阴离子交换层析法纯化聚唾液酸工艺

以大肠杆菌发酵所产聚唾液酸粗品(含蛋白质、核酸、无机盐和色素等杂质)为纯化对象,通过静态吸附和梯度洗脱实验选择了分离效果较好的阴离子交换介质Q-琼脂糖凝胶FF,对聚唾液酸的纯化工艺条件进行优化. 得到最佳洗脱条件为：洗脱液为pH 7.2的NaCl-0.02 mol/L磷酸钠缓冲液体系,流速0.8 mL/min,洗脱线性梯度方程为CNaCl=0.0017VEluent (CNaCl为NaCl浓度,VEluent为洗脱液体积),层析柱体积46 mL时最大进样量4.0 mL. 该条件下聚唾液酸回收率在86.0%以上,纯化后样品中的蛋白质含量从1.9%降低至0.04%,纯度在98%以上. 紫外吸收光谱和高效凝胶过滤色谱分析表明,聚唾液酸产品组分均一,重均分子量为303 kDa.     

Integrated Expanded-Bed Ion Exchange Chromatography as a Tool for Direct Recovery of Shikimic Acid from Illicium verum

Shikimic acid (SA) is the drug lead of oseltamivir phosphate (Tamiflu®). The pharmaceutical industry has great demand for SA to match the production of the drug. This article describes the development of an integrated expanded-bed adsorption chromatography (EBAC) system and its application in SA extraction and separation. The hydrodynamic behavior of an expanded-bed ion exchange resin, D293, was investigated to show that D293 resin is able to act as an adsorbent for recovery of SA from Illicium verum. SA was extracted from 8 g of I. verum in 150 mL of deionized water at an expansion ratio of 1.4 via integrated EBAC at 40°C. The SA was then eluted in 200 mL of a 2% NaCl solution. The recovery rate of SA was 96.7% and its purity was 59.6%. Different methods were compared, and the results indicated that the method developed in this article is promising for the recovery of SA from I. verum. The process efficiency of the integrated method was 2.6 times higher than that of the conventional method, while its energy efficiency was about 6 times of that of the conventional method.     

离子色谱法分离有效霉素中主要组分

建立的一种简单、有效的方法,以一种强碱性阴离子交换树脂为吸附剂,纯水为洗脱剂,利用自制的连续加压洗脱装置分离得到3种高纯度的有效霉素常量组分,这些组分中含有胺基环醇结构,是用于合成高附加值的α-糖苷酶抑制剂类抗糖尿病药物的重要中间体。     

应用离子交换树脂生产高纯度的癸二酸

介绍应用离子交换树脂工艺生产含铁量在PPM级的癸二酸。     

制备型氨基酸离子交换色谱的动态特性

为描述氨基酸离子交换色谱的动态过程，考虑传质机理，非线性离子交换平衡关系以及各种形式的进料函数，提出了色谱的机理模型及其数值解法，理论预测的洗脱峰与实验现象比较吻合，证明该理论模型可以指导氨基酸离子交换色谱的优化和设计。     

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.     

离子交换树脂在污酸净化中的应用

以烟气制酸排放污酸为研究对象,使用离子交换树脂脱出污酸中重金属。通过试验得出：该材料对重金属的脱出效率达到99.82%。当材料吸附饱和之后进行反冲洗脱附,脱附之后材料再次恢复吸附重金属之功能,从而开辟了一条污酸净化的技术途径。     

Optimal Integration of Directly Combined Hydrophobic Interaction and Ion Exchange Chromatography Purification Processes

Hydrophobic interaction and ion exchange chromatography are basic steps in purification of fermentative biopharmaceuticals. An optimization by statistical design of experiments requires a huge amount of feed. An alternative approach is the combination of model parameter determination using small scale experimental model parameter determination (1‐mL columns) and rigorous process modeling. Applicability for the prediction of the separation of a fermentation mixture of CHO mammalian cell culture is validated and hence IgG is purified from cell culture supernatant. Hydrophobic interaction chromatography directly combined with ion exchange chromatography is optimized. Any direct integration of those two main unit operations in purification processes is a methodological first step towards total process optimization. The potential for cost reduction and overall yield improvement is demonstrated and this leads to the conclusion that single step optimization is a feigned and not a real optimum.     

Cyanide Recovery from Gold Extraction Process Waste Effluents by Ion Exchange II. Modelling of the Fixed Bed Operation

Abstract

An ion exchange operation in a fixed bed column is tested as a method to recover copper cyanide complexes from gold extraction process waste effluents. With this aim in mind, load and elution breakthrough curves are obtained using the anionic resin Lewatit MP500. A good performance of the resin in the load stage can be deduced from the breakthrough curves obtained in all the assays at two different pHs (12, 8.5). After load step operation, column elution was carried out using NaSCN 1.25 M as eluent. A good elution peak is obtained in all cases, indicating a good performance of the resin and the eluent in this stage. With the aim of testing the design of the industrial operation, a phenomenological model is tested by fitting experimental data to theoretical equations. The model used for the simulation of both steps incorporates axial dispersion, ion exchange equilibrium, and diffusion inside particles described by the linear driving force approximation, as well as taking into account the fact that the resistance to mass transfer controls the kinetics of the ion exchange process. The models are able to simulate the experimental load and elution results reasonably well.     

扩散渗析法从钛白废酸中回收硫酸

针对钛白废酸的回收,在静态扩散条件下测定了硫酸、硫酸亚铁在阴离子交换膜中的渗析系数以考察膜的分离性能。进一步考察动态扩散操作参数如流量、流量比、停留时间等对回收率及回收酸浓度的影响。研究表明,使用的阴离子交换膜具有良好的分离性能,酸盐分离系数达23.6,在水酸流量比维持在1～1.1,废酸流量维持在0.6L·h-1左右的条件下,硫酸回收率大于85%,硫酸亚铁透过率小于7%。     

优化控制古龙酸离子交换工艺条件

控制好离子交换工艺条件,避免古龙酸溶液中出现钠盐,提高古龙酸收率和质量。     

离子交换法提取植酸的原理分析

离子交换法是一种先进的植酸生产方法,现从原理上对其整个生产中的酸浸、离子交换、脱色、浓缩等过程进行分析,以便能更好的指导生产。     

Removal of Alkaline Catalysts from Polyols by Ion Exchange

Abstract

Resin regeneration is crucial in the feasibility of polyol purification by ion exchange. In order to get an economically viable commercial process, a new regeneration process, including initial and final methanol flushing steps and treating with a 4.5 M aqueous mineral acid solution, has been investigated. An important reduction in regeneration costs was reached by minimizing the amount of acid used and recycling one part of the regenerant solution to the process. The composition of regeneration effluents has been studied in order to recover their valuable components. This simple resin regeneration technique lends itself to a technically and economically viable commercial process for the treatment of polyol products.     

Antioxidant Activity of Soybean Oil Containing 4-Vinylsyringol Obtained from Decarboxylated Sinapic Acid

4-Vinylsyringol was produced by decarboxylation from sinapic acid. To evaluate the antioxidant activity of 4-vinylsyringol, 500 ppm of 4-vinylsyringol, sinapic acid, or α-tocopherol was added to soybean oil and the oxidation processes were monitored by the peroxide value (PV), the thiobarbituric acid reactive substances value (TBARS) assay, and ¹H-NMR spectroscopy. The results obtained by PV and TBARS indicated that soybean oil containing 4-vinylsyringol (SBO-VS) showed the highest oxidative stability. ¹H-NMR analysis also showed concurring results. After 19 days of oxidation, the degradation rates of linoleic acid (4.2 %) and linolenic acid (4.4 %) in SBO-VS were significantly lower than those in other oils. Secondary oxidation products (i.e. aldehydes) were undetectable in SBO-VS by ¹H NMR, whereas concentrations of such compounds in soybean oils containing α-tocopherol or sinapic acid were 38.0 ± 0.4 and 2.75 ± 0.2 mM oil, respectively. In addition, synergistic antioxidant effect between any two antioxidants was not observed.     

离子交换法生产精制盐酸和高纯盐酸

总结了用离子交换树脂法生产精制盐酸和高纯盐酸的试验过程及规模生产的可行性,并根据试验结果,设计生产规模的工艺流程和装置。     

Gamma-Aminobutyric Acid Production Using Immobilized Glutamate Decarboxylase Followed by Downstream Processing with Cation Exchange Chromatography

We have developed a gamma-aminobutyric acid (GABA) production technique using his-tag mediated immobilization of Escherichia coli-derived glutamate decarboxylase (GAD), an enzyme that catalyzes the conversion of glutamate to GABA. The GAD was obtained at 1.43 g/L from GAD-overexpressed E. coli fermentation and consisted of 59.7% monomer, 29.2% dimer and 2.3% tetramer with a 97.6% soluble form of the total GAD. The harvested GAD was immobilized to metal affinity gel with an immobilization yield of 92%. Based on an investigation of specific enzyme activity and reaction characteristics, glutamic acid (GA) was chosen over monosodium glutamate (MSG) as a substrate for immobilized GAD, resulting in conversion of 2.17 M GABA in a 1 L reactor within 100 min. The immobilized enzymes retained 58.1% of their initial activities after ten consecutive uses. By using cation exchange chromatography followed by enzymatic conversion, GABA was separated from the residual substrate and leached GAD. As a consequence, the glutamic acid was mostly removed with no detectable GAD, while 91.2% of GABA was yielded in the purification step.     

离子色谱法测定硅氟酸中的硫酸根

采用离子色谱法对硅氟酸中的硫酸根进行测定。样品用盐酸挥发排除硅氟酸中的氟离子,采用883Basic IC Plus型离子色谱仪测定。方法的线性范围:0~20μg/m L,检出限:0.098μg/m L,,相关系数0.999,加标回收率在98%~103%之间。结果表明,此方法操作简单,分析速度快,准确,能满足生产需要。     

Separation and Purification of Sinigrin and Gluconapin from Defatted Indian Mustard Seed Meals by Macroporous Anion Exchange Resin and Medium Pressure Liquid Chromatography

Defatted seed meals, the byproducts of Indian mustard seed oil industry, which are just used as animal feedstock and nitrogen fertilizers, possess various nutrients and phytochemical compounds, such as sinigrin and gluconapin. The present study demonstrated a novel, low-cost, and efficient method for the co-production of sinigrin and gluconapin from defatted Indian mustard seed meals by D261 strong basic anion-exchange macroporous resin and medium pressure liquid chromatography (MPLC). The adsorption/desorption capacities of eight adsorbents characterized by BET, IR, and EDS were screened. 26.4 g defatted Indian mustard seed meals, which contained about 1210.3 mg sinigrin and 696.6 mg gluconapin, could produce 2059.6 mg of glucosinolate-rich extract of 53.67% sinigrin and 31.30% gluconapin after separation by D261 resin. Then, 949.40 mg of 97% sinigrin and 568.40 mg of 95% gluconapin could be obtained after the extracts were purified by MPLC, with the recovery of 76.03% of sinigrin and 77.38% of gluconapin. The products were assessed by analytical HPLC and characterized by UV, MS, ¹H NMR, and ¹³C NMR. In conclusion, this method is practical and environmentally friendly, and it is a low-cost process to make full use of Indian mustard seeds.     

流动床离子交换工艺在己二酸催化剂回收中的应用

介绍流动床离子交换装置回收催化剂的生产工艺，从交换装置的选择到运行，分析了流动床的优点、影响因素以及生产中应注意的问题和要求。     

离子交换法制取高纯度黄腐酸的研究

采用强酸性苯乙烯系阳离子交换树脂和大孔苯乙烯系螯合树脂相结合的方法制取高纯度的黄腐酸,探讨了离子类型、交换时间和树脂用量对FA纯度的影响,分析了离子交换机理。结论:粗FA溶液依次通过1个001×7 Na~+型、2个D751 Na~+型、1个001×7 H~+型树脂柱,其中001×7型流速1.5 m L/min左右,D751型流速1.5 m L/min左右,FA纯度达99%以上。