离子交换树脂对白扦中莽草酸的分离纯化

建立了离子交换树脂分离纯化白扦中莽草酸的工艺条件和参数。通过研究D261、D296、D301-R、D301-G、D290、201*7(717)、D201和D280共8种离子交换树脂对莽草酸的吸附和解吸附能力,筛选出最佳树脂为D290,确定了最佳的吸附与解吸附工艺参数,吸附条件为pH=6、25 ℃、流速为3 mL/min;脱附条件为：洗脱液为2.5%NaOH水溶液,洗脱流速为3 mL/min。莽草酸样品溶液经D290树脂吸附与脱附后回收率为92.53%,纯度由2.97%提高到46.76%,提高了15.74倍。实验结果表明,D290树脂对莽草酸的吸附量大,脱附容易,可以应用于莽草酸的分离纯化。     

Process research of macroporous resin chromotography for separation of N-(p-coumaroyl)serotonin and N-feruloylserotonin from Chinese safflower seed extracts

N-(p-Coumaroyl)serotonin (CS) and N-feruloylserotonin (FS) are two bioactive serotonin derivatives in safflower (Carthamus tinctorius L.) seeds with many biological effects. In the present study, the sorption and desorption characteristics of six widely used macroporous resins, coded D312, 860021, DM131, HZ801, AB-8 and XDA-1, respectively, is critically evaluated and compared for enrichment and preparative separation of CS and FS. Static adsorption and desorption experiments on these resins showed that XDA-1 had the best adsorption and desorption equilibrium for CS and FS, and its adsorption equilibrium fits the best to the Langmuir isotherm. Dynamic adsorption and desorption experiments on XDA-1 resin packed column were conducted to establish the optimum parameters as: CS and FS concentration in sample solution 0.346 and 0.276 mg/mL, respectively, sample size 5-bed volumes (BV), sample flow rate 2 mL/min, temperature 25 °C (for adsorption); eluent 80% ethanol, 11 BV, flow rate 1 mL/min (for desorption). After one run of adsorption and desorption, the contents of CS and FS were increased from 2.01%, 1.67% to 24.1% and 22.4%, and the recoveries were 77.2% and 68.5%, respectively. The chromatographic process optimized in the present work is a promising basis for large scale preparation of CS and FS upon further scaling up tests.     

大孔树脂对甘草酸的吸附纯化

从3种树脂中选择了D-101树脂为纯化甘草酸的最佳树脂。考察了各种因素对D-101树脂吸附和洗脱甘草酸的影响。实验结果获得吸附最佳条件为：上样液pH值6-8,甘草酸浓度5．710mg／mL,流速为1mL／min;洗脱最佳条件为：乙醇洗脱剂浓度50％和洗脱液流速1mL／min。洗脱产物甘草酸纯度最高达82．38％。     

大孔树脂法分离纯化申嗪霉素的工艺研究

通过大孔吸附树脂对申嗪霉素发酵滤液静态吸附和解吸试验,从6种大孔吸附树脂中筛选出分离纯化申嗪霉素最优的树脂,考察了该树脂对申嗪霉素的静态、动态吸附与解吸性能并对吸附与洗脱的最佳条件进行了研究。结果表明:AB-8树脂对申嗪霉素有很好的吸附和解吸性能,其最优的动态吸附工艺条件为:上样液浓度3 000μg/mL,上样量4 BV,上样流速2 BV/h;最优的解吸条件为:洗脱剂为80%乙醇溶液,洗脱液用量3 BV,洗脱流速1 BV/h。在此优化条件下,申嗪霉素的吸附率、解吸率、收率、纯度的平均值分别达到(90.33±0.14)%、(90.87±0.12)%、(82.1±0.1)%和(90.74±0.14)%(n=5)。     

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.     

离子交换树脂法吸附醋酸工艺

采用离子交换树脂法吸附醋酸溶液,并对该过程进行系统的研究. 通过树脂选型确定大孔弱碱性阴离子交换树脂D311,其对醋酸吸附容量较大,且膨胀收缩率较小. 用D311树脂对醋酸含量为1.5%(w)的醋酸溶液进行了吸附和脱附工艺优化研究,考察了体系温度、进料流量等对吸附和脱附过程的影响,在优化条件为温度30.0℃、进料流量4.0 mL/min时,吸附率达93.97%;温度50.0℃、洗脱剂3.98 mol/L NaOH、流量1.0 mL/min时,脱附率达100%. 树脂再生循环结果表明,D311重现性及机械强度较好.     

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%。     

大孔树脂吸附法吸附分离黄酮的研究

研究了D101、LD601、LS-303B、LX-28、LX-38型大孔树脂对黄酮的吸附及分离性能。结果表明,LD601型大孔树脂对黄酮的吸附效果较好,pH 2～4的盐酸溶液中,静态吸附量为5 849.312μg/g,对流速2 mL/min黄酮溶液的吸附率可达96.27%,负载1 500μg黄酮的LD601树脂,用40%乙醇50 mL以3 mL/min流速进行解吸,解吸率可达97.51%。     

大孔树脂纯化栾树叶多酚工艺研究

以栾树叶多酚提取物为原料,比较了7种大孔树脂对栾树叶多酚的静态吸附与解吸效果,结果表明AB-8树脂性能最佳,其24h静态吸附量为13.74mg/g,解吸率为98.35%,3h内达到吸附平衡与解吸平衡。AB-8树脂动态吸附较佳条件为上样液质量浓度为4g/L,上样液pH值为6,在此条件下吸附率为88.21%,动态洗脱较佳条件为洗脱剂乙醇体积分数为60%,洗脱速度为1mL/min,解吸率达到89.91%,在该条件下栾树叶总多酚经AB-8树脂纯化后,质量分数由50.36%增加到72.37%,回收率为86.83%。     

地黄中梓醇的超声提取-树脂分离纯化工艺

研究了地黄中梓醇的超声提取-树脂分离纯化工艺。结果表明,超声提取的最佳工艺条件为：提取溶剂采用68%（体积）的乙醇,液料体积(ml)质量(g)比5:1,超声时间36 min。考察了10种大孔树脂对地黄粗提液的分离纯化效果,其中以H103对梓醇的纯化效果最佳。通过实验进一步考察了H103的动态吸附性能,得到分离纯化的最佳工艺条件为：上柱液浓度为6.15 mg·ml^-1,上柱液流速为1.0 ml·min^-1,洗脱剂为75%乙醇,洗脱流速为0.5 ml·min^-1,洗脱体积为3.33 BV（bed volume）。提取、纯化两步操作后梓醇纯度达到62.39％。     

大孔吸附树脂分离纯化马缨丹总黄酮的工艺研究

探讨大孔吸附树脂纯化马缨丹总黄酮的最佳工艺,通过对4种型号大孔树脂的静态实验,筛选出最佳树脂;考察最佳树脂对马缨丹总黄酮的吸附及洗脱性能,优化工艺参数。结果表明:AB-8为最佳树脂,其最佳工艺条件为:上样液质量浓度0.198 mg/mL,吸附流速为2.0 mL/min,吸附pH为4.0;洗脱剂为70%乙醇,洗脱用量5 BV,减压浓缩得马缨丹总黄酮浸膏,纯度为32.45%。     

大孔树脂纯化废次烟叶中烟草多酚的工艺

通过吸附和解吸附实验,从6种大孔树脂中筛选出适于分离纯化废次烟叶中烟草多酚的大孔树脂,并确定该大孔树脂纯化工艺参数。结果显示,D101大孔树脂能够较好的富集纯化废次烟叶中的烟草多酚,当提取液浓度为2.5 mg/mL,pH值为4.0,上样液流速为2.0 mL/min,洗脱液为80%乙醇溶液,洗脱液流速为2.0 mL/min时,纯化效果最好,烟草多酚的动态回收率为70.37%。     

大孔吸附树脂分离纯化猪毛菜总黄酮及其抗氧化活性

采用不同大孔吸附树脂分离纯化猪毛菜总黄酮,并对纯化后的总黄酮进行体外抗氧化活性测试。通过考察影响树脂静态和动态吸附与洗脱的主要因素,确定猪毛菜总黄酮分离纯化优化工艺条件。静态吸附实验表明,AB-8树脂分离纯化效果较好,并且吸附符合Langmuir和Freundlich方程。动态吸附和解吸的最佳工艺条件为:上样液质量浓度1.25 g/L、p H=4.5、上样流速2 m L/min、上样量2.5 BV(BV指树脂柱内装载树脂的体积)、洗脱剂为体积分数80%的乙醇溶液、洗脱流速1.0 m L/min,洗脱剂用量4 BV。所得洗脱液中黄酮质量分数从纯化前10.20%增加到纯化后51.89%,回收率为84.43%。体外实验表明,纯化后的黄酮可以清除羟自由基和超氧阴离子自由基,并有较好的还原力。纯化后的黄酮可以作为一种潜在的天然抗氧化剂。     

大孔吸附树脂纯化芹菜黄酮的研究

研究6种大孔吸附树脂对芹菜黄酮类物质的吸附和解吸性能,筛选出吸附率较高的XAD-16树脂,并对XAD-16树脂静态吸附和动态吸附解吸工艺做了研究。优化出XAD-16树脂纯化芹菜黄酮的最佳工艺参数为：室温下吸附;上样流速4 BV/h,在上样浓度0.55 mg/mL下,上样体积为15倍柱床体积;洗脱溶剂采用体积分数50%的乙醇,洗脱流速为6 BV/h,洗脱液量为4倍柱床体积。     

树脂法精制蜂胶高生物活性黄酮醇

考察了5种树脂对蜂胶中的水溶性黄酮醇的吸附和洗脱性能。以质量分数为65%的乙醇为提取剂,提取温度为38℃,以质量分数为60%的乙醇洗脱,通过比较吸附量、洗脱率以及所得水溶性黄酮醇的含量,最后得出以V(D4020)∶V(聚酰胺)=2∶1的混合型树脂为最佳选择。采用该种树脂,水溶性黄酮醇的最大吸附量为32.76mg/mL,洗脱率为94.68%,提取率为8.27%。     

茶皂素提取条件的优化及纯化研究

以油茶茶籽粕为原料，采用乙醇水溶液提取茶皂素。在茶籽粉和乙醇料液比1 : 9(g : mL)，乙醇体积分数60%，提取温度60 ℃和提取时间3 h的最佳条件下茶皂素的提取得率达14.9%。用NKA-9型大孔吸附树脂吸附纯化茶皂素粗品，树脂静态吸附与解吸结果表明：树脂静态吸附茶皂素粗提液0.5 h基本饱和，体积分数80%乙醇解吸率为91.1%；动态吸附与解吸时，上样流速8 mL/min较佳，吸附率为66.04%，体积分数80%乙醇洗脱，洗脱流速5.0 mL/min，洗脱体积50 mL时，可使流出液中茶皂素质量浓度在1.25~1.57 g/L之间，茶皂素纯度为95%。     

大孔吸附树脂纯化黄花蒿黄酮及其抗氧化活性

该文对大孔吸附树脂纯化黄花蒿黄酮的工艺条件进行了研究与优化,并对纯化后的黄酮进行了抗氧化活性的研究。比较了AB-8,DM-101,DA-201,D-101及SD-401对黄花蒿中黄酮类物质的吸附及解吸附性能,结果显示,D-101的综合效果最佳。通过D-101大孔吸附树脂动态吸附解吸实验,获得较佳的纯化工艺:上样液黄酮质量浓度为1.55 g/L,流速为2 mL/min,上样100 mL后,用蒸馏水洗脱至溶液无色,再用250 mL体积分数70%乙醇以1 mL/min洗脱。在该条件下,黄酮质量分数从20.10%提高到80.32%,洗脱率达91.08%,黄酮回收率为68.25%。黄花蒿黄酮对油脂有明显的抗氧化性作用;黄花蒿黄酮对植物油的抗氧化能力强于柠檬酸和抗坏血酸,对动物油脂的抗氧化能力稍弱于抗坏血酸而略强于柠檬酸。     

AB-8大孔树脂对1,2-环己二醇动态吸附性能研究

针对双氧水氧化环己烯合成环氧环己烷的反应体系,采用大孔树脂动态吸附分离反应液水相中的1,2-环己二醇。结果表明,在自行设计吸附柱的基础上,AB-8大孔树脂吸附分离反应液水相中1,2-环己二醇的较佳条件为：上样流速1.0 mL/min,床层高度4.0 cm,常温;通过固定床吸附数学模型得到的速率常数、相关系数、吸附量和动力学参数, 能较好地描述AB-8大孔树脂固定床吸附1,2-环己二醇的吸附动力学。以乙酸乙酯为脱附剂进行脱附较佳条件为：洗脱流速1.0 mL/min,常温;AB-8大孔树脂经5次循环使用后其吸附率和脱附率仍在80％以上。     

Enrichment and Purification of Syringin, Eleutheroside E and Isofraxidin from Acanthopanax senticosus by Macroporous Resin

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol-water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively.     

树脂吸附法从含钼废水中回收制备三氧化钼

采用A325树脂对某含钼废水进行吸附,回收废水中的钼并制得了三氧化钼产品。整个过程分为废水中钼的吸附、解吸、除杂净化和三氧化钼的制备等几个步骤。在钼的吸附过程中,当原料液钼浓度2．8g／L时,适宜的工艺条件是：v（料液）：v（树脂）=45：1,料液pH值为3．0、料液温度25±2℃、料液流速10mL／min,钼的吸附率可达到94.3％。解吸时,采用10％的氨水溶液作为解吸液,口（解吸液）：v（树脂）=2：1进行配料。富钼解吸液再经除杂净化、酸化沉淀、过滤、洗涤、烘干、煅烧,制得三氧化钼产品。