连续环状色谱柱分离性能的模拟

连续环状色谱柱是有机物稀溶液及生物制品纯化的重要制备手段,为深入认识连续环状色谱柱的性能,开展了连续环状色谱柱分离性能模拟计算的研究。提出了二维空间网格差分的模拟计算方法,并采用文献报道的木糖-山梨糖分离的实验结果进行验证,模拟计算结果与实验数据基本吻合,证明了模拟计算方法的可行性。同时考察了单组分体系下进料流量、床层旋转速度、相间总传质系数、吸附平衡常数对流出曲线的影响;以木糖为分离关键组分,以木糖的收率和纯度为目标函数,对双组分体系下进料流量、床层旋转速度、床层高度、选择性系数对分离效果的影响进行了计算和讨论,结果表明,选择性系数是决定性因素,适当提高床层旋转速度或床层高度可以增大木糖的纯度。     

影响Porapak Q色谱柱分离能力差的原因及解决方法

通过改变进样系统、载气系统、分离系统、检测系统中的参数来探究Porapak Q色谱柱对乙烯乙烷分离能力差的原因,确认了原色谱填充柱分离效果差的原因在于固定相与柱内径不匹配,采用的1/8in柱内径80/100目粒径固体填料过大,不适合目前的分析。通过使用2m乃至1m柱长、3mm柱内径、80/100目粒径的固体填料的填充柱,可以实现低级烃类组分的有效分离。     

螺旋管连续逆流萃取色谱系统

介绍了一种新型连续分离制备性色谱系统——螺旋管连续逆流萃取色谱,可实现分馏萃取、普通逆流萃取、色谱洗脱等分离过程,而且易实现工业化放大,适用于天然产物、蛋白质和多肽、抗生素、精细化工等附加值高且较难分离物质的连续制备性分离.该系统是在逆流色谱分离原理的基础上开发出来的,主要由萃取部分、进样控制部分和样品收集部分组成.本色谱系统采用特殊的双向流动方式使得各组分能够在长度有限的管程内实现分离,可降低生产成本,缩短操作周期.利用自动控制技术对进样和溶剂的流量进行程序控制,其动作程序可根据分离条件和要求进行设定.     

WCX-HIC二维液相色谱柱对鸡蛋清中活性蛋白的分离纯化

使用一根色谱柱,采用离线单柱二维液相色谱技术对鸡蛋清中的3种蛋白质进行了的分离纯化。第一维采用离子交换色谱模式,可一步分离纯化得到抗生物素蛋白和溶菌酶,其纯度分别达到95.3%和95.6%。将在离子交换模式下不保留的组分再通过疏水色谱模式进行第二维分离,通过条件优化,一步可分离纯化得到球蛋白G2,其纯度可达到98.1%。     

三种混合模式色谱填料色谱性能的比较

以γ-缩水甘油醚氧丙基三甲氧基硅烷为中间活化剂,将3-氨基吡啶、2-巯基苯并咪唑和2-巯基-1-甲基咪唑3种杂环配基键合到粒径为5 μm、孔径为30 nm的球形硅胶上,制备3种高效疏水电荷诱导色谱填料。利用溶菌酶、牛血清白蛋白和免疫球蛋白G作为模型蛋白,考察其在3种不同配基色谱柱上的保留行为和分离行为。比较了3种不同性质的模型蛋白在不同色谱柱上的色谱性能的异同。发现以2-巯基-1-甲基咪唑为配基的色谱柱具有良好的pH控制色谱行为和良好的分离性能,初步验证了高效疏水电荷诱导色谱的分离模式及潜在应用。     

分析检测中液相色谱柱的选择及使用维护

液相色谱法广泛用于食品化工检验、药物研究、生命科学、临床、环境监测等多种领域，其最大的优势是分离混合物中各种组分。承担分离作用的色谱柱是液相色谱系统的核心，决定了分离的效果。本文通过色谱工作者及各大仪器厂商的研究，对分析检测中液相色谱柱的选择及使用维护等相关注意事项进行系统的介绍。     

色谱柱的失效分析及老化

长时期使用后的色谱仪,色谱柱失效是不可避免的,经色谱柱失效原因的分析,探讨分批、分步老化色谱柱,恢复色谱柱正常使用;通过柱效和分离度测算,评价色谱柱老化效果,保证仪器正常运行。     

连续制备色谱的研究进展

本文介绍了近30年来连续制备色谱分离的研究概况，从逆流和错流两个方面分别表述了半连续色谱精制器和连续环状色谱的基本原理，研究进展及应用前景。     

气相色谱-质谱法测定纸巾纸中二异丙基萘

优化检测纸巾纸中二异丙基萘(DIPN)含量的气相色谱-质谱法。样品经丙酮浸泡、样品量:提取溶剂加入量为1∶15、超声时间为45min对样品进行前处理的优化,用气相色谱-质谱进行测定,外标法定量。采用HP-INNOWax (60m×0.25mm×0.25μm)柱进行分离,进样口温度为250℃,氦气流速为1.0mL/min 7种同分异构体二异丙基萘在1～20mg/L浓度范围内呈良好的线性关系,在丙酮溶液中响应值是最高的,丙酮可以作为优化气相色谱-质谱的良好溶剂。此优化后的处理方法的平均回收率在85%左右。该前处理的方法既环保又有很好的稳定性,满足纸巾纸中不同二异丙基萘同分异构体的分析检测和准确定量。     

色谱理论数学模型的计算机模拟实现

根据色谱理论,建立了板高的数学模型,并对模型中的参数进行了初步的确定。通过使用面向对象语言对色谱柱进行编程,模拟绘制了多组分情况下的色谱图。通过色谱图分析,模拟柱温、柱长等参数的变化对色谱的影响与实际分析中色谱图改变是一致的。可以为色谱分析人员确定和优化实际样品的分离分析条件提供有效的参考意见。     

填料粒径对制备色谱生产的影响

随着绿色精细化工工业的发展,对制备色谱和模拟移动床色谱(SMBC)的需求越来越大。填料粒径的选择是制备色谱和模拟移动床色谱分离中的关键问题。填料粒径主要从柱效和压力两方面影响着制备色谱的应用。压力影响着运行成本,柱效影响着分离效果,但两者又互相制约。该文利用板高曲线和压力变化曲线斜率积对填料性能进行了比较。斜率积消除了填料粒径的影响,却又联系着其他与柱压力和柱效相关的因素。利用斜率积来评价填料性能对问题的分析更加深入。该文通过对不同粒径填料所填充柱的孔隙率、柱压和柱效的比较发现,随填料粒径减小,柱压力的上升幅度小于随填料粒径平方反比例增大的幅度,理论塔板高度减小。从银杏黄酮的模拟移动床色谱分离结果可以看出,使用粒径为20~25μm的填料,其产品纯度低于使用粒径为30~40μm的填料。     

Pressurized Continuous Chromatography

Abstract

A pressurized continuous annular chromatograph has been developed for preparative separations. This device utilizes a slowly rotating annular bed of sorbent material, fixed multiple feed points, and fixed withdrawal locations. Most of our investigations have been performed with a 28-cm-diam column, but a larger model is being designed and constructed. The separation of copper, nickel, and cobalt components from a carbonate solution has been studied in detail. This solution simulates the leach liquor from the Caron process for recovering nickel and cobalt from laterite ores. Use of continuous gradient elution has been demonstrated. Recent studies have investigated several separations, including that of zirconium and hafnium (necessary for the production of zirconium for use in nuclear reactors), on a preparative scale. This system, because of its continuous feed and product withdrawal, its adaptability to large-scale operations, and its ability to separate many components, is expected to make chromatography a more competitive process in the industrial sector.     

大型蛋白质色谱柱及凝胶介质的综述

1 INTRODUCTION The history of modern protein purification begins around 1950. Before then the separation and purifica-tion of enzymes and other proteins was primarily per-formed by precipitation and adsorption methods using a variety of inorganic as well as organic materials[1,2]. The first attempts to separate proteins by elution chro-matography were based on the weakly acidic resin cation exchanger Amberlite IRC-50 (a co-polymer of meth-acrylic acid and divinylbenzene)[3,4] and on cal…     

模拟移动床色谱分离药物PG05的实验研究

用实验室自行研制组装的一套 A型三带制备型模拟移动床色谱 (简称 SMBC)系统对手性药物 PG0 5进行了分离。以普通的反相 YWG ODS为固定相 ,甲醇和水的混合液为流动相 ,从含有大量杂质的 PG0 5原料中分离得到了纯度大于 95 %的 S(-) PG0 5产品。对色谱柱的配置、切换时间、进样量、萃取液流速、柱对称性、柱体积等各种影响因素做了实验分析。实验证明 ,用 A型三带SMBC分离 PG 0 5是可行的。同时 ,与传统的批处理层析工艺比较 ,SMBC系统可大大节约溶剂消耗 ,降低成本 ,提高产品的纯度和产量。     

柱径对制备色谱性能影响的分析

制备色谱是得到高纯度药物中间体的极好手段。柱径的选择是制备色谱分离中的关键问题。在制备色谱的应用中,柱效和压力是两个重要的参数。因此,分析柱径对压力和柱效的影响具有重要意义。本文在基本测试的基础上,研究了柱径对柱压力和柱效的影响。结果表明,随柱径增大,柱的孔隙率减小;柱压力并不随柱径的增大,呈平方倍数的增加;柱效随柱径的增大而增大。     

用于制备规模的超临界流体色谱分离对映体受到青睐

综述了超临界流体色谱应用于手性药物的进展。超临界流体色谱正在从单纯地对对映体进行鉴定的分析规模,转向能生产几毫克到几百克物质的半制备或制备规模。快速筛选手性固定相和调节剂是成功应用超临界流体色谱于制备过程的关键。     

Separation and Recovery of Nickel and Molybdenum Using Continuous Rotating Annular Chromatography

ABSTRACT

A continuous rotating annular chromatograph was developed for preparative separation of nickel and molybdenum. Dowex 50W-8X cation resin (hydrogen form) was packed in a 505-mm long and 10-mm wide stationary annular column. The feed solution was continuously introduced at the top of the bed by a rotating feed nozzle and was carried down through the annular column with an eluent of 10% sulfuric acid. The products were collected by a rotational tray rotating at the same speed as the feed nozzle. To evaluate the performance of this device, the effect of feed flow rate and rotational speed of feed nozzle were measured. Experimental results were compared with results calculated using model-plate theory. It was found that the optimum feed flow rate, at a constant eluent flow rate of 48.8 mL/min and a rotational speed of 4.5 degree/min, was 3.5 mL/min.     

Management and control of modifier content in preparative SFC solvent cycles

The objective of this work was to establish a solvent cycle with a possibility for modifier control in a preparative supercritical fluid chromatography simulated moving bed plant (SFC-SMB). Fourier transform infrared (FTIR) spectroscopy and flame ionization detection (FID) have been investigated for measuring alcohol concentrations in supercritical carbon dioxide. The integration of these in-line techniques into a modifier control schema allowed the operation of a closed loop SFC-SMB cycle. The applicability of the developed control concept for usage of 2-propanol in supercritical carbon dioxide has been verified by an experimental test series involving an eight column SFC-SMB plant. Different process variations have been compared in terms of energy and solvent consumption. Hereby, savings of almost all CO₂ and 76% modifier could be achieved.     

Separation of Amino-Acids by Reversed Phase Chromatography: Development of a Model Mixture Dedicated to the Study of Solvent Gradient Chromatography Processes

Solvent gradient is currently used in analytical chromatography and presents an increasing interest in preparative chromatography. The applications relate to complex separations of mixtures where the target species has an intermediate affinity for the solid support compared to that of the other species, which is often the case during the purification of biomolecules extracted from natural raw materials or resulting from biotechnologies. In this case, separation leads to three fractions, impurities weakly retained, an intermediate fraction, and impurities strongly retained. An inexpensive and non-toxic mixture, containing five amino-acids, was identified as a good model mixture for such studies. These amino-acids were selected by taking into account their non-polar and hydrophobic nature. They were selected because of their aptitude for being easily detected in UV-visible spectroscopy without derivation. Separations were carried out by reversed phase chromatography. An experimental study first enabled determining the adsorption isotherm parameters of each amino-acid on an analytical column then on a preparative column for various organic solvent fractions. An empirical law was chosen to express the retention factor k as a function of the mobile phase composition (k=f (x_M)). An approach based on the column modeling by mixed cells in series enabled to simulate the separations obtained on the two types of columns. The use of the laws giving retention factor k as a function of the organic solvent fraction x_M then made it possible to carry out simulations for various solvent gradients. A simple methodology was developed to calculate the optimal solvent gradient. The gradient was optimized by minimizing the separation time and by respecting a constraint on the peaks resolution of the two species which are the most difficult to separate. A really good adequacy was observed between the experimental simulations and results for the weakly retained fraction as well as for the intermediate fraction which comprises components difficult to separate. Adequacy is not as good for strongly retained fraction but it is worth using these two species in the model mixture. This model mixture proves to be interesting to study solvent gradient preparative chromatography processes. The retention of these compounds is sensitive to the organic solvent fraction. It is easy to get these products which are inexpensive, non-toxic, and detectable without any derivation.     

离心分配色谱技术及其在天然产物分离中的应用

作为现代逆流色谱的一种，离心分配色谱(CPC)是一种新型的制备色谱技术。简单介绍了离心分配色谱的设备原理和操作方法，综述了离心分配色谱的研究现状和其应用于天然产物分离方面的相关报道，特别对离心分配色谱反应器和离子交换置换离心分配色谱等一些CPC研究领域出现的新技术进行了介绍；对离心分配色谱的研究前景进行了展望。