共查询到20条相似文献,搜索用时 78 毫秒
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用反相高效液相色谱法纯化白细胞介素-2条件初探胡明(沈阳军区军事医学研究所沈阳110031)关键词反相高效液相色谱法,白细胞介素-21前言高效液相色谱法(HPLC)是一项分辨率很高的液相色谱技术,具有速度快,灵敏度高、样品可回收等优点。除被广泛地应用... 相似文献
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高效液相色谱法测定复方芦丁片中芦丁和维生素C的含量 总被引:14,自引:0,他引:14
采用反相高效液相离子对色谱法,以对氨基苯甲酸为内标,测定了复方芦丁片中芦丁和维生素C的含量。色谱柱为μ-BondapakC_(18),流动相为甲醇-水(50:50)配制的樟脑磺酸溶液(0.0025mol/L),检测波长为254nm。并做了线性范围和回收率测定。 相似文献
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高效液相色谱法同时测定食品中脂溶性维生素A,D3,E,K3 总被引:3,自引:0,他引:3
1引言维生素是维持细胞正常生理功能的营养成分之一。许多维生素是酶的辅基或酶的组成成分,因此,测定食品中维生素的含量是食品营养分析的主要内容之一。脂溶性维生素的分析方法一般采用生物法、分光光度法及薄层色谱法等,但这些方法都只能单独测定食品中的维生素,进入80年代后,随着高效液相色谱(HPLC)技术在食品分析中的应用,国外许多研究工作者在利用高效液相色谱技术分析脂溶性维生素的研究上作了许多工作,发展了更具选择性的方法如电化学法、质谱法等,并且对同时测定脂溶性维生素的方法作了一些探索。本文旨在综合国内… 相似文献
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用反相高效液相色谱法分析测定Cd,Hg,Pb和Cu 总被引:5,自引:0,他引:5
用直接进样(C18柱)反相高效液相色谱法研究了Men+-Dz(二硫腙)体系的色谱行为,建立了同时测定Cd,Hg,Pb和Cu的分析方法。方法的线性范围为0.01~2.0mg/L,最低检出质量浓度为2.4~5.0μg/L,相对标准偏差为1.8%~9.7%,回收率为94%~103%(Hg除外)。直接进样反相高效液相色谱法比萃取进样正相液相色谱法更快速,更简便,更容易操作,已用于人发测定。 相似文献
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柱切换高效液相色谱法在生物样品中的应用 总被引:1,自引:0,他引:1
评述了柱切换高效液相色谱法(CSHPLC)在生物样品分析中的应用进展.分别对柱切换装置,血样、尿样提取液中被测组分浓度的测定,在线浓缩样品技术以及CSHPLC的联用进行了介绍. 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献