大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺研究

优选大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺。以总皂苷的洗脱率为考察指标,通过单因素实验对大孔树脂型号、上样液浓度、吸附流速、上样量、洗脱浓度、洗脱流速、洗脱体积、氧化铝用量等因素进行考察,优选分离纯化三七总皂苷的最佳工艺条件。以D101大孔树脂纯化效果最好,最佳上样液浓度为0.5 g生药/mL,上样流速为2 BV/h(BV为柱体积),上样量(药材量∶树脂)为1∶1,依次用水、30%乙醇除杂,用量为3 BV,洗脱流速为2 BV/h,80%乙醇5 BV洗脱,收集洗脱液,将洗脱液过氧化铝柱吸附除杂,氧化铝用量为0.5 g生药/g,中试放大实验平行3次,总皂苷的纯度分别为85.96%,84.53%,86.32%,RSD值为1.13%,出膏率分别为6.45%,6.57%,6.32%,RSD值为1.94%,优选的纯化工艺稳定可行,适用于工业生产。     

大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺研究

优选大孔树脂与氧化铝联用分离纯化三七总皂苷的工艺。以总皂苷的洗脱率为考察指标,通过单因素实验对大孔树脂型号、上样液浓度、吸附流速、上样量、洗脱浓度、洗脱流速、洗脱体积、氧化铝用量等因素进行考察,优选分离纯化三七总皂苷的最佳工艺条件。以D101大孔树脂纯化效果最好,最佳上样液浓度为0.5 g生药/mL,上样流速为2 BV/h(BV为柱体积),上样量(药材量∶树脂)为1∶1,依次用水、30%乙醇除杂,用量为3 BV,洗脱流速为2 BV/h,80%乙醇5 BV洗脱,收集洗脱液,将洗脱液过氧化铝柱吸附除杂,氧化铝用量为0.5 g生药/g,中试放大实验平行3次,总皂苷的纯度分别为85.96%,84.53%,86.32%,RSD值为1.13%,出膏率分别为6.45%,6.57%,6.32%,RSD值为1.94%,优选的纯化工艺稳定可行,适用于工业生产。     

大孔吸附树脂分离纯化胡芦巴中总皂苷工艺

通过对11种大孔吸附树脂对比研究,筛选出了一种对胡芦巴中总皂苷具有最佳吸附解吸性能的树脂,并对该树脂的静态和动态吸附性能进行了研究,确定了树脂纯化总皂苷的工艺参数。结果表明,HPD-400A型树脂对总皂苷有良好吸附分离性能,Freundlich等温吸附模型较Langmuir模型更适宜描述树脂对胡芦巴总皂苷的吸附;吸附分离总皂苷的工艺条件:树脂柱径高比为1∶10,上柱液质量浓度为1.358 mg/mL,流速为2 BV/h,解吸流速1 BV/h,解吸液为体积分数60%的乙醇,洗脱剂用量为1.5 BV。经大孔树脂纯化前总固物中总皂苷质量分数为11.38%,纯化后总固物中总皂苷质量分数为42.76%,纯度提高了近4倍。     

大孔吸附树脂分离纯化荔枝核总皂苷的工艺研究

目的:研究D-101型大孔吸附树脂吸附提取荔枝核总皂苷的工艺条件及参数。方法:以荔枝核总皂苷为考察指标,研究不同浓度乙醇洗脱溶剂对其总皂苷分离纯化工艺条件的影响。结论:60%的乙醇为最佳的洗脱剂浓度。     

大孔吸附树脂纯化细梗香草总皂苷的工艺研究

筛选纯化细梗香草总皂苷的最佳大孔树脂,采用单因素试验和正交设计试验优化细梗香草总皂苷的大孔吸附树脂纯化工艺。结果表明,DM130型大孔树脂对细梗香草总皂苷的吸附性能良好,优化后的纯化工艺条件为:上样药液浓度0. 25 g生药·mL~(-1)(p H=8),上样流速4 BV·h~(-1),吸附0. 5 h,依次用蒸馏水、40%乙醇、70%乙醇洗脱4 BV,洗脱流速4 BV·h~(-1)。在此条件下,细梗香草总皂苷的洗脱率达92. 03%,纯度50. 37%。     

大孔吸附树脂分离纯化番石榴叶总皂苷的工艺研究

研究大孔吸附树脂分离纯化番石榴叶总皂苷的工艺条件.番石榴叶用70%乙醇回流提取后,上D101型大孔树脂,水洗后分别用30%,50%,70%乙醇洗脱,以番石榴叶总皂苷的洗脱率为指标,考察大孔树脂分离纯化番石榴叶总皂苷的吸附性能和洗脱参数.番石榴叶总皂苷主要富集于30%、50%乙醇洗脱液部分,大孔吸附树脂的吸附容量为17.53 mg·g-1,洗脱率达70.42%,而50%乙醇洗脱时总皂苷纯度可达55.68%,优选洗脱条件为用水洗去水溶性杂质,50%乙醇洗脱总皂苷.     

大孔树脂吸附分离无患子皂苷的研究

采用两次大孔树脂吸附分离工艺从无患子果皮中提取无患子皂苷,结果表明,通过丙酮沉降及正丁醇萃取,两次D101大孔树脂富集与纯化,得到的无患子皂苷纯度为90.27%。     

大孔树脂纯化萼翅藤总黄酮工艺

筛选纯化萼翅藤总黄酮的最佳树脂,并对影响这种树脂分离的主要因素进行研究,确定大孔树脂纯化总黄酮的最佳工艺参数。选择4种大孔树脂分别对萼翅藤总黄酮进行静态与动态吸附性能研究,考察影响分离的各种因素如上样液pH值、上样液质量浓度、上样量和洗脱剂体积分数等。HPD-450树脂分离效果最好,Langmuir等温吸附模型较Freundlich模型更适宜描述树脂对萼翅藤总黄酮的吸附,其吸附分离萼翅藤总黄酮的最佳工艺为:上样液pH值为5,质量浓度为0.6—0.8 mg/mL,上样量为3 BV(树脂床体积),洗脱液为体积分数70%的乙醇,洗脱剂用量为3 BV。经HPD-450树脂吸附分离后,总固物中总黄酮质量分数从20.23%提高到75.86%,纯度提高了3倍多,回收率为62.65%。     

大孔树脂富集纯化黄酮类化合物的研究进展

大孔树脂具有操作简便、回收率高、纯化效果好等特点,目前被广泛应用于黄酮类化合物的富集纯化。该文对近年来大孔树脂富集纯化黄酮类化合物的研究现状进行综述,分析和探讨影响大孔树脂富集纯化效果的因素,旨在为利用大孔树脂纯化黄酮类化合物的研究提供参考。     

HPLC-ELSD法同时测定黄芪中两种皂苷成分及大孔树脂纯化工艺研究

目前针对黄芪的皂苷的提取分离方法繁杂且效率较低,分析检测和质量控制基本是以某个化合物为基础,而鲜有将黄芪的不同组分同时测定的方法。建立同时检测黄芪皂苷Ⅱ及黄芪甲苷的HPLC-ELSD法,利用该分析方法对三种不同大孔树脂及不同洗脱条件的提取物皂苷成分含量进行评价,筛选出最佳吸附树脂及大孔树脂富集纯化条件,为黄芪的进一步开发利用提供可靠的提取纯化工艺方案以及分析检测手段,为黄芪的质量控制提供新的途径。     

大孔吸附树脂纯化百合皂甙的工艺研究

以百合中总皂甙质量分教为考察指标,用AB-8大孔吸附树脂纯化百合皂甙.采用正交实验法对纯化工艺进行优选,考察生药浓度、洗脱剂浓度、洗脱速率对百合中总皂甙提取率的影响.最佳工艺条件为:取溶胀后AB-8大孔吸附树脂20 mL、生药浓度O.7 g/mL、用10倍树脂体积ψ(乙醇)=70%以1.0滴/s的洗脱速率洗脱,百合皂甙样品中百合皂甙的质量分数为87.8%.     

大孔吸附树脂对喜树叶中喜树碱的纯化工艺研究

研究通过静态吸附/解吸实验对大孔吸附树脂进行筛选,优选AB-8大孔吸附树脂作为层析柱填料,并对其进行喜树碱纯化工艺研究;研究表明AB-8树脂对喜树碱的静态吸附率为95.31%;体积分数95%的乙醇静态解吸率为92.4%;最佳吸附条件为:上样液质量浓度为0.175mg/mL,上样液不调pH值,吸附流速为2BV/h,平衡吸附5h;最佳洗脱条件:体积分数95%乙醇,洗脱流速1BV/h,洗脱体积为8BV。在该工艺条件下,洗脱物中喜树碱质量分数为7.43%,洗脱率为83.1%。     

Static and dynamic studies of adsorption by four macroporous resins to enrich oridonin from Rabdosia rubescens

Oridonin, one of the active ingredients in Rabdosia rubescens(R. rubescens), has been reported to induce cell apoptosis and cell cycle arrest in many cancers. Conventional extraction methods tend to result in unsatisfied enrichment and poor quality of oridonin present in a given biomass. This paper aims to evaluate the performance and separation characteristics of four different macroporous resins to arrive at the most suitable methodology for the isolation and purification of high-quality oridonin. Static absorption kinetics, thermodynamic and dynamic adsorption were evaluated. HP-20 was selected for further study due to its high adsorption capacity of 32 mg·g~(-1) and desorption ratio with 98.5%. The pseudo-secondorder model was considered to be the most suitable for kinetic results, and Langmuir model was chosen to better describe the absorption thermodynamics. Under optimum conditions(flow rate of 4 ml·min~(-1),bed depth with 6 cm and initial concentration of 2.15 mg·min~(-1)), the effective content of oridonin increased from 33.9% to 79.1% in the dry extract with a recovery of 81% and the purity of oridonin improved from 76% to 93%. The results confirm that HP-20 provides an efficient method to purify most oridonin from R. rubescens.     

Separation of salidroside from the fermentation broth of engineered Escherichia coli using macroporous adsorbent resins

Salidroside (8-O-β-D-glucoside of tyrosol), a plant-derived natural product, is used for treatment of hypoxia, fatigue and aging diseases. The availability of salidroside is restricted since it is extracted from 3-5 years old Rhodiola roots, which grow very slowly in the cold region of northern hemisphere of Earth. Our laboratory has constructed an engineered Escherichia coli and established a fermentation process to produce salidroside from glucose. In this article, nine macroporous resins from polarity to non-polarity, including NKA-9, S-8, AB-8, SP825, D101, LSA-8, LX-12, LX-18 and LX-68 resins, were tested to separate salidroside from fermentation broth. After static and dynamic experiments, the weakly polar SP825 resin had a better separation efficiency among nine resins. The adsorption kinetic and isotherm of salidroside on the SP825 resin were determined, and the pseudo-second-order kinetic model and Langmuir model could be fitted well. The effects of the pH on adsorption and ethanol concentration on desorption were investigated, and an optimal separation process was established. The adsorption for salidroside in the SP825 resin column was conducted with loading 150 ml at pH 7, and desorpted by washing 50 ml of 80% ethanol solution. Under the best process conditions, the purity and yield of salidroside in the final product were 91.6% and 74.0%, respectively. The results showed that the macroporous SP825 resin would be feasible and effective to prepare salidroside and has promising application in the downstream process of microbial fermentation.     

The performance of solid phosphoric acid catalysts and macroporous sulfonic resins on gasoline alkylation desulfurization

Sulfur removal has received increasing attention in recent years primarily for environmental protection purpose. As an attractive technology in the case of gasoline, OATS (olefinic alkylation of thiophenic sulfur) proposed to separate sulfur compounds by distillation after being weighed down by alkylation with olefins in the feed. In this paper, alkylation reactions of thiophenic compounds were studied over solid phosphoric acid catalysts (SPAM and SPAS using MCM-41 and Silicalite-1 zeolite as supporters respectively) and macroporous sulfonic resins (including NKC-9, D005-2 and Amberlyst 35) with model gasoline and FCC (fluid catalytic cracking) gasoline. Results showed that macroporous sulfonic resins showed better performance than solid phosphoric acid catalysts under milder conditions in both feeds. Among the resins, Amberlyst 35 was the most suitable catalyst for the application of catalytic distillation for its good performance at the temperature range of 353-413 K in FCC gasoline. However, the selectivity of isoamylene dimerization over Amberlyst 35 decreased with the temperature, which was harmful to the product yield and catalyst stability. Besides, different activity orders of solid phosphoric acid catalysts in model gasoline and FCC gasoline were explained by combining the acidic properties of the catalysts with the species of olefins in two feeds.     

大孔树脂分离纯化沙芥黄酮的工艺研究

用大孔吸附树脂分离纯化沙芥总黄酮,比较了7种大孔树脂对沙芥总黄酮的静态吸附动力学特性,优选出D-4020型大孔吸附树脂分离纯化沙芥总黄酮,并对其进行动态吸附实验。结果表明,D-4020纯化沙芥总黄酮的最佳工艺参数为:上样液浓度0.4 mg/mL,pH值5,上样流速2 mL/min;使用4BV用量95%的乙醇作为洗脱剂,洗脱流速为2 mL/min。采用该工艺分离纯化沙芥总黄酮含量达40.91%。     

竹节参总皂苷的纯化方法研究

比较了大孔树脂吸附与丙酮沉淀法对竹节参总皂苷的纯化效果。结果表明,大孔吸附树脂对竹节参总皂苷具有较好的纯化能力,D101大孔树脂对竹节参总皂苷的吸附能力最佳。最佳洗脱条件为:60%的乙醇洗脱,洗脱剂用量为3BV(BV为树脂体积倍数),洗脱流速为1 mL/min。该条件下竹节参总皂苷纯度可达88.12%(丙酮沉淀法64.30%)。     

大孔磺酸树脂催化合成7-羟基-4-甲基香豆素

考察了DT-852大孔磺酸树脂催化合成7-羟基-4-甲基香豆素的工艺。结果表明,DT-852大孔磺酸树脂具有较好的催化活性;7-羟基-4-甲基香豆素较佳的合成工艺为:反应温度105℃,反应时间2.5h,催化剂用量1.0g,物料比n(乙酰乙酸乙酯)∶n(间苯二酚)=1∶1,产率为93.8%,w(7-羟基-4-甲基香豆素)=98.3%(HPLC),催化剂可重复使用多次。产物结构经FTIR验证。     

大孔树脂富集诃子中没食子酸的工艺研究

考察了6种不同极性的大孔树脂对诃子中没食子酸的富集能力,发现极性树脂NKA-9的静态吸附能力和静态解析能力明显优于其它树脂。进一步考察了NKA-9树脂对诃子中没食子酸的静态吸附和动态吸附能力,结果表明其分离的最佳工艺为：没食子酸浓度为0.152 mg/mL的样品溶液、控制pH 3.0、温度25℃、以3 BV/h的流速上样、上样量为3 BV,上样后饱和吸附5 h;先用5 BV去离子水以3 BV/h的流速洗脱,再用7 BV的30%乙醇以2 BV/h的流速洗脱并收集,使提取物中没食子酸含量由4.7提高到25.3%,获得的回收率为82.6%。