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1.
毛细管电泳-电化学法对发芽黑米胚芽中γ-氨基丁酸含量的检测 总被引:5,自引:1,他引:4
采用邻苯二甲醛(OPA)为柱前衍生化试剂,用毛细管电泳-电化学检测的方法(CE-ED)测定发芽黑米胚芽中γ-氨基丁酸、缬氮酸和亮氨酸的含量.以直径为300μm的碳圆盘电极为工作电极,50mmol/L硼砂(pH 8.2)为运行缓冲液,对上述3种组分的分离检测条件进行优化研究.在优化条件下,3组分可在15min内完全分离.γ-氨基丁酸、缬氨酸和亮氨酸的线性范围分别为5.0×10-3~0.12、5.0×10-3~0.08和5.0×10-3~0.12g/L,检出限(S/N=3)分别为2.5×10-3、2.5×10-3、2.6×10-3g/L;7次平行进样峰高的相对标准偏差(RSD)分别为2.5%、4.9%、3.9%. 相似文献
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采用电化学沉积法制备了纳米金修饰玻碳电极,并用循环伏安法和电化学阻抗法进行了表征,以此建立了一种直接测定鸟嘌呤的电分析方法。在磷酸盐缓冲溶液(pH 6.0)中,研究了鸟嘌呤在纳米金修饰电极上的电化学行为,实验结果表明,纳米金修饰电极可以增强鸟嘌呤在电极表面的吸附,并加快鸟嘌呤在电极表面的电子传输,使其电化学信号明显增大,检测灵敏度大大提高,该修饰电极对鸟嘌呤表现出良好的电催化性能。在优化实验条件下对鸟嘌呤进行测定,方法的线性范围为8.0×10-7~6.0×10-5mol/L,检出限为1.0×10-8mol/L,在鸟嘌呤浓度为1.0×10-5mol/L时测得RSD(n=10)为2.5%。 相似文献
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运用循环伏安法与线性扫描伏安法研究了阿奇霉素在多壁碳纳米管修饰玻碳电极上的电化学行为,建立了一种直接测定阿奇霉素的电化学分析方法。结果表明,与裸玻碳电极相比,多壁碳纳米管修饰电极能显著提高阿奇霉素的氧化峰电流,阿奇霉素的电极过程完全不可逆,存在典型的吸附特性。在优化的实验条件下,氧化峰电流与阿奇霉素浓度在3.0×10-7~2.5×10-5 mol/L和2.5×10-5~5.0×10-4 mol/L范围内呈现良好的线性关系,检出限为1.0×10-7 mol/L。 相似文献
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以铜圆盘电极为工作电极,利用毛细管电泳-1.5次微分伏安法检测系统,在10 mmol/L混合磷酸盐缓冲溶液中,对3种氨基酸(色氨酸、组氨酸、苏氨酸)的分离检测条件进行了研究,采用小波技术,对含有高频扫描响应信号的复合信号进行分离和重构,获得电泳分离图谱.研究结果表明:在1.67×10-3~2.17×10-6 mol/L范围内可达r≥0.995的良好线性,该方法对苏氨酸、色氨酸和组氨酸的检出限分别可达1.91×10-8、3.05×10-7和2.50×10-7mol/L. 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