的效果最佳;以AB-8树脂为目标,进行了动态吸附实验,考察了上柱液浓度、pH值、上柱液流速、乙醇浓度、解吸剂流速、解吸体积等对AB-8树脂吸附和解吸效果的影响,确定出AB-8树脂动态吸附白花龙胆花总黄酮的最佳条件:上柱液浓度为6.5mg/mL,pH为3.79,上柱流速4BV/h;最佳洗脱条件:用50%乙醇进行洗脱,解吸流速为3BV/h,解吸体积4BV。在此条件下,白花龙胆花总黄酮纯度由原来的22.10%,变为65.75%,产品精制倍数为65.75%/22.10%=2.97,表明AB-8树脂可用于白花龙胆花总黄酮的分离纯化。     

大孔吸附树脂对熊果酸吸附性能的研究

研究了从山楂叶中纯化熊果酸的柱层析工艺。静态吸附结果表明,X-5、NKA和AB-8树脂的吸附率分别为91.32%,72.28%和41.19%;以90%乙醇为洗脱剂,X-5、NKA和AB-8树脂的洗脱率分别为83%,70%,87%。静态实验表明X-5树脂具有较好的吸附解吸性能。动态实验优化了在X-5树脂中的流速、上样液的熊果酸浓度和上样体积。结果表明,流速为3BV/h(BV为倍量体积),上样液的熊果酸浓度为0.304mg/mL,上样体积为3BV为最优上样条件。动态洗脱中采用梯度洗脱方式,结果表明在90%的乙醇洗脱下,熊果酸纯度达93.21%。对层析工艺制备的熊果酸进行结晶处理,所获得的熊果酸纯度为98.61%,与熊果酸标准品的红外光谱一致。     

Separation and purification of flavonoid from Taxus remainder extracts free of taxoids using polystyrene and polyamide resin

An efficient separation process of flavonoid from Taxus wallichiana var. mairei remainder extracts free of taxoids was developed in this study. AB‐8 macroporous resin and polyamide resin offered the fine adsorption capacity, and its adsorption rate at 30°C fitted well to the Langmuir and Freundich isotherms. Resin dynamic adsorption and desorption experiments were conducted to optimize the separation process of total flavonoids from T. wallichiana var. mairei remainder extracts free of taxoids. The optimum parameters for adsorption by AB‐8 resin were as follows: (1) the concentration of flavonoids in a sample solution of 5.61 mg/mL with a processing volume of 2 bed volume (BV) (60 mL); (2) for desorption, ethanol–water (80:20, v/v), with 6 BV as an eluent at a flow rate of 2 BV/h. After a one‐run treatment with AB‐8 resin, the content of flavonoids was increased 5.10‐fold from 4.05 to 20.65%. The optimum parameters for adsorption by polyamide resin were as follows: processing volume of 2 BV (30 mL); for desorption, ethanol–water (70:30, v/v), with 8 BV as an eluent at a flow rate of 2 BV/h. After one‐run treatment with polyamide resin, the content of total flavonoids increased from 20.65 to 65.21%. The method will provide a potential approach for large‐scale separation and purification of flavonoid for its wide pharmaceutical use.     

NAK-12树脂脱除蚕蛹复合氨基酸异味及褐变物质的研究

本文研究了用NAK－12吸附树脂脱除蚕蛹复合氨基酸异味及褐变色素的条件，初步分析了蚕蛹复合氨基酸异味产生的原因，实验结果表明：当流速为3BV／h时，1ml NAK-12吸附树脂能吸附1．75g蚕蛹复合氨基酸中的异味物质；能吸附1．45g蚕蛹复合氨基酸中的褐变物质。甲醇是异味物质和褐变物质的良好洗脱剂，用pH1．0的甲醇以1BV／h流速洗脱，仅用3．5BV的洗脱剂即可完全洗脱异味物质和褐变物质，蚕蛹复合氨基酸异味产生的可能机理是：加热蚕蛹复合氨基酸液时，其苯丙氨酸，蛋氨酸，蛋氨酸，异亮氨酸，亮氨酸，苏氨酸被氧化脱氨，生成挥发性醛，而其褐变则是赖氨酸，精氨酸与还原糖发生Maillard反应生成褐变物质引起的。     

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。     

大孔吸附树脂富集板蓝根中(R,S)-告依春工艺研究

采用静态吸附法考察了D101、AB-8、NKA-2、NKA-9、HPD 100、HPD600等6种大孔吸附树脂对(R,S)-告依春的吸附及解吸性能,筛选出效果最佳的AB-8树脂,并对其进行动态考察.最佳富集条件为:上样液pH 6,生药质量-体积浓度为0.200g/mL,解吸液为2BV量70％乙醇,在优化条件下(R,S)-告依春在浸膏中含量可从0.76％提高到12.48％.结果表明,AB-8型大孔吸附树脂可用来从板蓝根水提取液中富集(R,S)-告依春.     

Separation of injectable salidroside by column chromatography of macroporous resins for treating myocardial ischemia

The objective of the present study is to develop a method for large-scale separating and purifying salidroside from rhodiola kirilowii roots and for preparing injectable medicinal ingredient.Crude extract of salidroside was prepared by water-ethanol system,and purified by column chromatography of macroporous resins.Static adsorption and desorption studies were performed on six kinds of macroporous resins,and SP825 resin was chosen,followed by optimizing process parameters.The optimum sample volume,feed concentration,ratio of diameter to height,and feeding flow rate were 1.5 bed volumes(BV),15 mg/mL,1:10 and 1 BV/h,respectively.Dynamic desorption was performed consecutively with 8 BV of distilled water,3 BV of 5% ethanol and 8 BV of 10% ethanol at a flow rate of 2 BV/h.After three cycles in separating 3.5 tons of rhodiola kirilowii roots,salidroside purity was increased from 3.4% in the crude extract to 93.6% in purified salidroside product.This study provides a novel method to separate salidroside for injectable use.     

ADSORPTION AND DESORPTION OF DSD ACID MANUFACTURING WASTEWATER ON MACROPOROUS RESIN

4,4‘-diaminostilbene-2,2‘-disulfonic acid (DSD acid) manufacturing wastewater was treated by a macroporous resin in a fixed-bed column.The results showed that this method was suitable for removal of chemical oxygen demands(COD) and color,About 91% COD and 99.5% color removal were obtained under the optimum adsorption conditions.i.e.temperature 20℃,flow rate lbed volume/hour(BV/hr)and pH1-2.The resin was efficiently regenerated with aqueous sodium hydroxide and water.Furthermore,65.5% of 4,4‘-dinitrostilbene-2,2‘-disulfonic acid(DNS) could be recovered from wastewater for possible recycling to the manufactureing process.The adsorption capacity of resin remained constant during the repetition process of adsorption and desorption.     

Optimization of luteolin separation from pigeonpea [Cajanus cajan (L.) Millsp.] leaves by macroporous resins

In the present study, the performance and separation characteristics of eight macroporous resins for the separation of luteolin (LU) from pigeonpea leaves extracts have been evaluated. The adsorption and desorption properties of LU on macroporous resins including AB-8, NKA-9, NKA-2, D3520, D101, H1020, H103 and AL-2 have been compared. AL-2 resin offers the best adsorption and desorption capacity for LU than other resins based on the research results, and its adsorption data at 25 degrees C fit best to the Freundlich isotherm. Dynamic adsorption and desorption experiments have been carried out with the column packed by AL-2 resin to optimize the separation process of LU from pigeonpea leaves extracts. The optimum parameters for adsorption were sample solution LU concentration 65.5 microg/ml, pH 5, processing volume 3 BV, flow rate 1.5BV/h, temperature 25 degrees C; for desorption were elution solvent ethanol-water (50:50, v/v) 2 BV and followed by ethanol-water (60:40, v/v) 2 BV, and flow rate 1BV/h. After treated with AL-2 resin, the LU content in the product was increased 19.8-fold from 0.129% to 2.55%, with a recovery yield of 78.54%. The results showed that AL-2 resin revealed a good ability to separate LU. Therefore, we conclude that results in this study may provide scientific references for the large-scale LU production from pigeonpea or other plants extracts.