液芯波导与光强差技术测定食品中痕量亚硫酸根

采用超高亮绿色发光二极管作光源,使用9 cm液芯波导管和光强差技术分光光度法测定食品中痕量亚硫酸根.分析采用国标GB/T5009.34-2003方法,线性范围的下限及检出限比通常的分光光度法均下降了1000倍.其线性范围为1.6×10-11～1.6×10-9 g/mL,检出限为5×10-12 g/mL,RSD (n=11,1.6×10-10 g/mL)＜1%.     

甲醛-溴酸钾-变色酸2R作用体系的研究与应用

基于甲醛对KBrO3氧化变色酸2R褪色反应的催化效应,建立了新的甲醛测定体系,研究探讨了体系的作用机理。在H2SO4介质中,方法的线性范围为0.020~0.48μg/mL,检出限为5.4×10-9g/mL,方法已用于啤酒中痕量甲醛的测定。     

表面活性剂增敏催化动力学光度法测定痕量钯

基于非离子表面活性剂Tween-20存在下,痕量Pd(Ⅱ)能灵敏地催化K2S2O8氧化靛红的褪色反应,据此建立了测定Pd(Ⅱ)的催化动力学光度新方法。方法的线性范围为8×10-4~1.28×10-2μg/mL,检出限为5.3×10-9g/L,催化反应表观活化能为53.92 kJ/mol。方法已用于矿样中痕量钯的测定。     

催化动力学光度法测定锰

研究了在活化剂氮三乙酸(NTA)存在下,Mn2 催化KIO4氧化刚果红(Gongo Red)褪色反应的条件。建立了催化动力学光度法测定痕量锰的新方法。在测定波长496 nm时,锰测定的线性范围为0~2.8×10-9g/mL,检出限为2.76×10-11g/mL,探讨了有关的反应机理,考察了20余种共存离子对测定的影响,用于大米、绿豆、小米和水样中痕量锰的测定。     

偶合发光法测定熟肉制品中亚硝酸盐的含量

用亚硝酸盐把亚铁氰化钾氧化为铁氰化钾后,与鲁米诺、尿酸组成化学发光体系,建立了一种间接测定痕量亚硝酸盐的方法。探讨了酸度、反应物浓度、干扰离子等因素的影响。该方法的检出限为5.0×10~(11)g/mL,线性范围为1.0×10~(-9)～1.0×10~(-5)g/mL。对熟肉制品样品进行11次平行测定,回收率为92.8％～107.6％,测定结果的相对标准偏差为2.2％～3.9％。     

二甲苯蓝FF褪色光度法测定超痕量铬(Ⅵ)的研究

在H2SO4介质中,超痕量Cr(Ⅵ)能催化H2O2和KIO3协同氧化二甲苯兰FF褪色,从而建立了测定超痕量Cr(Ⅵ)的新方法。该方法检出限为6.40×10-11g/mL,测定范围为0~4.0×10-3μg/mL,用于测定食物中的铬量。     

金橙褪色光度法测定痕量铈(Ⅳ)

基于在硫酸介质中,铈(Ⅳ)催化H2O2氧化金橙使其褪色的反应,建立了测定痕量铈(Ⅳ)的新方法。该法的线性范围为0~250μg/L,检出限为5.8×10-9g/mL。用本法对人发中的铈(Ⅳ)含量进行了测定,分析结果满意。     

偶氮氯膦mk催化动力学光度法测定痕量铱(Ⅳ)

实验发现,在硫酸介质中,Ir(Ⅳ)对KBrO3氧化偶氮氯膦mk的反应具有催化作用,据此建立了测定痕量铱(Ⅳ)的催化光度法。方法测定铱(Ⅳ)的线性范围为0.2~1.2μg/25mL,检出限为6.88×10-10g/mL。拟定的方法已用于冶金产品和岩矿中痕量铱(Ⅳ)的测定,分析结果满意。     

阻抑动力学分光光度法测定食品中痕量碘

研究了在稀硫酸介质中,痕量碘离子对亚硝酸根催化溴酸钾氧化甲酚红的阻抑作用,建立了测定痕量碘离子的阻抑动力学光度分析的新方法。测定碘离子的线性范围为0～0.62μg/mL,检出限为7.43×10-9 g/mL。已用于食品中痕量碘的测定,结果满意。     

KMnO4-甲醛-茚三酮化学发光体系的研究

在甲醛存在下,KMnO4与茚三酮能够发生化学发光反应,产生很强的化学发光.据此采用流动注射技术,建立了一种利用KMnO4-甲醛-茚三酮化学发光体系测定茚三酮的方法.方法的检出限为3×10-8 g/mL;相对标准偏差为1.1%(4.0×10-6g/mL茚三酮,n=11);线性范围为1.0×10-7～2.0×10-4 g/mL.本法已用于样品中茚三酮的测定.     

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.