尿素包合法纯化油脂中花生四烯酸的工艺研究

采用尿素包合法从被孢霉菌体油脂中提取花生四烯酸。试验运用正交设计，考察了包合反应中尿素、溶剂的量等因素对产品中花生四烯酸含量的影响，优化了工艺条件．花生四烯酸的纯度由粗油中的23．21％提高到61．52％。     

花生四烯酸的研究进展

花生四烯酸(AA)是人体必需脂肪酸,具有极高的保健价值。对菌种培育、发酵条件优化进行了分析,综述了该研究领域的国内外发展现状、动态及存在的问题,并对其发展趋势作了展望。     

藻类花生四烯酸的提取工艺

花生四烯酸作为一种重要的保健、营养品,越来越受到人们的重视。从鱼油、真菌丝、微藻中都可以提取花生四烯酸,但这些工艺都有着明显的缺点。设计了一种从藻类提取花生四烯酸的新工艺过程。     

尿素包合法富集分离花生四烯酸的工艺研究

为提高尿素包合法富集花生四烯酸(AA)效率,研究了降温速度、甲醇用量、尿酯比及结晶温度对花生四烯酸(AA)晶体大小、收率及纯度的影响。结果表明,当结晶温度为-7℃,降温速度为10℃/h,m(脂肪酸甲酯)∶m(尿素):v(甲醇)为1 g∶2 g∶20 mL时,AA生成大颗粒晶体。AA的质量分数w(AA)=87.0%,收率为88.7%。杂质主要为亚麻酸(w=9.21%)。产品总不饱和脂肪酸质量分数大于99%。     

大孔树脂法分离纯化阿维菌素工艺研究

研究了大孔树脂分离纯化阿维菌素的工艺。采用HPLC检测方法,从7种大孔树脂中筛选出吸附阿维菌素性能最好的树脂并优化其吸附和洗脱参数。结果表明,采用大孔树脂HZ816吸附阿维菌素的效果最佳,其动态吸附量为62mg·mL^-1,在吸附流速为1．5～2BV·h^-1、90％乙醇作为洗脱剂的优化条件下,解吸收率大于90％、阿维菌素中B1a含量大于91％、总收率大于65％。该阿维菌素分离纯化方法工艺简单。分离效果好,适于工业化生产。     

柿叶总黄酮的大孔树脂分离纯化工艺研究

采用动态的吸附方法,用紫外分光光度法测定柿叶总黄酮的含量,对工艺参数进行评价.该法简单可行,纯化效果好,更接近实际的生产,适用于生产中推广.     

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%。     

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%。     

膨胀污泥床-接触氧化工艺处理花生四烯酸生产废水的工程启动调试

采用膨胀污泥床-生物接触氧化作为前处理工艺处理花生四烯酸生产废水。EGSB反应器进水容积负荷约为6.55kg[COD]/(m3·d),混合液升流速度为6m/h,pH值为6.3~7.3,处理工艺对COD、NH3-N和磷的去除效果较好,EGSB反应器出水COD、NH3-N、色度和磷的去除率分别达到69%、55%、48%和65%,前处理工艺的COD、NH3-N、色度和磷的平均去除率分别为94%、73%、63%和72%,再经过絮凝、气浮和过滤工艺处理之后,出水各项指标均能达到了设计排放标准。运行数据表明温度对EGSB反应器的污染物去除效果影响较大,但对接触氧化池去除COD的影响不大。     

聚酰胺树脂分离纯化箬叶总黄酮的工艺研究

采用单因素和正交实验,优化了聚酰胺树脂分离纯化箬叶总黄酮的工艺条件,并进行了梯度洗脱。结果表明,最佳上样条件为:上样液质量浓度2.60 g/L,上样量20 m L,上样流速1.0 m L/min;最佳洗脱条件为:体积分数为80%的乙醇,洗脱剂用量150 m L,洗脱流速0.5 m L/min,在该条件下平均解吸率为94.54%,其中洗脱剂用量及其浓度为显著因素。梯度洗脱物的显色反应可鉴定出黄酮类、黄酮醇类及异黄酮类。     

无细胞百日咳疫苗纯化新工艺的建立

目的建立适合大规模生产的无细胞百日咳疫苗(Acellular pertussis vaccine,APV)纯化新工艺,使疫苗主要成分的比例稳定可控。方法复苏百日咳菌种并传代培养,在大罐发酵培养收获前,调整菌液的pH值至弱酸性,再通过离心获得上清液,经超滤浓缩和脱盐处理,使用阳离子交换层析进行目的组分的分离纯化,纯化产物经SDS-PAGE分离并经Western blot鉴定,确定最佳纯化条件。用建立的层析纯化新工艺连续纯化3批APV,检测各项指标,验证该工艺的重复性。结果收获前菌液pH值调至5.8～6.0,可使疫苗主要保护抗原在上清液中的含量明显提高;采用强阳离子交换层析的方法,从目的蛋白的捕获到多组分的分离提纯可一步完成,各目的蛋白组分的纯度均可达85%以上,回收率可达90%以上;建立的纯化新工艺具有良好的重复性。结论初步建立了可线性放大、适合APV大规模生产的层析纯化新工艺,为疫苗质量标准的提高奠定了基础。     

Optimization of a tandem ion exchange—extraction chromatographic scheme for the recovery of strontium from raw urine

ABSTRACT

A previously reported ion-exchange/extraction chromatographic scheme for the recovery of radiostrontium from urine for subsequent determination is systematically optimized to minimize reagent consumption, enhance system reusability, and maximize sample throughput. In addition, a preliminary assessment of the effect of mobile phase flow rate on strontium uptake is described. The results show that the tandem system can be re-used without loss of performance, and that the rate at which samples can be processed by the system is ultimately limited by the time required for regeneration of the ion-exchange column and the kinetics of metal ion uptake on the extraction chromatographic sorbent.

Abbreviations: LOV: lab on valve CDC: Center for Disease Control and Prevention EXC: extraction chromatography EDTA: ethylenediaminetetraacetic acid MDL: method detection limit MSA: methanesulfonic acid     

Development of a chromatographic process for largescale purification of staphylococcal enterotoxin B

A process for large-scale purification of staphylococcal enterotoxin B (SEB) is presented. The process consists of three chromatographic steps. The first two steps are based on ion-exchange chromatography and the final one on gel filtration. Diluted culture supernatant (2000 dm³) with a SEB content of 0.4 mg dm^?3 were processed and purified. SEB was obtained in 1.5 dm³ of 0.1 mol dm^?3 ammonium hydrogen carbonate buffer, pH 8.0. The final product produced a single band on SDS polyacrylamide gel electrophoresis and a single peak when subjected to analytical gel filtration. The overall recovery was 74%.     

Preparative scale isocratic chromatographic purification of a polyethylene mono-alcohol accompanied by high resolution evaluation of molecular weight distribution

A simple preparative-scale adsorption chromatographic method for separating a commercially available polyethylene mono-alcohol from its non-functional polyethylene impurities has been established using silica as the stationary phase and toluene at 75°C as the isocratic eluant. Characterization of the chromatographic fractions by ¹H-NMR spectroscopy also provided unexpected comprehensive information on the molecular structure and molar mass distribution of the polyethylene mono-alcohol. © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Harnessing metal ion affinity for the purification of plasmid DNA

The recent surge in plasmid DNA (pDNA) vaccine research has generated demand for an efficient large-scale pDNA purification process. In this study, three process intensification strategies harnessing the interactions of pDNA, RNA and endotoxin with immobilised and/or free transition metal ions were investigated for the purification of plasmid pcDNA3.1D, containing dengue fever antigenic gene (NS3), from the alkaline cell lysate. In the first process scheme, alkaline cell lysate was applied to Cu²⁺-iminodiacetic acid (IDA) for simultaneous removal of RNA and endotoxin. Subsequent addition of CuCl₂ to the supernatant afforded selective precipitation of pDNA, resulting in substantially purified pDNA at an overall recovery yield of 92% with significant reduction in RNA (96%) and endotoxin (>99%). In the second process scheme, pDNA, RNA and endotoxin were first isolated from other impurities in alkaline cell lysate by CuCl₂ precipitation. Addition of EDTA to the precipitated pellets selectively solubilised pDNA and RNA while endotoxin remained insoluble. Subsequent application of solubilised pDNA and RNA to Cu²⁺-IDA resulted in highly purified pDNA with almost complete removal of RNA and any residual endotoxin (∼100% pDNA recovery, ∼100% removal of RNA and endotoxin). In the third process scheme, RNA and endotoxin were first removed from alkaline cell lysate by ZnCl₂ precipitation. pDNA in the supernatant was then recovered by CuCl₂ precipitation (64% pDNA recovery, 86% RNA and >99% endotoxin removal). In essence, the combination of metal ion (CuCl₂) precipitation, followed by immobilised metal affinity chromatography (IMAC) employing Cu²⁺-IDA, provides a great potential to achieve significant intensification of pDNA purification process with improved efficiency and throughput.     

Adsorptive separation of rhenium and rhodium in nitric acid solution using a column packed with an extractant impregnated resin

An adsorptive separation of rhenium and rhodium was performed by using a jacketed glass column packed with an extractant impregnated resin (EIR). The EIR bed showed a successful separation of rhenium and rhodium with about 122 BV of a breakthrough volume. The breakthrough behavior in the column was modeled to assess the mass transfer resistances in the column. The model predicted the column dynamics for rhenium quite well by assuming a homogeneous diffusion in the particle phase. The effective diffusivities of rhenium were in the order of 10⁻⁷ cm²/min. The EIR loaded beds could be eluted with a high purity of more than 99% by using a nitric acid solution.     

Design and optimization of a dividing wall column for debottlenecking of the acetic acid purification process

The dividing wall column (DWC) has gained increasing application in a variety of chemical processes because of its potentiality in energy and capital cost savings in multicomponent separations. The main objective in this work is investigation of its use for removing the bottleneck phenomenon within the column when increasing the throughput of an existing distillation process, particularly, the acetic acid (AA) purification process. Optimal column sequence design, involving both conventional and DWC, is considered. The internal recycle flow distribution around the dividing wall was investigated as a primary optimizing variable. Several column arrangements were analyzed to show that the DWC requires less investment and energy costs than conventional distillation, the Petlyuk column, or the prefractionator arrangement.     

Development of a pre‐purification process for homoharringtonine

A novel pre‐purification method was developed for producing homoharringtonine from Cephalotaxus koreana, giving high purity and yield. The simple, efficient procedure involved biomass extraction, liquid–liquid extraction, and synthetic adsorbent treatment, followed by low‐pressure chromatography. The use of active clay treatment and silica gel low‐pressure chromatography in the pre‐purification process allowed for the rapid, efficient separation of homoharringtonine from interfering compounds and, compared with alternative processes, increased the yield and purity of crude homoharringtonine for subsequent high‐performance liquid chromatography (HPLC) purification. Homoharringtonine of over 52% purity could be obtained simply with high yield from biomass using this pre‐purification method, while minimizing solvent use and the scale and complexity of HPLC operations for homoharringtonine purification. Copyright © 2005 Society of Chemical Industry     

生物制品中残留甲醛含量衍生-气相色谱检测方法的建立及初步应用

目的建立生物制品中残留甲醛含量衍生-气相色谱检测方法,并进行验证及初步应用。方法采用液体进样方式,毛细管色谱柱(SH-Rxi-5MS,30 m×0. 25 mm×0. 25μm)分离,FID检测器检测,外标法定量,测定样品中残留甲醛含量。进样前,对照品及样品使用2,4-二硝基苯肼(2,4-dinitrophenyl-hydrazine,2,4-DNPH)衍生处理,考察不同衍生条件(包括衍生时间、衍生温度和提取溶剂等)对甲醛衍生及提取效率的影响。色谱条件:初始温度为150℃,保持1 min;以20℃/min的速率升温至250℃,保持10 min;检测器温度为250℃,进样口温度为250℃,分流比为10∶1;载气为N2;进样量为1μL。对建立的方法进行重复性、准确性验证及初步应用。结果游离甲醛质量浓度在1～100μg/mL范围内时,浓度与峰面积呈良好的线性关系,回归方程为A=3 789. 7 C-1 030. 2,相关系数为0. 999 8。用建立的方法重复检测甲醛标准液6次,相对标准偏差(relative standard deviation,RSD)为1. 73%;在百白破疫苗样品中加...     

A rapid high-performance liquid chromatographic method for the determination of sinapine and sinapic acid in canola seed and meal

A high-performance liquid chromatographic (HPLC) method has been developed to separate sinapine and sinapic acid from other phenolics in canola seed and meal in a single run. The separation was achieved with a reverse-phase C18 column. Owing to the higher recovery of phenolics and ease of use, refluxing with 100% methanol for 20 min was selected as the extraction method for HPLC analysis and determination of total phenolics using Folin-Ciocalteu reagent. A 10-min isocratic/linear/concave gradient and a 15-min isocratic/linear gradient were selected as the best gradients for the separation of these phenolic compounds. Peak identities for sinapine and sinapic acid were verified with ion exchange separation followed by HPLC analysis. The method was calibrated using sinapine bisulfate and sinapic acid standards; correlation coefficients (R ²) for the calibration curves were 0.997 and 0.999 for sinapine bisulfate and sinapic acid, respectively. The extinction coefficient of sinapine was determined to be 1.16 times that of sinapic acid at the detector wavelength (330 nm). Applying this method to routine canola phenolic analyses can greatly reduce the cost by simplifying the procedures and reducing the time required for each determination.