催化光度法测定肉制品中亚硝酸盐

基于亚硝酸根在稀磷酸溶液中催化文思蓝－氰钾氧化还原反应,建立了微量ＮＯ＾－２的催化光度法。在最大吸收波长６１０ｎｍ处,ＮＯ＾－２在０－３．０μｇ／２５ｍｌ范围内呈线性关系,检出下限为３．５１＊１０＾－９ｇ．ｍｌ＾－１。方法用于肉制品中ＮＯ＾－２的测定。结果满意,且与国家标准方法结果相符。     

二甲苯蓝FF分光光度法测定微量亚硝酸根

研究了在稀盐酸介质中微量亚硝酸根与二甲苯蓝ＦＦ发生的亚硝化反应，建立了测定微亚硝酸极的新方法，方法的线性范围为０．２×１０＾－６～１５×１０＾－６ｇ／２５ｍｌＮＯ＾－２其Ｓａｎｄｅｌｌ灵敏度为９．１５×１０＾－１０ｇ／ｃｍ＾２，方法已用于水微量亚硝酸根的测定，并对反应机理进行了初步探讨。     

亚硝酸根的催化光度法测定

本法基于甲酸介质中，亚硝酸根对溴酸钾氧化甲基橙褪色的催化效应，用正交法确定最佳测定条件。本法测定亚硝酸根的线性范围为０～０．２０μｇ／ｍＬ灵敏度为２．８３×１０－１０ｇ／ｍＬ。用于测定水样中的亚硝酸根，结果良好。     

溴酸钾氧化中性红催化光度法测定NO-2的研究

研究了盐酸介质中,痕量亚硝酸根催化溴酸钾氧化中性红褪色反应及其动力学条件,建立了催化动力学光度法测定痕量亚硝酸根的新方法,ＮＯ＾－２的测定线性范围为１－７μｇ／２５ｍｌ,检出限为１．５＊１０＾－８ｇ．ｍｌ＾－１。用于化学试剂及唾液中痕量ＮＯ＾－２的测定,结果满意。     

动力学催化光度法测定痕量亚硝酸根

磷酸和棉红在１００℃下反应生成天蓝色物质（λｍａｘ＝６７５ｎｍ）,该物质在痕量亚硝酸根的催化下被ＫＢｒＯ３氧化褪色,研究了反应的条件,测定了动力学参数,建立了测定痕量亚硝酸根的方法,方法检出限是４＊１０＾－１０ｇ／ｍＬ,测定范围是０．４０－２０．００μｇ／Ｌ,用于水体中痕量亚硝酸根的测定,结果满意。     

荧光动力学光度法同时测定硝酸根及亚硝酸根的研究

基于亚硝根对溴酸钾氧化罗丹明６Ｇ的催化及锌粉使硝酸根还原为亚硝酸根的原理，建立了同时测定亚硝酸根和硝酸根的荧光动力学法，用于饮用水、质控水样、饮料中硝酸根及亚硝酸根的测定，测定下限分别为０．０７４ｎｇＮＯ２＾－／ｍｌ和０．２５ｎｇＮＯ３＾－／ｍｌ。     

溴酸钾氧化吡罗红G催化动力学光度法测定痕量NO2^—

研究了在磷酸介质中亚硝酸根催化溴酸钾氧化吡罗红Ｇ而使褪色，建立了催化动力学光度法测定痕量亚硝酸根的新方法，测定范围为０．２－２０μｇ／ｍＬ，检出限为０．２ｎｇ／ｍｌ，用于食品和水样中的亚硝酸根测定获得满意结果。     

基于亚硝化反应吖啶红极谱法测定亚硝酸根

研究了在稀盐酸介质中吖啶红与亚硝酸根发生亚硝化反应,建立了极谱法测定亚硝酸根的新方法。反应产物的２．５次微分波的峰谷电位为－０．４９Ｖ,亚硝酸根浓度在０．０２－０．６μｇ．ｍｌ＾－１范围内与峰高呈线性关系,检出限为６．２＊１０＾－３μｇ．ｍｌ＾－１。相对标准偏差为１．８４％,用于测定环境水样中亚硝酸根,结果满意。     

催化光度法测定痕量亚硝酸根的研究：溴酸钾—维多利亚蓝B …

基于在稀磷酸介质中，亚硝酸根在溴酸钾氧化维多利亚蓝Ｂ反应具有催化作用，建立了测定痕量亚硝酸根的新催化光度法，方法的检出限为２．５×１０＾－９ｇ．ｍｌ＾－１，线性范围为７．４～１４８ｎｇ．ｍｌ＾－１，回收率为９６％～１０３％，用于地面水及地下水的测定，结果满意。     

亚硝酸根—对氨基苯磺酸—H酸偶联反应体系光度法测定亚硝酸根的研究

本根据亚硝酸根与对氨基苯磺酸、Ｈ酸在酸性介质中进行的重氮偶联反应，提出了一个测定痕量亚硝酸根的分光光度新体系。最大吸收波长为５２０ｎｍ摩尔吸光系数为３．１× １０＾４Ｌ／ｍｏｌ．ｃｍ亚硝酸根浓度在０－１．２μｇ／ｍＬ范围内符合比耳定律。用于水样中亚硝酸根的分析，测定结果与经典的α－萘胺法一致。     

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.     

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.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

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 Cu^I 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).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(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.