Nafion修饰玻碳电极测定痕量地尔硫Zhou的研究

本以玻碳电极为基体，制备了Ｎａｆｉｏｎ修饰电极，研究了非电活性阳离子药物地尔硫Ｚｈｏｕ在该电极上的测定原理及方法，将地尔硫Ｚｈｏｕ加入到含电活性阳离子药物多巴胺的电解质溶液中，使多巴峰电流下降，峰电流的降低与地尔硫Ｚｈｏｕ的浓度对数在１．２×１０＾－７－８．０×１０＾－６ｍｏｌ／Ｌ范围内呈良好线性关系。本方法检测下限为６．２×１０＾８ｍｏｌ／Ｌ；回收率范围为９５．８％－１０４．９％；相对标准偏差     

伏安式多酚氧化酶电极的研究

本报道了一种能性能良好的以吩嗪甲酯（ＰＭＳ）修饰的玻碳电极为基体电极的优安式多酚氧化酶电极。采用从蘑菇中粗提取的多酚氧化酶固定於电极表面，可用循环伏安法测定５×１０＾－＾７ｍｏｌ／Ｌ的多巴胺。本首次采用丙烯酸丁酯－丙烯酸甲酯共聚乳液固定酶，所制得电极性能与戊二醛交联法所得电极基本相同。在降低电极充电电流方面，采用半微分技术使电极性能得到很大改善，测定灵敏度达到２．５×１０＾－＾７ｍｏｌ／Ｌ，且     

聚2-吡啶甲酸修饰电极伏安法测定多巴胺

用循环伏安法制备了聚２－吡啶甲酸修饰玻碳电极，研究了神经递质多巴胺（ＤＡ）在该聚合物薄膜修饰电极上的电化学行为。实验结果表明，在ｐＨ７．０的磷酸盐缓冲溶液中，ＤＡ在该电极上的线性范围为１．０×１０－７～１．０×１０－５ｍｏｌ／Ｌ。该修饰电极对抗坏血酸（ＡＡ）无响应，从而可有效消除其对ＤＡ测定的干扰。     

生物大分子肝素修饰电极的制备及其应用——痕量铜的测定

本文利用肝素与某些金属离子之间强烈的亲和作用，设计成了一种新型的伏安传感器，这处用肝素修饰的玻碳电极被用于前量铜的阳极溶出伏安测定。该电极制作简便，具有较好的重现性，选择性和较高的灵敏度，本方法测定铜的线性范围为２．０×１０＾－８ｍｏｌ／Ｌ～１．０×１０＾－６ｍｏｌ／Ｌ，检测下限为１．０×１０＾－９ｍｏｌ／Ｌ，同一支修饰电极平行测定１０次的相对标准偏差是３．２０％。     

硅钼杂多阴离子薄膜修饰电极线性扫描伏安法测定黑液中要溶性硅

本报导了以玻碳电极为基体的１∶１２硅钼杂多阴离子薄膜化学修，铈电极的制备及其电化学特性。并应用于导数伏安法测定。在４．０×１０＾－３ｍｏｌ／Ｌ９ＮＨ４）６Ｍｏ７Ｏ２４－６６．８×１０＾－２ｍｏｌ／ＬＮａ３Ｃｉｔ－０．４８ｍｏｌ／Ｌ ＮＨＯ３体系中，硅浓度在８．３×１０＾－７～１．７×１０＾－３ｍｏｌ／Ｌ。对可溶性硅（以ＳｉＯ２计）为２４５．０５ｍｇ／Ｌ的黑液，稀释１０倍后，取２．００ｍＬ平行测定     

阿霉素在钴离子注入修饰电极上的电化学行为及其应用

阿霉素在０．１ｍｏｌ／Ｌ ＨＡｃ－ＮａＡｃ（ｐＨ４．６２）缓冲溶液中用注入钴的修饰玻碳电极为工作电极进行伏安测定,得到一良好的还原峰;Ｅｐ＝－０．５２２Ｖ（ｖｓ．ＳＣＥ）。峰电流与阿霉素浓度在１．４×１０＾－６－１．４×１０＾－６ｍｏｌ／Ｌ和１．４×１０＾－６－５．６×１０＾－５ｍｏｌ／Ｌ范围内呈线性关系,。     

硅钼杂多阴离子薄膜修饰电极的研究和应用—线性扫描伏安法测定水中可溶性

本研究了以玻碳电极为基体的１：１２硅钼杂多酸根修饰电极的制备及其电化学行为，将１２－ＭＳＡ电极应用于线性扫描伏安法测定天然水中可溶性硅酸盐，结果满意，硅浓度在８．０×１０＾－７－１．７×１０＾－３ｍｏｌ／Ｌ，相对标准偏差（ｎ＝７）为１．８５％，加标回收率为９８．２％－１０３．６％，ＳｉＭｏ１２电极具有优良的选择性和稳定性。     

酮康唑在玻碳电极上的吸附行为及其测定

报道了一种抗真菌治疗新药酮康唑的吸附行为及其测定。该药物在玻碳电极上预富集后，用示差脉冲伏安法测定，其响应电流与药物浓度在２．０×１０＾－１０－１．０×１０＾－－５ｍｏｌ／Ｌ范围内呈线性关系；检屈限为４．０×１０＾－１１ｍｏｌ／Ｌ。可用于尿和血清样品中药物含量的测定。     

2-氨基吡啶修饰电极的电化学性质及对抗坏血酸的测定

研究了２－氨基吡啶聚合膜修饰玻碳电极的制备及其电化学性质,并用于抗坏血酸（ＡＡ）的测定。在ｐＨ５．７ＢＲ缓冲溶液中,ＡＡ在 ２－氨基吡啶修饰电极上产生一灵敏的氧化峰,峰电流与ＡＡ浓度在４ × １０－６～１０－３ｍｏｌ／Ｌ范围内呈良好的线性关系,检测下限为 １．３ × １０－６ｍｏｌ／Ｌ。该电极对 ＡＡ有增敏作用,对多巴胺（ＤＡ）有排斥作用,重现性良好,可用于ＡＡ的测定。     

钴—5,10,20—四（3—甲氧基—4—羟基苯基）卟啉修饰玻碳电极的L—抗坏血…

将水合５，１０，１５，２０－四－（３－甲氧基－４－羟基苯基）钴卟啉修饰在玻碳电极表面，制成ＣｏＴＭＨＰＰ修饰电极，电极稳定性好且灵敏度高，对抗坏血酸有良好的电催化氧化作用，测定线性响应范围为１．０×１０＾－５－１．０×１０＾－２ｍｏｌ／Ｌ，响应时间小于１２ｓ。本研究了电极的性质和应用，并用于药物中抗坏血酸的测定，其测定结果与碘量法一致。     

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.