反相流动注射化学发光法测定单宁

在碱性介质中 ,单宁对高碘酸钾氧化鲁米诺的化学发光反应有较强的增敏作用 ,据此建立了反相流动注射化学发光测定单宁的新方法 ,并研究了最佳反应条件。该方法快速、准确、线性范围宽 ,测定单宁的检出限为 1 .1 2× 1 0 - 9g/ m L,方法的线性范围为 2 .0× 1 0 - 8～ 6 .0× 1 0 - 6 g/ m L,对于 4.0× 1 0 - 6 g/ m L单宁 1 0次测定的相对标准偏差为 0 .79%。应用于中药五倍子、诃子中单宁的测定 ,结果满意     

阻抑动力学光度法测定食品中痕量单宁

基于在硫酸介质中,溴化十六烷基吡啶对于溴酸钾氧化曙红Y褪色反应的增敏作用和单宁对此反应的阻抑作用,建立了阻抑动力学光度法测定痕量单宁的方法.研究了该体系的最佳反应条件和动力学参数.方法的线性范围为0.02～0.35 mg·L-1,检出限为0.01 mg·L-1,方法可直接测定茶叶和啤酒中痕量单宁,相对标准偏差在0.78%～2.36%之间,回收率在99.6%～101.0%之间.对阻抑褪色反应的机理进行了探讨.     

碘氧化法测定中药五倍子中的单宁

碘氧化法测定中药五倍子中的单宁;单宁;五倍子;碘氧化;紫外分光光度法     

催化动力学光度法测定茶叶和中药中的单宁

在盐酸介质中,微量单宁对碘酸钾氧化丙基红的褪色反应有显著的催化作用,据此建立了催化动力学光度法测定微量单宁的新方法。方法的线性范围为0．1～3．0／μg／mL,检出限为0．04／μg／mL。本法简便、快速、灵敏度高和选择性较好,用于茶叶和中药五倍子、诃子中单宁含量的测定,结果满意。     

线性扫描极谱法间接测定中药中的单宁

基于乙酸铜与单宁生成沉淀，铜离子在NH3-NHCl介质中能产生灵敏的极谱波，利用线性扫描极谱法测定剩余铜离子，建立了间接测定中药中单宁的新方法。测定单宁的线性范围为2．0—12．0ug／mL．检出限为1．1ug/mL。该方法应用于中药五倍子、诃子中单宁的测定，测定结果的相对标准偏差小于5％(n=4)，回收率为97．1％-101．5％。     

高灵敏示波电位动力学分析法测定茶单宁

本文利用KBrO3和KBr的氧化还原反应与茶单宁的溴代反应间的速度差异，将动力学分析法与示波电位法结合起来，提出了测定痕量茶单宁的新方法。在0．032mol／LHCl介质中，KBrO3和KBr浓度为0．0005和0．001mol／L时，方法的检出限为3．8μg／L，相对标准偏差为2．8％。调整上述试剂浓度，可使测定范围延伸几个数量级（从ng级到mg级）。该方法灵敏、简便、快速，且不受颜色等干扰。用于饮料、体液和茶树样品中茶单宁的测定，结果与酒石酸铁比色法相差—7．9％～5．5％。     

IO3--I--丁基罗丹明B体系测定面粉中痕量溴酸根

在磷酸介质中,BrO3-氧化I-形成I3-络阴离子,I3-络阴离子可进一步与丁基罗丹明B阳离子形成离子缔合物,在聚乙烯醇存在下,缔合物呈清亮的紫色溶液,以试剂空白为参比,最大吸收波长位于587nm,吸光度A与BrO3-浓度呈线性关系。线性范围0.20～3.50μg/10mL,表观摩尔吸光系数为9.79×104L·mol-1.cm-1,检出限为0.012μg·mL-1,样品回收率94.0%～100.3%,RSD为2.81%。该方法用于面粉中痕量溴酸根测定,结果令人满意。     

单宁协同高碘酸钾氧化亚甲基蓝褪色动力学光度法测定单宁

1 引言。单宁是一类广泛存在的多元酚类化合物,来源于某些植物(如茶、水果等)。单宁具有收敛性,可用于治疗胃肠道出血、溃疡和水泻等症;外用于创伤、灼伤,可减少分泌和防止感染,有局部止血作用;此外单宁还具有抗癌变、抗衰老、消炎、驱虫、降血压等医疗作用,成为近年来酚类物质的研究热点。因此,研究简单、快速,操作简便的单宁测定方法具有重要意义。目前测定单宁的方法有滴定法、蛋白质预沉淀法、高效液相色谱法和化学发光法等;实验观察到在碱性和室温条件下,高碘酸钾氧化亚甲基蓝的反应较慢;而加人少量的单宁后,高碘酸钾与单宁反应,产生单线态活性氧。单线态活性氧极为活泼,高碘酸钾和单线态活性氧共同作用于亚甲基蓝,从而加快了亚甲基蓝的氧化,单宁起了协同氧化的作用。据此建立了测定单宁的协同氧化动力学光度法,应用于巾药五倍子、诃子中单宁的测定,结果满意。     

高灵敏示波电位动力学分析法测定茶单定

本文利用ＫＢｒＯ３和ＫＢｒ的氧化还原反应与茶单宁的溴代反应的速度差异，将动力学分析法与示波电位法结合起来，提出了测定痕量茶单宁的新方法。     

溴代十四烷基吡啶共振散射光谱法测定痕量过氧化氢

基于辣根过氧化物酶催化H2O2氧化过量KI生成I3-,I3-与溴代十四烷基吡啶形成的缔合微粒在478 nm产生共振光散射峰,建立了一种测定痕量H2O2的共振散射光谱法.在选定条件下,478 nm处的共振光散射强度△I478nm与H2O2浓度在2.67×10-8～1.73×10-5 mol/L内呈良好的线性关系,其回归方程为△I478nm=2.54×107c-3.81,检出限为2.67×10-8 mol/L.该方法已用水样的测定,回收率在97.2%～105.2%之间.     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

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.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

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.     

A carbanion induced synthesis of highly congested pyrazole and imidazole containing heterocycles

An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

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.     

正丁胺对激光染料荧光谱影响的研究

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.     

Selective synthesis of 4,5-dihydroimidazo- and imidazo[1,5-a]quinoxalines via modified Pictet–Spengler reaction

An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction.     

Understanding the Diels-Alder reactivity of 1,2-azaborine analogues

The Diels-Alder reactivity of 1,2-heteroborines (H₄C₄B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed.