碳糊电极阳极吸附伏安法测定氧氟沙星

碳糊电极阳极吸附伏安法测定氧氟沙星;氧氟沙星; 阳极吸附伏安法; 碳糊电极     

甲巯咪唑基于血红素修饰碳糊电极的电化学测定

制备了一种血红素修饰碳糊电极,用循环伏安法研究了甲巯咪唑在该修饰碳糊电极上的电化学响应特征,并对各实验参数进行了优化.相对于裸碳糊电极,甲巯咪唑在血红素修饰碳糊电极上的氧化峰电位明显负移,氧化峰电流大大提高,说明血红素对甲巯咪唑的氧化具有一定的促进作用.微分脉冲伏安实验结果表明,甲巯咪唑的氧化峰电流与其浓度在4×10-7 ～2×10-4 mol/L范围内呈良好的线性关系,检出限(S/N=3)为2×10-7 mol/L.该修饰碳糊电极显示了较好的抗干扰能力,尿酸几乎不干扰测定.用于实际尿样中甲巯咪唑的加标回收测定,结果满意.     

掺杂硒修饰碳糊电极伏安法测定对乙酰氨基酚

采用循环伏安法制备了掺杂硒修饰碳糊电极,用循环伏安法和差分脉冲伏安法研究了对乙酰氨基酚在掺杂硒修饰碳糊电极上的电化学行为,建立了掺杂硒修饰碳糊电极测定对乙酰氨基酚的电化学方法。在pH 4.6的0.1mol·L-1乙酸-乙酸钠缓冲溶液中,对乙酰氨基酚在+0.61V呈现一个灵敏的氧化峰。对乙酰氨基酚的浓度在6.0×10-7~1.5×10-4 mol·L-1范围内与其氧化峰电流呈线性关系,检出限(3s/k)为2.8×10-7 mol·L-1。方法用于药品中对乙酰氨基酚的测定,测定结果与药典法测定值相符,测定值的相对标准偏差(n=5)在2.1%~2.5%之间。     

米吐尔在离子液体修饰碳糊电极上的电化学行为及其测定

用离子液体1-庚基-3-甲基咪唑六氟磷酸([HMIM][PF6])作修饰剂制备了离子液体修饰碳糊电极(IL/CPE).在0.5 mol/L HAc-NaAc(pH=4.8)缓冲溶液中,采用循环伏安法(CV)和方波伏安法(SWV)研究了米吐尔在该修饰电极上的电化学行为,建立了测定米吐尔的新方法.研究表明,米吐尔在IL/CPE上的氧化、还原峰电位差比其在裸碳糊电极(CPE)上的小,而峰电流却显著增加,说明IL/CPE对米吐尔有电催化作用;共存物对苯二酚干扰米吐尔的测定,通过方波伏安法可以消除其干扰.在方波伏安曲线上,米吐尔的还原峰电流与其浓度在1.0×10-7 ～2.0×10-5 mol/L范围内呈线性关系,检出限为3.0×10-8 mol/L.该法可用于照相废液中米吐尔的测定.     

利眠宁在混合粘合剂碳糊电极上的伏安特性研究

制备了混合粘合剂碳糊电极并研究了利眠宁在该电极上的伏安特性，在０．０１０ｍｏｌ／ＬＨＣｌ溶液中，当有０．０１０％ＳＬＳ存在时，利眠宁在－０．８０Ｖ左右产生一灵敏的阴极溶出伏安峰。制备了混合     

金在碳糊电极上的静电吸附及溶出伏安测定

阳极溶出伏安法测定金具有灵敏度高,操作简便等优点,但共存金属往往干扰测定,影响该方法的应用。为减少干扰,已有阴极溶出伏安法的报道。 作者曾采用修饰了三烷基叔胺的碳糊电极,通过开路萃取富集和介质交换,测定矿样中的金,并且发现,碳糊电极本身能在正电位下直接富集微量金,在阴极溶出伏安法中显示了     

多壁碳纳米管修饰碳糊电极测定爽肤水中甲硝唑

研究甲硝唑在多壁碳纳米管修饰碳糊电极上的电化学行为,建立多壁碳纳米管修饰碳糊电极测定爽肤水中甲硝唑的方法。在pH 1.84的BR缓冲溶液中,以经过1 mg/mL多壁碳纳米管修饰的碳糊电极为工作电极,采用循环伏安法扫描试样溶液,记录扫描图谱的峰电位和峰电流。甲硝唑于–0.4 V处有明显的还原峰,其峰电流与甲硝唑的浓度在10～500μmol/L范围内具有良好的线性关系,相关系数为0.999 2,检出限为0.132μmol/L。实际样品加标回收率为98.8%～102.4%,测定结果的相对标准偏差为1.3%～2.3%(n=5)。甲硝唑在多壁碳纳米管修饰碳糊电极上有良好的响应,电极选择性好、灵敏度高;该方法简便、经济,可应用于化妆品、药品中甲硝唑的测定。     

蒙脱石修饰碳糊电极测定苯酚的研究

本文报道蒙脱石修饰碳糊电极在醋酸盐缓冲溶液(pH=3.6)中,用微分脉冲伏安法测定苯酚。在+0.90 V(vs.Ag/AgCl)有一灵敏的氧化峰,伏安响应要比碳糊电极高得多.对测定苯酚的条件进行了研究,苯酚在0.1～1.0μg/ml范围内呈线性,检出限为40ng/ml,相对标准偏差为6.7％,平均回收率为97.2％。用此方法,不经分离直接测定饮料中的酚。还对苯酚在蒙脱石修饰碳糊电极上的反应机理进行了探讨。     

离子液体修饰碳糊电极对黄芩苷的电催化作用及其分析应用

伏安法;电催化;离子液体;碳糊电极;黄芩苷     

3,6-二氧杂-1,8-辛二硫醇-汞(Ⅱ)配合物修饰碳糊电极的制备及循环伏安行为研究

利用3，6-二氧杂-1，8-辛二硫醇（H2L）和HgCl2反应，得到组成为Hg3L2Cl2的配合物。制备了Hg3L2Cl2修饰的碳糊电极，研究了在1mol／L KCl水溶液中的循环伏安行为。研究结果表明在1mol／L KCl介质中，在0．3～-0．8V（vs．SCE）范围内出现Hg3L2Cl2的还原和L^2-在汞膜表面的吸附，在一0．30—0．30V范围内出现汞膜的氧化还原反应。     

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.