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制备了多壁碳纳米管修饰玻碳电极(MWNT/GCE),研究了维生素B2、B6、B12和维生素C共存时在该电极上的电化学行为.实验发现,在HAc-NaAc缓冲溶液中,该电极可同时测定以上四种维生素,线性范围分别为1.0×10-6~1.0×10-4 mol/L、5.0×10-5~2.0×10-3 mol/L、5.0×10-5~7.5×10-4 mol/L和5.0×10-5~2.0×10-3 mol/L,其检出限分别为7.0×10-7 mol/L、1.0×10-5 mol/L、2.5×10-5 mol/L和5.0×10-6 mol/L.样品分析的RSD分别为1.66%、1.71%、2.26%和1.46%.方法简便快捷,可用于四种维生素同时分析测定. 相似文献
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流动注射化学发光法测定3种氟喹诺酮类药物 总被引:1,自引:0,他引:1
研究发现,氟喹诺酮类药物对可溶性Mn(-甲醛化学发光体系有强烈的增敏作用,结合流动注射技术,建立了3种氟喹诺酮类药物诺氟沙星、氧氟沙星和环丙沙星的流动注射化学发光新方法。在优化的实验条件下(2×10-4molMn(-3%甲醛-3mol/L磷酸),本方法测定诺氟沙星、氧氟沙星和环丙沙星的线性范围分别为1.0×10-7~1.0×10-5mol/L,1.0×10-7~1.0×10-5mol/L和3.0×10-7~5.0×10-5mol/L;检出限分别为3×10-8mol/L,3×10-8mol/L,1×10-7mol/L;相对标准偏差(5.0×10-6mol/L氟喹诺酮类药物,n=11)分别为2.6%,1.6%和2.8%。该方法已用于诺氟沙星胶囊中诺氟沙星的含量测定。 相似文献
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对硫磷在纳米氧化铝薄膜修饰电极上的电化学行为及其测定 总被引:2,自引:0,他引:2
制备了纳米氧化铝修饰玻碳电极(nano-Al2O3/GCE/CME),用循环伏安法(CV)、线性扫描伏安法(LSV)研究了对硫磷(TP)在nano-Al2O3/GCE/CME上的电化学行为.实验表明,该修饰电极与裸电极相比能显著提高TP的氧化还原峰电流并降低其氧化峰电位.在0.1 mol/L HAc-NaAc缓冲溶液(pH =5)中,TP在该修饰电极上产生1个不可逆的还原峰( Epc1=-0.567 V)和1对可逆氧化还原峰( Epa2=0.018 V和Epc2=-0.008 V) ,氧化峰电流与TP的浓度在2.5×10-9~1.0×10-7 mol/L和1.0×10-7~1.0×10-5 mol/L范围内具有良好的线性关系,回归方程分别为: ip(μA)=0.2529+4.201C(μmol/L), r=0.9984和ip(μA)=0.6752+0.3181C(μmol/L), r=0.9946.开路富集30 s后,检出限为1.0 ×10-9 mol/L(S/N=3).在1.0×10-5 mol/L TP试液中连续测定10次,其RSD为3.8%.用此方法测定了蔬菜中TP的含量,回收率为95. 6%~100.5% ,结果满意. 相似文献
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基于硼砂溶液中Ru(bpy)32+的弱电化学发光信号可被苯磺酸顺阿曲库铵增敏,建立了测定苯磺酸顺阿曲库铵的电化学发光(ECL)新方法。在最佳条件下,苯磺酸顺阿曲库铵浓度在2.0×10-6~3.2×10-5mol/L范围内与其相对发光强度呈线性关系(r2=0.9999),检出限为4.0×10-8mol/L(S/N=3)。重复测定高、低浓度(2.4×10-5mol/L,3.2×10-6mol/L)的苯磺酸顺阿曲库铵溶液9次,其RSD均为3.2%,方法具有较好的重现性。方法已用于注射用苯磺酸顺阿曲库铵的测定。 相似文献
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研究了Cu-酪氨酸荧光静态猝灭体系,络合物为Cu(Tyr)22 ,猝灭常数K为1.59×1010.以时间驱动模式代替浓度模式,在pH 8.8的硼砂介质中,测得Cu2 的线性范围为4.00×10-7~1.12×10-5 mol/L和8.00×10-6~1.12×10-4 mol/L,相关系数R=0.9996/0.9992,检出限(3σ)为6.6 × 10-8 mol/L,相对标准偏差(RSD)为0.78%(n=11,C(Cu2 )=2.4×10-6 mol/L).本方法可用于实际样品中痕量铜的测定. 相似文献
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在裸金电极上制备了巯基乙酸(mercaptoacetic acid)自组装膜修饰电极(MA/SAMs-Au/CME),并对电极的表面结构进行了电化学表征.结果表明该修饰电极对维生素E(VE)的电化学氧化具有明显的增敏作用. 该文利用VE在MA/SAMs-Au/CME上的氧化和高锰酸钾(KMnO4)在裸金电极上的还原构建了双安培检测体系,成功地建立了在外加电压为0 V条件下流动注射直接测定VE的方法.VE的氧化峰峰电流与其浓度在8.0×10-6 ~8.0×10-5 mol/L范围内呈线性关系(r=0.995 6, n=6),回归方程为I(nA)= 9.87×107c 10,在1×10-4 ~1×10-3 mol/L范围内呈线性关系(r=0.997 0,n=6),回归方程为I(nA)=1.6×107c 104,方法检出限为4.0×10-7 mol/L. 连续20次测定1.00×10-4 mol/L的VE溶液,电流值RSD为2.28%,进样频率为每小时进40个样品.对维生素E片剂中VE含量的测定结果比较满意. 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