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。     

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。     

大孔吸附树脂分离纯化香椿叶总黄酮的研究

比较了AB-8、S-8、X-5、NKA-9、D-3520、NKA、聚酰胺、硅胶8种吸附剂对香椿叶黄酮类化合物的吸附及脱附性能.在静态吸附试验的基础上,筛选出效果较好的X-5树脂进行动态试验研究.结果表明,X-5树脂在约15℃下对香椿叶总黄酮动态吸附-脱附较优的工艺参数为:上柱液pH值5～6,上柱速度3BV/h,溶液处理量6BV/次;脱附剂为70%乙醇,脱附剂的流速3BV/h,脱附剂用量6BV/次.此工艺条件能够分离纯化香椿叶黄酮类化合物,树脂使用1次时,总黄酮的收率达95.5%,总黄酮的纯度由7.2%提高到43.5%;树脂重复使用5次时,总黄酮的收率仍达80%以上,总黄酮的纯度可由7.2%提高到20%以上.     

S-8树脂分离纯化姜黄素类化合物工艺的研究

在静态吸附的基础上,建立了S-8树脂吸附姜黄素类化合物的等温方程和静态吸附动力学方程,发现其静态吸附规律符合Langmuir方程模型和准二次动力学模型。构建了动态吸附的传质方程,对动态吸附过程中的传质区长度与总传质系数进行探究。采用单因素试验确定了S-8树脂对姜黄素类化合物的纯化工艺,姜黄提取液直接配制上样,上样液乙醇浓度60%,上样流速2BV/h,上样量5BV;经水洗后,用无水乙醇洗脱,洗脱流速4BV/h,洗脱量为5BV。经验证,该工艺稳定,平均回收率为88.04%,姜黄素类化合物纯度从16.88%升至42.16%,表明S-8树脂适合用于初步纯化姜黄素类化合物。     

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。     

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%。     

大孔树脂吸附分离速溶茶副产品中茶多酚的研究

通过静态试验比较了不同树脂对速溶茶副产品中茶多酚的吸附和解析特性,筛选出对茶多酚有较好的吸附率和解析率的NKA-9型树脂。动态试验确定了最佳的吸附和解析参数:上样流速为0.8mL/min、上样液温度为60℃、pH为5,洗脱流速为0.9mL/min、乙醇浓度为80%、洗脱剂用量为3BV。经过NKA-9纯化后速溶茶副产品中茶多酚含量达到58.7%,得率为14%。     

大孔吸附树脂对金莲花黄色素的吸附性能研究

本文研究了大孔吸附树脂吸附金莲花黄色素的性能.研究结果表明:采用静态吸附法,从X-5、AB-8、D-296R、NKA、S-8 五种吸附树脂中筛选出一种吸附、解吸性能都较为理想的大孔吸附树脂X-5,并对其进行了静态吸附动力学的研究,得出的静态吸附动力学曲线反映了树脂的吸附量随时间的变化关系,其吸附动力学方程符合Langmiur提出的吸附速率方程.采用动态吸附法,得到动态吸附透过曲线和动态解吸曲线,其中采用80%乙醇溶液作为洗脱剂,其动态解吸率为88.79%.     

大孔吸附树脂纯化迷迭香脂溶性总酚酸的研究

从X-5、D4020、AB-8、H1020、NKA-Ⅱ、HPD-100A、SIPI、HPD800和D3520大孔吸附树脂中筛选出H1020树脂,研究了其对迷迭香脂溶性总酚酸的静态与动态吸附和解吸性能.结果表明,H1020树脂对迷迭香脂溶性总酚酸的饱和吸附量为19.84mg/g干树脂,饱和吸附时间为3h,适宜的解吸荆为体积分数90%的乙醇溶液;以质量浓度为4.45m/mL的迷迭香提取液上柱,流速为1.0mL/min,当吸附平衡后,2.7BV体积分数90%的乙醇溶液可将吸附的总酚酸完全洗脱.经动态纯化后,脂溶性总酚酸质量分数从47.74%提高到70.46%,该组分清除DPPH自由基的IC50值为0.0469mg/mL.     

大孔吸附树脂对莲房原花青素吸附纯化性能的研究

比较了14种大孔吸附树脂对莲房中原花青素(proanthocyanidins of lotus seedpod,LSPAs)的吸附及解吸性能,在研究静态吸附的基础上,筛选出效果较好的树脂进行动态实验研究,并对所得组分LSPAs含量及其相对分子量进行初步分析.结果表明,DM130大孔吸附树脂分离纯化LSPAs效果最佳,上样浓度为2.5mg/mL,流速为3BV/h时,饱和吸附量为4～4.5个BV;当用体积分数为50%乙醇以3BV/h的流速洗脱5BV时,LSPAs的累积回收率可达96.43%,含量从22.54%提高到95.31%;经质谱分析,(M+H)分子量范围为291.1～1155.3,聚合度≤4.     

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。     

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.     

Separation of 7-xylosyl-10-deacetyl paclitaxel and 10-deacetylbaccatin III from the remainder extracts free of paclitaxel using macroporous resins

The separation and enrichment of 10-deacetylbaccatin III (10-DAB III) and 7-xylosyl-10-deacetyl paclitaxel were studied on seven macroporous resins with special structures. The performance of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III on macroporous resins including AB-8, ADS-17, ADS-21, ADS-31, ADS-8, H1020 and NKA-II was compared according to their adsorption and desorption properties. AB-8 provided a much higher adsorption capacity for 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III than other resins, and its adsorption data fitted well to the Langmuir and Freundlich isotherm. According to the adsorption and desorption capacities and the adsorption isotherms, AB-8 demonstrated a remarkable capability for the preparative separation of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III from the remainder extracts free of paclitaxel. In order to optimize parameters of separation, dynamic adsorption and desorption experiments were carried out on the columns packed with AB-8 resin. The optimal conditions were: the processing volume 15 BV; concentrations of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III in feed solution 0.0657 mg/mL and 0.1494 mg/mL; flow rate 1 mL/min; temperature 35 degrees C. The gradient elution program was as follows: 30% ethanol for 3 BV, then 80% of ethanol for 6 BV, flow rate 1 mL/min. After the AB-8 resin treatment, the contents of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III in the product had increased from 0.053% and 0.2% to 3.34% and 1.69%, which were 62.43-fold and 8.54-fold of those in the untreated extracts, respectively, and the recoveries of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III were 85.85% and 52.78%. The performance achieved good separation and higher recovery of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III from remainder extracts free of paclitaxel by using AB-8 resin. It is a fast and effective method for the separation and enrichment of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III.     

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.     

制备型液相色谱法分离纯化3-甲基吡啶光氯化产物中的2-氯-5-三氯甲基吡啶

利用制备型高效液相色谱从3-甲基吡啶光氯化产物中分离纯化得到2-氯-5-三氯甲基吡啶,对制备色谱的洗脱方式、洗脱剂组成及浓度、进样量等参数进行了优化。使用的制备柱为Zorbax-C18柱,以乙腈-水为流动相,采用速度梯度洗脱方式进行洗脱,用二极管阵列检测器在240 nm波长下检测,进样体积为100 μL。该方法的制备回收率为82.7%,相对标准偏差为4.0%（n=5）,产品纯度为99.01%。     

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.     

HPLC法同时测定白花蛇舌草中对香豆酸和熊果酸的含量

建立高效液相色谱法同时测定白花蛇舌草药材中对香豆酸和熊果酸含量的方法。采用Eclipse SB–C18色谱柱(250 mm×4.6 mm,5μm),以甲醇–0.05%甲酸梯度洗脱,流量1 m L/min,对香豆酸和熊果酸的检测波长分别为310 nm和210 nm,柱温30℃。对香豆酸和熊果酸含量分别在0.001 79~0.028 64 mg/m L和0.021 3~0.340 8 mg/m L范围内与色谱峰面积呈良好的线性关系,线性相关系数r分别为0.999 8,0.999 6。对香豆酸和熊果酸的平均加标回收率分别为98.59%,98.23%,测定结果的相对标准偏差分别为0.81%,0.94%(n=6)。样品溶液在24 h内稳定。该方法适用于白花蛇舌草药材中对香豆酸和熊果酸的含量测定。     

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%.     

大孔吸附树脂对大豆皂苷的吸附研究

比较了5种大孔吸附树脂对大豆皂苷的吸附等温线、吸附容量、解吸率和吸附动力学。发现ZTC-1树脂对大豆皂苷吸附量大、解吸容易、吸附速度快，是一种良好的大豆皂苷吸附荆，AB-8树脂次之．选择ZTC-l树脂纯化大豆皂苷粗提液，得到大豆皂苷产品纯度为78．2％(干物质)，回收率为93．1％．     

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.