制备型高效液相色谱技术的研究进展

制备型高效液相色谱是一种快速,有效的分析分离工具.本文介绍了制备型高效液相色谱基础理论及基本装置,介绍了样品的预处理和应用实例,分析了目前制备型高效液相色谱技术存在的问题并对该技术未来的发展进行了展望.     

模拟移动床色谱技术的应用研究进展

模拟移动床色谱技术是一种高效的现代化分离技术。该技术具有分离能力强、设备体积小、投资成本低、环境污染少、便于实现自动控制等优点,特别有利于分离热敏性物质及难分离的物系,近年来,越来越受到工业界和研究者的关注,研究不断深人,应用领域也不断扩大。对模拟移动床色谱技术在石化、食品、制药三大领域的应用研究进展进行了详细的介绍,以期为相关研究提供参考。     

色谱分离技术在淀粉糖工业中的应用

本文论述了色谱分离技术在淀粉糖工业中的应用情况。并对模拟移动床色谱技术在淀粉糖工业中的发展和应用特点,以及作者在这方面的工作进行了介绍。     

高效液相色谱-质谱联用技术在食品安全中的应用及进展

高效液相色谱-质谱联用技术是以高效液相色谱为分离手段,以质谱为鉴定工具的一种分离分析技术.本文介绍了高效液相色谱-质谱联用仪的基本原理和进展,及其在食品安全检测中的应用.     

生 化 分 离 技 术──制备型高效液相色谱

制备型高效液相色谱（ＨＰＬＣ）是在传统的分析型ＨＰＬＣ的基础上发展起来的一种高效分离纯化技术，主要用于制备高纯度生物活性物质。本文介绍了制备型ＨＰＬＣ的装置组成、制备规模及应用实例。     

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。     

模拟移动床技术在中药有效成分分离中的应用

模拟移动床色谱(simulatedmovingbedchromatography)或简称模拟移动床(SMB)是连续色谱的一种,是模拟移动床技术和色谱技术的结合,是以模拟移动床的运转方式来实现色谱的连续分离。该文主要从模拟移动床的发展、结构、原理及其特点、难点和该项技术在中药有效成分分离中的应用等几个方面做一介绍。引用文献20篇。     

高速逆流色谱在手性拆分中的应用

高速逆流色谱是一种新型的、连续高效的液液分配色谱技术.它的固定相和流动相都是液体,没有不可逆吸附,具有样品无损失、无污染、高效、快速和大制备量分离等特点,此项技术已被广泛用于中药成分分离、保健食品、生物化学、生物化工、天然产物化学、有机合成、环境分析等领域.近年来,由于其与传统的分离纯化方法相比有明显的优点,高速逆流色谱技术被逐渐用于手性物质拆分,文章总结了溶剂体系的选择标准,以及目前在高速逆流色谱中进行手性拆分的研究进展.     

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.     

生化分离中模拟移动床色谱模型的驻波设计研究进展

模拟移动床色谱(SMBC)是一种高效的分离手段，而SMBC模型的驻波设计(Standing Wave Design，SWD)针对目前广泛应用的低压分离系统，已经日益受到重视。对该设计的原理，在分离行为的研究及分离操作参数确定等方面的研究进展作了介绍，并报道了该模型设计在当前生化分离与手性拆分中的应用。     

Scale-up purification for rutin hyrdrolysates by high-performance counter-current chromatography coupled with semi-preparative high-performance liquid chromatography

The study made the isolation of three constituents from rutin and exemplified how to achieve quercetin separation and quantification in rapid and scale-up processes by high-performance counter-current chromatography (HPCCC). Meanwhile, we also isolated the other two constituents, kaempferol and isorhamnetin, by semi-preparative high-performance liquid chromatography. After systematic optimization of solvent systems, sample concentration and flow rate on analytical Mini-DE centrifuge, the same conditions were scale-up by 50-fold in preparative Midi-DE centrifuge to purify quercetin, and the maximum sample loading achieved 1.65 g. Eventually, we successfully isolated quercetin, kaempferol and isorhamnetin with the purity of 99.80%, 99.84% and 99.95%, respectively. The process, therefore, provided an efficient method of obtaining sufficient quantities of highly purified quercetin, as well as kaempferol and isorhamnetin.     

Computational algorithm to predict peak profiles in preparative high-performance chromatography

The computational algorithm and the Prep-LEAR program have been performed on the basis of the LEA model of chromatography. This program intends for calculation of peak profiles in non-linear high-performance chromatography and uses unsimplified adsorption isotherm equations. The computational algorithm and program have been tested by applying these to experimental data of thymine adsorption under conditions of reversed-phase high-performance liquid chromatography. The results of numerical calculations for different sample size introduced agree satisfactorily with experimental data and show the characteristic properties of high-performance chromatography. The usefulness of the Prep-LEAR program was confirmed by predicting peak profiles in preparative adsorption Chromatographic processes.     

制备型高效液相色谱分离过程的放大研究（Ｉ）填料尺寸

利用制备型高效液相色谱（ＨＰＬＣ）分离装置,对牛血清白蛋白（ＢＡＳ）和牛血清红蛋白（ＨＧ）进行了制备分离,考察了填料尺寸对柱效和分离度的影响,结果表明,在制备分离过程中,对于难分离物系,可以采用较小直径的色谱填料,以提高分离效率,但在分离度可以满足分离要求的前提下,使用较大直径的色谱填料将更为有利。     

Separation and purification of six isoflavones from Iris tectorum Maxim by macroporous resin-based column chromatography coupled with preparative high-performance liquid chromatography

ABSTRACT

A rapid and robust preparation method of six isoflavones from ethanol aqueous extract of Iris tectorum Maxim (I. tectorum) was established by using macroporous resin column chromatography and preparative high-performance liquid chromatography (Prep-HPLC). After separation by AB-8 resins, total flavonoids content increased from 10.60% in the crude extract to 54.20% with a recovery yield of 75.12%. Subsequently, the extracts were purified by Prep-HPLC, and the purities were more than 82.2% after assessment by analytical HPLC and characterization by mass spectrometry. The established method is expected to be used for preparing available quantities of pure isoflavones from I. tectorum.     

液相色谱技术在煤衍生液体组成与结构测定中的应用

本文综述了液相色谱技术在煤衍生液体分析中的应用及进展。经典的液相柱色谱法仍广泛地用于制备分离；新出现的萃取色谱法分离量大，且吸附剂、洗脱溶剂耗量小；高效液相色谱法无论用于组成分析还是制备分离都极为有效；排阻色谱法做为一种特殊的液相色谱技术可用于分子量分布的测定及按分子量的不同进行的制备分离。     

Characteristics of moving feed-injection chromatography

An alternate method for preparative chromatography, moving feed-injection system was studied with a modified plate model and was compared with the conventional preparative case. Experiments were performed for the separation of diethylether and dichloromethane by a gas-liquid chromatography. The moving feed technique had some advantages over the conventional preparative system; decreased bandwidths, higher peak maxima, and better resolution. The moving feed chromatography can be optimized by variation of the feed port velocities. A plate model was used successfully to predict the experimental concentration profiles. The effects of the particle size were also studied experimentally.     

Separation and identification of triximenynin from Santalum spicatum R. Br.

Seed lipids of Western Australian sandalwood (Santalum spicatum) were separated using preparative thin-layer chromatography. The oil contains about 49% oleic acid and about 40% ximenynic acid. The individual triacylglycerol bands were characterized by high-performance liquid chromatography and gas chromatography. The oil consisted of three major triglycerides: triximenynoyl-glycerol (triximenynin), an oleoyl-diximenynoyl-glycerol, and a dioleoylximenynoyl-glycerol, as demonstrated by gas chromatography with mass selective detection.     

制备型液相色谱分离技术进展

从分离科学的现有水平来看，液相色谱法是目前分离纯化生物大分子的最佳手段。简要介绍了制备液相色说分离技术及其进展。     

CHROMATOGRAPHIC RESOLUTION OF ENANTIOMERS

In the pharmaceutical industry, the increasing demand of new single enantiomer products has raised a great interest towards chromatographic separation methods. While analytical applications of high performance liquid chromatography and gas chromatography are well established, the scaling up to preparative applications still needs a better comprehension and rationalization of the elementary phenomena involved.

In this work the analytical and preparative separation of an isoxazoline racemic mixture on triacetylcellulose has been studied. In order to determine the thermodynamic properties and the equilibrium isotherms of adsorption several experiments at very low concentration (in a HPLC column) and at higher concentrauon (using the frontal analysis technique) have been performed. Moreover, pulse experiments on a preparative column have been run at different temperature and at different racemic concentration. The comparison between experimental data and model results is discussed.     

新型多组分连续制备色谱系统--阵列式柱色谱

本文介绍了一种新型多组分连续制备色谱系统———阵列式柱色谱。该系统是在综合了模拟移动床色谱和旋转环状色谱的工作原理的基础上开发出来的 ,主要由控制部分、流体输送部分、分离部分、检测部分和收集部分所组成。在分离部分中 ,本系统用色谱柱阵列代替了旋转环状色谱的环形填料层 ,即避免了溶质横向扩散和动密封问题 ,又可以根据实际生产需要增减色谱柱数目 ;在收集部分中 ,使用了专门为本系统设计的收集器实现了所有色谱柱流出液的集中收集 ;本系统采用将试验和生产一体化的设计 ,通过将单柱模式下的使用在线检测得出的优化分离条件应用到多柱模式中 ,实现了系统的柔性设计 ,降低了设备成本 ;用户可以通过使用装有系统控制软件的上位机与系统进行实时交互 ,大大提高了系统运行自动化程度 ,简化了操作。具有上述优点的本系统必将有着广泛的应用前景