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.     

大孔树脂-高速逆流色谱法分离纯化地黄中毛蕊花糖苷

该文建立了大孔树脂-高速逆流色谱分离中药材地黄中有效成分毛蕊花糖苷的方法。考察了4种大孔树脂对地黄粗提物中毛蕊花糖苷的静态吸附与解吸情况,其中D101大孔树脂对目标成分的吸附率与解吸率最理想,实验结果表明体积分数为10%的乙醇洗脱得到的毛蕊花糖苷含量最高,目标成分含量从4.9%提高到32.6%。最后,部分纯化的样品（165 mg）采用高速逆流色谱进一步纯化,两相溶剂系统由乙酸乙酯-正丁醇-水（1：4：5,v/v/v）组成,分离得到45 mg纯度为96%的毛蕊花糖苷。     

Enrichment and purification of deoxyschizandrin and γ-schizandrin from the extract of Schisandra chinensis fruit by macroporous resins

In present study, the performance and separation characteristics of 21 macroporous resins for the enrichment and purification of deoxyschizandrin and γ-schizandrin, the two major lignans from Schisandra chinensis extracts, were evaluated. According to our results, HPD5000, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for deoxyschizandrin and γ-schizandrin than other resins. Columns packed with HPD5000 resin were used to perform dynamic adsorption and desorption tests to optimize the technical parameters of the separation process. The results showed that the best adsorption time is 4 h, the rate of adsorption is 0.85 mL/min (4 BV/h) and the rate of desorption is 0.43 mL/min (2 BV/h). After elution with 90% ethanol, the purity of deoxy-schizandrin increased 12.62-fold from 0.37% to 4.67%, the purity of γ-schizandrin increased 15.8-fold from 0.65% to 10.27%, and the recovery rate was more than 80%.     

聚（对乙烯基苄基脲）大孔吸附树脂对银杏叶黄酮的吸附性能

通过静态吸附平衡和动态柱吸附试验,研究了自制大孔交联聚（对乙烯基苄基脲）树脂（简称PMVBU树脂）对银杏叶黄酮的吸附性能．结果表明,在pH=5．00时,该树脂对银杏叶黄酮有较好的吸附性能;PMVBU树脂对黄酮的吸附等温线符合Langmuir吸附等温方程,相关系数R^2〉0．99．308K时,PMVBU干树脂对黄酮的静态饱和吸附量达293．3mg／g．298K时,干树脂的动态吸附穿透容量为180mg／g．用75％的乙醇溶液对吸附在PMVBU树脂上的黄酮可进行有效洗脱．银杏叶提取液经过该树脂吸附柱吸附纯化后,黄酮纯度提高了18．6％,且树脂具有良好的重复使用性．     

Preparative separation of vitexin and isovitexin from pigeonpea extracts with macroporous resins

Vitexin and isovitexin are a pair of isomeric compounds known as the major constituents in pigeonpea leaves and possess various pharmacological activities. In the present study, the preparative separation of vitexin and isovitexin with macroporous resins (Nankai Hecheng S & T, Tianjin, China) was studied. The performance and adsorption characteristics of eight macroporous resins including ADS-5, ADS-7, ADS-8, ADS-11, ADS-17, ADS-21, ADS-31 and ADS-F8 have been evaluated. The research results indicate that ADS-5 resin is most appropriate for the separation of vitexin and isovitexin. Langmuir and Freundlich isotherms were used to describe the interactions between solutes and resin at different temperatures, and the equilibrium experimental data were well fitted to the two isotherms. Column packed with ADS-5 resin was used to perform dynamic adsorption and desorption tests to optimize the separation process. The optimum parameters for adsorption were as follows: the concentration of vitexin and isovitexin in sample solution: 0.22 and 0.40mg/mL, respectively, processing volume: 3 BV, flow rate: 1mL/min, pH 4, temperature: 25 degrees C; for desorption: ethanol-water (40:60, v/v), 5 BV as an eluent, flow rate: 1mL/min. After one run treatment with ADS-5 resin, the contents of vitexin and isovitexin were increased 4.07-fold and 11.52-fold from 0.86%, 1.53% to 3.50% and 17.63%, the recovery yields were 65.03% and 73.99%, respectively. In conclusion, the preparative separation of vitexin and isovitexin can be easily and effectively achieved via adsorption and desorption on ADS-5 resin, and the method can be referenced for the separation of other flavone C-glucosides from herbal materials.     

丹参酚酸B生产中去除胶体类杂质的工艺方法

胶体类杂质的去除是丹参酚酸B(salvianolic acid B, SB)纯化工艺的难点之一。实验中基于前沿色谱与置换色谱相结合的原则,改良常规大孔吸附树脂柱的操作方法,将树脂按一定的比例装入大小两支柱。小柱与大柱串联,上样至胶体类杂质在小柱上达到吸附饱和,用50%甲醇单独洗脱大柱上的SB部分,利用树脂吸附色谱法实现了SB与胶体类杂质的分离。结果表明,经过去胶体类杂质处理后,SB的加权平均纯度由59.6%提高到64.5%,收率由69.75%提高到80.0%,并且SB的洗脱条件降低。本工艺方法适合于规模化工业生产。     

大孔吸附树脂分离提取多杀菌素

采用大孔吸附树脂法分离提取多杀菌素.从11种大孔吸附树脂中筛选出DM11进行了静态、动态吸附性能实验,并考察了不同吸附、解吸条件的影响.结果表明,DM11的静态吸附容量为25.63mg/g(wet resin),其吸附等温线符合Langmuir吸附等温式.采用丙酮做洗脱剂,洗脱率为97.5%,动态吸附最佳吸附pH为9.5,吸附流速为6BV/h,穿透吸附容量为21.2mg/ml(wet resin),洗脱流速1.5BV/h.     

树脂吸附法分离纯化桑叶总黄酮(Ⅰ)H103树脂对桑叶水提液中总黄酮的吸附性能

采用大孔吸附树脂法从桑叶水提液中分离黄酮类化合物。通过比较10种大孔吸附树脂对桑叶水提液中总黄酮的吸附特性及机理,发现H103树脂对桑叶总黄酮吸附量大、洗脱容易、吸附速度快,是一种良好的桑叶总黄酮吸附剂。实验表明,H103树脂吸附桑叶黄酮的适宜上样浓度为6.05mg/mL,吸附动力学符合Bangham模型,吸附过程符合内扩散模型。     

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.     

SP700大孔树脂纯化酸枣仁中三萜总皂苷的研究

从7种极性不同的大孔树脂中筛选出一种对酸枣仁三萜总皂苷具有良好吸附和解吸性能的树脂—三菱SP700树脂。静态实验中,该树脂的最高吸附容量可达131.0mg皂苷/g树脂,皂苷在树脂表面的吸附符合Langmuir模型,用体积分数为90%的乙醇解吸得率最高可达97.8%;动态实验中,样液在膨胀床模式下上样,树脂的平均动态吸附容量为15mg皂苷/g树脂,上样后,用体积分数分别为50%和90%的乙醇溶液进行分段洗脱,洗脱得率最高可达到95.1%,经过纯化的皂苷提取物的含量提高了4倍。SP700大孔吸附树脂作为一种对酸枣仁中三萜总皂苷进行纯化的介质具有良好的性能和应用价值。     

几种树脂对芦荟苦素的吸附性能

研究硅胶H和三种不同极性的大孔吸附树脂对芦荟苦素的吸附与洗脱性能，用静态实验筛选树脂、动态实验考察芦荟苦素提取液浓度、上样流速和温度对GD-10大孔吸附树脂吸附能力影响。结果表明GD-10吸附树脂对芦荟苦素的吸附能力较强，洗脱能力最好，且易于再生。     

Separation of salvianic acid A from the fermentation broth of engineered Escherichia coli using macroporous resins

Salvianic acid A (also known as danshensu) is a plant‐derived polyphenolic acid, and has a variety of physiological and pharmacological activities. Our laboratory previously constructed an unprecedented artificial biosynthetic pathway in Escherichia coli and established the fermentation process to produce salvianic acid A. Here, we developed an efficient method for separating salvianic acid A from the fermentation broth of engineered Escherichia coli by macroporous resins. Among ten tested macroporous resins, the static and dynamic adsorption/desorption experiments demonstrated that X5 resin was the best to separate salvianic acid A from fermentation broth. Other parameters during static and dynamic procedures were also investigated. Under the optimum separation conditions, the average adsorption capacity of SAA were 10.66±0.54 mg/g dry resin and the desorption ratio was 85.6±4.1%. The purity and recovery yield of salvianic acid A in the final dry product were 90.2±1.5 and 81.5±2.3%, respectively. The results show that adsorption separation with macroporous resin X5 was an efficient method to prepare salvianic acid A from fermentation broth. This work will benefit the development and application of plant‐derived salvianic acid A and its derivatives.     

用大孔吸附树脂分离利血平

以利血平的吸附量和解吸率为指标,筛选大孔吸附树脂.研究吸附和解吸的优化条件,并考察选定树脂的吸附等温线、吸附动力学、吸附和解吸性能.结果表明,将催吐萝芙木根粉浸提液蒸去乙醇且不调pH(pH 1)进行吸附,HZ-818型大孔吸附树脂对利血平的吸附量可达到9.34mg/mL.使用工业乙醇-水(80:20,pH 1.0)为解吸剂,解吸率可达99.3%.该树脂的吸附符合Langmuir吸附等温方程.吸附前期,吸附速度较快,以后速度减慢.HZ-818型树脂对利血平的吸附量大,解吸率高,通过大孔树脂吸附和解吸,利血平浓度提高50倍以上,适宜于工业化生产.     

The application of macroporous resins in the separation of licorice flavonoids and glycyrrhizic acid

Glycyrrhizic acid (GA) and licorice flavonoids (LF) are the two classes of bioactive components in licorice with known pharmacological effects. But long-term excessive intake of GA may cause sodium retention and hypertension. In this study, the performance and adsorption characteristics of four widely used macroporous resins for the separation of deglycyrrhizinated, flavonoids enriched licorice has been critically evaluated. The sorption and desorption properties of LF and GA on macroporous resins including XDA-1, LSA-10, D101 and LSA-20 have been compared. The adsorption capacity was found to depend strongly on the pH of the feed solution. XDA-1 offers much higher adsorption capacity for GA and LF than other resins, and its adsorption data fit the best to the Freundlich isotherm. XDA-1 also shows much higher adsorption affinity towards LF than that of GA based on calculated results from the measured adsorption isotherms. Dynamic adsorption and desorption experiments have been carried out on a XDA-1 resin packed column to obtain optimal parameters for separating GA and LF. An enriched LF extract (about 21.9% purity) free of GA, and an enriched GA extract with 66% purity can be separated from crude licorice extract in one run.     

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.     

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%.     

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.     

两种大孔吸附树脂结合分离纯化京尼平甙

比较了H103、NKA-II、HPD100A、HPD400A及D141等5种大孔吸附树脂对栀子提取液中栀子黄色素和京尼平甙的吸附性能。在通过静态吸附实验研究其吸附量、吸附动力学特征的基础上,确定了用H103和HPD100A两种非极性大孔树脂进行京尼平甙的分离纯化,并确定了工艺参数。首先用H103树脂吸附京尼平甙,用蒸馏水洗脱杂质,再用一定浓度的乙醇洗脱;所得的京尼平甙洗脱液再用HPD100A树脂吸附,进一步除去栀子黄色素等杂质,得到的京尼平甙纯度达到81.3%,回收率为88.5%。     

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.