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本文设计制作了一种对烯丙基杯 [4 ]芳烃涂层毛细管。用于毛细管电泳分离的结果表明 ,此管能分离 5 羟色胺 ( 5 HT)、多巴胺 (DA)、去甲肾上腺素 (NE)、肾上腺素 (E)等结构相近的单胺类神经递质 ,而无涂层管则不能。本涂层管在pH4~ 9范围内的电渗较无涂层管下降约 75% ,且当pH <8时 ,电渗随pH的变化接近于线性关系 ,有利于高重现分离。杯芳烃涂层毛细管不降低紫外检测灵敏度。其主要问题是酚羟基对胺类仍有吸附 (或静电 )作用 相似文献
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建立了高效毛细管电泳结合柱上紫外检测测定单胺类神经递质多巴胺(dopamine,DA)和5_羟色胺(5_hydroxytryptamine,5_HT)的毛细管电泳方法 ,优化了缓冲液 pH值、浓度、电压等实验参数 ;结果表明 ,在优化的实验条件下 ,多巴胺、3,4_二羟苄胺 (3,4_dihydroxybenzylamine)和5_羟色胺在10min内得到很好的分离 ,检出限分别为2.02×10 -5mol/L,1.01×10 -5mol/L,1.20×10 -5mol/L ;该法简便、快速 ,样品用量少 ,结果准确 ,重现性好 相似文献
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胶束电动毛细管色谱半导体激光诱导荧光测定单胺类神经递质 总被引:3,自引:0,他引:3
建立了用半导体激光诱导荧光结合胶束电动毛细管色谱测定单胺类神经递质——去甲肾上腺素和多巴胺的高灵敏分析方法。考察了青色素衍生物 ( Cy5 )对去甲肾上腺素和多巴胺的衍生条件。在优化条件下 ,去甲肾上腺素和多巴胺在 3× 1 0 - 8~ 5× 1 0 - 6 mol/L浓度范围内与荧光强度呈良好的线性关系。去甲肾上腺素和多巴胺的检出限分别为 5 .9× 1 0 - 9、 5 .4× 1 0 - 9mol/L。方法简便、灵敏、样品用量少 ,可用于痕量单胺类神经递质分析 相似文献
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建立了单胺类神经递质(5-羟色胺、多巴胺和肾上腺素)、神经递质类代谢产物(高香草酸、5-羟吲哚乙酸和香草扁桃酸)及神经递质类前体(精氨酸和酪氨酸)混合物的毛细管电泳(CE)分离方法. 利用标准试剂混合样考察了缓冲体系的组成、pH值及添加剂对分离的影响,并探讨了尿液中基体成分如肌酸酐、尿酸和乙酰乙酸对分离的干扰. 在Na2B4O7-NaOH缓冲体系(pH=9.90)及紫外(UV)检测(波长200 nm)条件下对8种神经递质类相关物质的分析获得了良好的定量线性关系,检出限(LOD)为0.04~0.60 μmol/L,迁移时间和峰面积的相对标准偏差(RSD,n=5)范围分别为0.09% ~0.48%和0.47% ~3.34%. 利用该方法对实际尿液中的精氨酸和香草扁桃酸进行了定性和定量分析,其定量结果分别为(95.8±3.8)和(44.6±3.5) μmol/L,加标回收率为96.65%~104.5%. 相似文献
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就1993-2005年生物胺类神经递质包括多巴胺、肾上腺素、去甲肾上腺素、5-羟色胺的各种电化学检测方法的应用研究和发展方向进行了评述。引用文献58篇。 相似文献
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径向电场调制毛细管电泳法用于神经递质分离 总被引:5,自引:0,他引:5
利用双向电场控制毛细管电泳系统,考察了神经递质的分离。在pH2.5的0.01mol/L磷酸盐缓冲体系中,通过加入20%(V/V)正丙醇,改善了多巴胺和5-羟色胺的分离效果,但仍不太理想。通过施加径向电场,可进一步提高分离度。本研究不仅拓宽了径向电场调控的样品分离范围,而且为生物活性物质的痕量分析提供了参考依据。 相似文献
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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%. 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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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
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. 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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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. 相似文献
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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. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
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. 相似文献