多维液相色谱分离技术及其在蛋白质组研究中的应用

对近年来多维液相色谱技术及其在蛋白质组学研究中的应用进行了系统综述。详细描述了由不同液相色谱模式构建的多维液相色谱系统,并介绍了其在蛋白质组表达谱、翻译后修饰、定量等方面的应用。此外,还对多维液相色谱的发展趋势和前景进行了展望。     

高效液相色谱表征高聚物*

最常用的测试高聚物的分子量和分子量分布的体积排除色谱(SEC)是高效液相色谱 (HPLC)的一个重要分支,HPLC的另一个重要分支是相互作用液相色谱, 它是20世纪90年代开始用于高分子分离和表征的研究领域。相互作用液相色谱可以根据高分子的化学结构（如共混物组成、共聚物组成、端基）来分离,它比SEC 有更高的分离效率。本文介绍了高聚物液相色谱的分离模式,并就高聚物体积排除色谱、相互作用液相色谱、临界液相色谱和全二维液相色谱用于分离和表征高聚物的研究进展进行了较系统的综述,并对该技术目前存在的问题和今后可能的发展前景进行了探讨。     

《色谱联用技术》（第二版）

该书主要介绍了色谱-质谱、色谱-傅立叶变换红外光谱、色谱-原子光谱和色谱-色谱联用技术。该书简述了质谱、傅立叶变换红外光谱、原子光谱和核磁共振仪器的结构、工作原理、以及与色谱联用时对接口的一般要求。该书内容丰富，包括：液相色谱-质谱、毛细管电泳-质谱、色谱-傅立叶变换红外光谱、液相色谱-傅立叶变换红外光谱、薄层色谱-傅立叶变换红外光谱、色谱-原子光谱等联用技术，以及液相色谱-液相色谱、气相色谱-气相色谱、气相色谱-液相色谱等不同的分离模式色谱联用技术的应用实例。该书是《色谱技术丛书》之分册，在第一版基础上作了修改和充实，补充了新近发展的仪器、技术与应用实例。     

多维液相柱色谱

多维液相柱色谱分离分析复杂样品越来越受到重视。本文介绍了国内外多维液相柱色谱的近期发展,详细讨论了二维液相色谱的实现,其中包括固定相、流动相的选择、温度变量的作用以及两维间切换的实现,并对多维液相柱色谱的应用现状进行了总结。     

中药物质基础的高效液相色谱分离分析方法研究

高效液相色谱方法已成为中药物质基础研究的重要手段．在中药质量控制、中药标准品制备、活性化合物发现等方面发挥着不可替代的作用．然而我们的实验数据表明,一个中药材可能包含上万个化合物．中药物质基础的复杂性对高效液相色谱方法提出了巨大挑战．本文针对液相色谱方法在中药物质基础分离分析中存在的问题与难点,结合红花、黄连、姜黄三味药材样品,从亲水色谱分离模式、新型色谱固定相、二维液相色谱分离系统和液相色谱质谱联用技术等方面讨论了液相色谱的分离分析方法和发展方向．结果表明,高效液相色谱新技术新方法在中药复杂体系的分离分析中具有很大的发展潜力和应用前景．     

中国科学院兰州化物所色谱技术研究开发中心

中国科学院兰州化物所色谱技术研究开发中心是我国唯一从事研制、生产高效气相色谱柱、高效液相色谱柱、液相色谱填料以及相关产品的高科技企业。中心致力于我国色谱柱产业核心技术体系的发展,独创出国际领先的液相沉渍。原位一体化合成制备高效PLOT色谱柱技术:拥有先进的超净-静态制备高效WCOT色谱柱技术:在国内率先完成了球形硅胶色谱填料制备研究开发工作,研制开发出多种液相手性分析填料以及国内急需的专用色谱柱,创造出多项     

中国科学院兰州化物所色谱技术研究开发中心

<正>中国科学院兰州化物所色谱技术研究开发中心是我国唯一从事研制、生产高效气相色谱柱、高效液相色谱柱、液相色谱填料以及相关产品的高科技企业。中心致力于我国色谱柱产业核心技术体系的发展,独创出国际领先的液相沉溃、原位一体化合成制备高效PLOT色谱柱技术;拥有先进的超净-静态制备高效WCOT色谱柱技术;在国内率先完成了球形硅胶色谱填料制备研究开发工作;研制开发出多种液相手性分析填料以及国内急需的专用色谱柱;创造出多项     

特殊结构的新型液相色谱填料的研究进展

<正>在高效液相色谱中,提高分离效率和分析速度是色谱工作者关注的永恒主题[1]。从最初的无定型硅胶发展到多孔硅胶、金属氧化物微球以及聚合物整体柱,针对不同的分析目的,已经研制出大量具有特殊结构的液相色谱填料并被产业化,为液相色谱方法的发展提供了更多的选择。近年来,随着超高效液相色谱、二维液相色谱的发展,人们对可极大提高     

微径高效液相色谱法分离三唑类手性化合物的对映体

 采用微径高效液相色谱技术在手性纤维素色谱柱上分离了一系列 1 1,2 ,4 三唑类手性化合物。比较了微径液相色谱与传统液相色谱的分离结果 ,研究了化合物的苯环上不同取代基及取代基位置对分离的影响 ,并探讨了分离机理。     

高效液相色谱技术在代谢组学研究中的应用

高效液相色谱技术逐渐广泛应用于代谢组学的研究中。迄今为止,该技术已经在不同生理状态的生物体液的代谢指纹谱分析中得到了应用。本文评述了传统高效液相色谱技术、毛细管技术和超高效液相色谱等技术在代谢组学的应用。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.