大孔吸附树脂法纯化槐米中芦丁的工艺研究

采用AB-8大孔吸附树脂法分离纯化槐米水提取物中的芦丁,利用紫外分光光度法测量芦丁的浓度,计算其收率和含量。考察了加样时吸附液体积、pH值、流速以及洗脱时解吸液浓度、温度、流速等因素对芦丁收率的影响。大孔吸附树脂纯化槐米中芦丁的最佳条件为:加样时吸附液体积为1900mL,pH值为4～5,吸附液流速10mL/min;洗脱时采用70%的酒精水溶液作解吸液,解吸温度为70℃,流速为10mL/min左右。获得的芦丁产品相对于原料槐米的收率为17.6%,含量为99.06%。     

大孔吸附树脂纯化右旋龙脑的工艺研究

研究洗脱剂乙醇体积分数、洗脱流速、上样液浓度对D101大孔吸附树脂纯化右旋龙脑效果的影响,确立右旋龙脑纯化工艺。通过单因素考察实验和正交实验,确立的最佳工艺条件为:洗脱剂乙醇体积分数为80%,洗脱流速为3.5 BV/h,上样液浓度为0.55 g/mL。在此条件下,右旋龙脑收率可达81.6%,纯度为98.32%。考察的因素对分离效果的影响程度为:洗脱剂乙醇的体积分数洗脱流速上样液浓度。建立的右旋龙脑精制工艺操作简便、收率高,适合扩大化生产。     

不同型号大孔吸附树脂对枸杞多糖纯化工艺影响的研究

探索HPD300、AB-8、HPD100、DM301、D101五种不同型号大孔吸附树脂对枸杞多糖纯化工艺的影响。将水提法与大孔吸附树脂相结合,采用静态吸附法,以除杂率和多糖保留率作为评价指标,比较对枸杞多糖纯化效果的影响。结果表明,在同等条件下,HPD300大孔吸附树脂对枸杞多糖的除杂率和保留率较为理想。     

大孔吸附树脂纯化杏仁皮单宁工艺的研究

通过静态吸附及解吸实验,考察5种大孔吸附树脂对杏仁皮单宁的吸附及解吸性能,确定效果最佳的大孔吸附树脂。考察上样浓度、上样流速、上样量对吸附性能的影响,乙醇浓度、洗脱流速、洗脱液用量对解吸性能的影响。结果表明,最佳纯化条件为:采用HP-20型大孔吸附树脂,上样液浓度为1.20 mg/mL,上样流速为1 BV/h,上样量为4 BV,洗脱液为70%乙醇溶液,洗脱液用量为3 BV,洗脱流速为1.5 BV/h。在此条件下,杏仁皮单宁纯度由9.97%提高到32.58%。表明HP-20型大孔吸附树脂纯化杏仁皮单宁工艺可靠、效果良好。     

大孔吸附树脂纯化石榴皮多酚

从D3520、D4020、AB-8、D140、D141、D160、DM-301、DA-201、SAD-7和D101大孔吸附树脂中筛选出D141树脂,研究了其对石榴皮多酚的静态与动态吸附和解吸性能。结果表明,D141树脂对石榴皮多酚的饱和吸附量为19.86 mg/g(干树脂),吸附等温线符合Langmuir方程,饱和吸附时间为5 h,适宜解吸剂为体积分数70%的乙醇溶液;以质量浓度9 mg/mL的石榴皮提取液上柱,流速为1.8~2.0 BV/h时,树脂的多酚穿透吸附容量为39.42 mg/g(干树脂),2.5 BV体积分数70%的乙醇溶液可将吸附于柱上的石榴皮多酚完全洗脱。以该条件纯化石榴皮多酚提取物时,纯化样的收率为15.4 g/100 g(石榴皮),多酚质量分数从34%提高到76.34%。     

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%.     

大孔吸附树脂分离纯化银杏叶总黄酮的研究

利用4种大孔吸附树脂分离纯化银杏叶总黄酮.结果表明,HPD100型大孔吸附树脂最适合分离纯化银杏叶总黄酮,该树脂的静态饱和吸附量(以干树脂计)为63.8 mg·g-1,静态洗脱率为91.2%,动态饱和吸附-洗脱量为14.0 mg·g-1,洗脱剂为70%乙醇,洗脱剂用量为4倍树脂体积,树脂可重复使用7个周期.     

大孔吸附树脂纯化化香树果序总黄酮工艺研究

以吸附量和解吸率为指标对9种大孔吸附树脂进行对比,H-327B是分离纯化化香树总黄酮的理想树脂;热力学、动力学研究表明,Langmuir模型描述化香树果序黄酮在大孔树脂上的吸附规律更为适宜,该吸附属单分子层吸附,提高温度有利于吸附的进行,吸附过程可自发进行;对吸附?解吸工艺条件优化研究表明:当上样质量浓度为8.9 mg/mL、流速为3 BV/h时,H-327B型树脂对化香树果序总黄酮的吸附量较大。采用体积分数90%乙醇水溶液进行洗脱时,用5 BV乙醇洗脱,解吸率达到65%。     

大孔树脂吸附纯化葡萄籽原花青素的研究

采用大孔树脂对葡萄籽原花青素进行吸附纯化,以吸附率和解吸率及纯化效果为指标,比较了7种大孔树脂对原花青素的吸附解吸性能。研究了上样量、洗脱剂浓度、上样流速、洗脱剂用量对原花青素纯化效果的影响。结果表明,AB-8大孔树脂对葡萄籽中原花青素的吸附效果最好,树脂体积为20 mL,上样量为80 mL,上样流速为40 mL/h,用40%的乙醇洗脱,洗脱剂用量为100 mL,洗脱流速为80 mL/h时的纯化效果最好,该条件下原花青素洗脱率为94.37%,所得溶质纯度可达89.63%。     

大孔吸附树脂分离纯化普那霉素的研究

用大孔吸附树脂法代替溶媒萃取法分离纯化普那霉素。将普那霉素发酵液预处理后,以大孔吸附树脂XAD1600作吸附剂,在吸附流速为2 BV·h-1的条件下进行吸附;再用40％乙醇—60％酸水(含0.1％的乙酸,下同)进行洗脱,去除色素和杂质;最后用90％乙醇—10％酸水以0.5 BV·h-1流速进行洗脱。得到的普那霉素含量达...     

大孔树脂分离富集匙羹藤总皂苷研究

采用大孔树脂对匙羹藤总皂苷进行分离富集.考察了5种树脂对匙羹藤总皂苷的静态吸附效果并筛选出D101树脂用于分离富集匙羹藤总皂苷,通过动态吸附性能考察,确定了D101树脂固定床分离富集匙羹藤总皂苷的工艺条件,在ρ(总皂苷)=5 mg/mL,pH=6,料液以1.0 mL/min的流速通过D101树脂固定床进行吸附,分别用去...     

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.     

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.     

Ultrasonic-assisted reductive extraction of matrine from sophorae tonkinesis and its purification by macroporous resin column chromatography

In this work, ultrasonic-assisted reductive extraction of matrine from Sophorae tonkinesis was studied for the first time. During this process, sodium metabisulfite was added as a reducing agent in order to covert maximum amount of oxymatrine, sophocarpine, and oxysophocarpine to matrine. After optimization by response surface methodology, the extraction yield of matrine was found to be 2.03%, much higher than the yield obtained through traditional extraction method. After filtration, H103-macroporous adsorption resin column chromatography, concentration, and recrystallization, matrine with 98.2% purity was obtained.     

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.     

Preparative separation and purification of rosavin in Rhodiola rosea by macroporous adsorption resins

Rosavin is one of the main bioactive components in Rhodiola rosea L. with known pharmacological effects. In this study, a simple method for preparative separation and purification of rosavin from R. rosea L. was developed with macroporous adsorption resins. The adsorption isotherms and desorption performances of some resins have been determined and compared. Depending on its hydrophobic force, HPD-200 resin, a styrene-divinylbenzene (SDVB) copolymer, offers the best adsorption and desorption properties for rosavin based on the research results, its adsorption data fit best to the Langmuir adsorption model. Dynamic adsorption and desorption was performed on HPD-200 resin packed in a glass column to obtain optimal parameters for the separation of rosavin. The optimum conditions were as follow. The volume, concentration, bed height and flow rate of loading sample were 4 bed volumes (BV), 0.24 mg/mL, 30 cm and 2 BV/h, respectively, at 25 °C; desorption was performed successively with 30% ethanol of 4 bed volumes, 40% ethanol of 2.5 bed volumes and 60% ethanol of 3 bed volumes. After one run treatment with HPD-200, the rosavin content in the product was increased from 0.69% to 11.02% with a recovery of 82.46%. In this case, the process throughout is 1.34 g rosavin/L adsorbent/day, solvent usage is 7.14 L ethanol/g rosavin. The simple purification scheme avoids toxic organic solvent and thus, increases the safety of the process with a potential industrial application prospect.     

分子量可控乙烯基MQ硅树脂制备工艺研究

通过正硅酸酯法制备了分子量可控乙烯基MQ硅树脂,并对其制备工艺条件进行了研究。反应适宜的操作条件为:M单元与Q单元的摩尔比(M/Q值)0.9,水与乙氧基摩尔比0.8,乙醇的起始加入质量为加入反应体系中物质总质量的10%,盐酸质量占总进料质量的1%,回流时间2 h,水解反应温度75℃。此条件下得到的乙烯基MQ硅树脂分子量适中,有利于后续操作。     

Separation of glycyrrhizic acid from licorice root extract using macroporous resin

Glycyrrhizic acid (GA) is the major active ingredient of licorice which has many pharmacological activities. In the present study, separation of GA from licorice root extract has been carried out by adsorption on five different macroporous resins. Static and dynamic adsorption of GA from crude licorice root extract is studied on ion exchange resins followed by desorption. Indion 810 shows the maximum adsorption as well as desorption capacity. The adsorption experiments indicate that equilibrium can be achieved in 360 min. The adsorption equilibrium data is well fitted in the Langmuir isotherm. The separation process is optimized by investigating the effect of pH on adsorption capacity and effect of concentration of ethanol on desorption capacity. The dynamic adsorption is carried out in a column packed with Indion 810 resin and effect of feed flow rate and initial concentration of GA in extract has been studied. The results showed that increase in feed flow rate as well as initial feed concentration of GA lowers the dynamic binding capacity and mass transfer coefficient while increases the HETP. The purity of GA is increased from 14.3% to 71.5% by the dynamic desorption with 60% ethanol. Indion 810 resin can efficiently separate GA from licorice root extract with the HPLC recovery of 63.6%. This study forms the basis for large scale preparation of GA by resin adsorption.