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.     

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.     

Zn2＋型磺酸树脂对维生素B12的配位吸附及洗脱性能

原位吸附;分离;Zn2＋型磺酸树脂对维生素B12的配位吸附及洗脱性能     

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.     

离子交换法从发酵液中提取L-亮氨酸

用离子交换法提取发酵液中的L-亮氨酸,比较了不同型号的强酸性阳离子树脂对L-亮氨酸的静态吸附量和吸附动力学,其中以WA-2型树脂对L-亮氨酸吸附量最大、吸附速度快,适于L-亮氨酸的提取.测定了WA-2型树脂对L-亮氨酸的吸附等温线,并回归得到Freundlich方程.考察了固定床操作工艺条件,结果表明:发酵液经预处理后,以1BV/h流速上柱吸附,上柱量为2BV;再用0.3mol/L的氨水洗脱,速度为1BV/h,洗脱效果较好,L-亮氨酸回收率达到95.7%.提取过程中WA-2型树脂不会受到不可逆的污染,也没有机械损坏,其使用寿命不受影响.     

强碱性树脂IRA-400对富马酸吸附性能的研究

通过静态吸附试验,研究了强碱性树脂IRA-400对富马酸的吸附性能。结果表明,该树脂与弱碱性树脂IRA-94相比,受pH值影响较小,在pH=3.5时,该树脂对富马酸具有较好的吸附性能,其静态饱和吸附容量为1.466mmol/g湿树脂;该树脂对富马酸的吸附等温线符合Freundlich等温方程,在298.15K,308.15K和318.15K下的相关系数R2均大于0.99,方程的特征参数n1,属"优惠吸附";吸附过程ΔG0,ΔS0,ΔH0,表明此反应过程是放热的,自发进行的,降低温度有利于吸附反应的发生;吸附动力学研究表明,IRA-400树脂对富马酸的吸附过程主要受液膜扩散控制。     

Preparative separation of lithospermic acid B from Salvia miltiorrhiza by polyamide resin and preparative high-performance liquid chromatography

Adsorption on polyamide resin was investigated as a means of separating lithospermic acid B (LAB) from a crude extract of the roots of the traditional Chinese medicine Salvia miltiorrhiza Bunge ("Danshen"). Variables affecting adsorption capacity (solution pH, contact time on resin, initial LAB concentration) were studied. Adsorption was strongly dependent upon the initial concentration of LAB and pH. In all conditions, the polyamide resin gave optimal adsorption of LAB at an initial concentration of 2.66 mg/mL and pH <3.0. The adsorption isotherm correlated well with the Langmuir-type adsorption isotherm. Maximal adsorption capacity was calculated to be 380 mg/g at pH 2.0 and 25°C. LAB purity of 85.30% could be obtained by polyamide resin adsorption followed by elution with 70% ethanol solution, and the recovery was 87.1%. After preparative HPLC, the maximum HPLC purity obtained was 99.28% with a recovery of 75.2%. This method provides an efficient and low-cost method for LAB purification for industrial applications.     

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。     

大孔吸附树脂对熊果酸吸附性能的研究

研究了从山楂叶中纯化熊果酸的柱层析工艺。静态吸附结果表明,X-5、NKA和AB-8树脂的吸附率分别为91.32%,72.28%和41.19%;以90%乙醇为洗脱剂,X-5、NKA和AB-8树脂的洗脱率分别为83%,70%,87%。静态实验表明X-5树脂具有较好的吸附解吸性能。动态实验优化了在X-5树脂中的流速、上样液的熊果酸浓度和上样体积。结果表明,流速为3BV/h(BV为倍量体积),上样液的熊果酸浓度为0.304mg/mL,上样体积为3BV为最优上样条件。动态洗脱中采用梯度洗脱方式,结果表明在90%的乙醇洗脱下,熊果酸纯度达93.21%。对层析工艺制备的熊果酸进行结晶处理,所获得的熊果酸纯度为98.61%,与熊果酸标准品的红外光谱一致。     

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。     

Preliminary extraction of tannins by 1‐butyl‐3‐methylimidazole bromide and its subsequent removal from Galla chinensis extract using macroporous resins

In recent years, ionic liquids have become increasingly attractive as ‘green solvents’ used in the extraction of bioactive compounds from natural plant. However, the separation of ionic liquid from the target compounds was difficult, due to their low vapour pressure and high stabilities. In our study, ionic liquid‐based ultrasonic and microwave‐assisted extraction was used to obtain the crude tannins, then the macroporous resin adsorption technology was further employed to purify the tannins and remove the ionic liquid from crude extract. The results showed that XDA‐6 had higher separation efficiency than other tested resins, and the equilibrium experimental data were well fitted to Langmuir isotherms. Dynamic adsorption and desorption were performed on XDA‐6 packed in glass columns to optimise the separation process. The optimum conditions as follows: the ratio of column height to diameter bed was 1:8, flow rate 1 BV/h (bed volume per hour), 85% ethanol was used as eluant while the elution volume was 2 BV. Under the optimised conditions, the adsorption and desoption rate of tannins in XDA‐6 were 94.81 and 91.63%, respectively. The content of tannins was increased from 70.24% in Galla chinensis extract to 85.12% with a recovery of 99.06%. The result of ultra‐performance liquid chromatography (UPLC)‐MS/MS analysis showed that [bmim]Br could be removed from extract.     

ADSORPTION AND DESORPTION OF DSD ACID MANUFACTURING WASTEWATER ON MACROPOROUS RESIN

4,4‘-diaminostilbene-2,2‘-disulfonic acid (DSD acid) manufacturing wastewater was treated by a macroporous resin in a fixed-bed column.The results showed that this method was suitable for removal of chemical oxygen demands(COD) and color,About 91% COD and 99.5% color removal were obtained under the optimum adsorption conditions.i.e.temperature 20℃,flow rate lbed volume/hour(BV/hr)and pH1-2.The resin was efficiently regenerated with aqueous sodium hydroxide and water.Furthermore,65.5% of 4,4‘-dinitrostilbene-2,2‘-disulfonic acid(DNS) could be recovered from wastewater for possible recycling to the manufactureing process.The adsorption capacity of resin remained constant during the repetition process of adsorption and desorption.     

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.     

酚醛型吸附树脂对VB_(12)的吸附性能研究

研究了酚醛型吸附树脂JDW 1、JDW 2 (自制 )和DuoliteS 76 1对VB12 的静态和动态吸附 .结果表明 ,JDW 1对VB12 的吸附量达 84mg g ,明显优于DuoliteS 76 1;吸附VB12 的初始阶段 ,即达到 4 3%～6 9%平衡吸附时 ,吸附速率数据和半经验速率方程很吻合 ;酚醛型吸附树脂等温吸附VB12 的平衡吸附数据符合Langmuir方程 ,相关系数在 0 99以上 ,因此 ,酚醛型吸附树脂吸附VB12 属单分子层吸附 ;在动态条件下 ,用含甲醇 80 %溶液以 1 1BV h来洗脱吸附VB12 的JDW 2 ,在 4 2、6 4个床体积的洗脱率分别是 92 2 0 %、95 93% ,这表明酚醛型吸附树脂具有良好的洗脱性能 ,用含甲醇为 80 %溶液作洗脱剂从JDW 2洗脱VB12 ,效果很好     

Purification of L-Lysine in Simulated Moving Bed and Fixed-Bed Chromatography

 L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed （SMB） chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 g/(g·h) (per gram resin and per hour) at an eluent flow rate of 10 mL/min in fixed-bed chromatography. The results obtained from SMB were 0.11 g/(g·h) for L-lysine purification rate and 96% for L-lysine recovery.     

Synthesis of molecularly imprinted polymer nanoparticles for the fast and highly selective adsorption of sunset yellow

Novel molecularly imprinted polymer nanoparticles were synthesized by precipitation polymerization with sunset yellow as the template and [2‐(methacryloyloxy)ethyl] trimethylammonium chloride as the functional monomer. The molecularly imprinted polymer nanoparticles were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy, and their specific surface area and thermal stability were measured. The molecularly imprinted polymer nanoparticles had a high adsorption capacity in wide pH range (pH 1–8) for sunset yellow. The adsorption equilibrium only needed 5 min, and the quantitative desorption was very fast (1 min) by using 10.0 mol/L HCl as the eluant. The maximum adsorption capacity of the molecularly imprinted polymer nanoparticles for sunset yellow was 144.6 mg/g. The adsorption isotherm and kinetic were well consistent with Langmuir adsorption model and pseudo‐second‐order kinetic model, respectively. The relative selectivity coefficients of the molecularly imprinted polymer nanoparticles for tartrazine and carmine were 9.766 and 12.64, respectively. The prepared molecularly imprinted polymer nanoparticles were repeatedly used and regenerated ten times without significant absorption capacity decrease.     

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．     

Suitability of teicoplanin-aglycone bonded stationary phase for simulated moving bed enantioseparation of racemic amino acids employing composition-constrained eluents

The suitability of a teicoplanin-aglycone based chiral stationary phase for the simulated moving bed (SMB) enantioseparation of amino acids under enzyme-compatible conditions was shown following a procedure that is based solely on model-based simulations and HPLC experiments. A set of eight amino acids could be separated employing aqueous solvent containing only 10% (v/v) methanol, five of them with baseline resolution. The impact of type and concentration of organic modifier and pH modifier and pH on the separation characteristics of racemic methionine was investigated. Invariant elution profiles of repetitive adsorption/desorption of large amounts of methionine representing SMB-like conditions suggest stable adsorption behavior. Competitive loading capacity (20 mg of methionine per g of chiral stationary phase (CSP)) and SMB productivity (1 g of D-methionine per g of CSP per day) were predicted. The applied transport-dispersive model based on a competitive Bi-Langmuir isotherm was validated and its parameter estimated by model-based experimental analysis.     

离子交换法从发酵液中提取聚苹果酸

用离子交换法提取发酵液中的聚苹果酸,比较了不同型号的阴离子树脂对聚苹果酸的静态吸附量,其中以D296树脂对聚苹果酸的吸附量最大.通过静态和动态方法,考察了不同操作条件对固定床分离工艺的影响.结果表明,发酵液经预处理后,调pH至9.5,以lBV/h流速上柱吸附,上柱量为4BV;用0.5mol/L NaCl洗脱,速度为1BV/h.该工艺能够将发酵液中大部分杂质去除,PMLA样品的纯度达到 93.2%,提取收率为79.46%.