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1.
将一种杂环席夫碱N,N′-2 ,6 -二乙酰吡啶缩双苯胺和Nafion修饰在铂电极上 ,然后与钴 (Ⅱ )反应 ,得到Nafion -钴席夫碱膜修饰电极。实验结果表明 ,该修饰电极具有良好的机械、化学和电化学稳定性 ,对生物分子一氧化氮的电化学氧化有显著的催化作用。以1.5次微分线性扫描伏安法测定一氧化氮 ,当浓度在2.8×10-6~8.4×10-8 mol/L范围时 ,氧化电流与浓度有良好的线性关系 ,抗坏血酸、精氨酸及亚硝酸根不干扰测定。  相似文献   

2.
一氧化氮在聚钴-席夫碱修饰电极上的电催化氧化   总被引:5,自引:0,他引:5  
研究了一种新合成的杂环席夫碱N,N’-二乙酰吡啶缩双苯胺在铂电极上的电化学聚合、聚合膜与钴(Ⅱ)的配合反应及聚合物膜的电化学性质。实验结果表明,该席夫碱可在电极表面通过电化学聚合反应形成具有良好的机械、化学和电化学稳定性的聚合物膜,该聚合物膜可与钴离子形成稳定的配合物,这种配合物对和分子一氧化氮的电化学氧化有显著的催化作用。  相似文献   

3.
设计了一种大环钴铬合物-Nafion膜修饰电极并将其应用于神经递质多巴胺的毛细管电泳的测定,结果表明该种修饰电极对多巴胺具有较好的催化效应,在优化的实验条件下,多巴胺在10min内得到检测,检出限(S/N=3)为0.05mg/L;将该法应用于多巴胺注射液的检测,结果令人满意。  相似文献   

4.
本文采用滴涂法制备了还原氧化石墨烯/Nafion溶液修饰玻碳电极(rGO/Nafion/GCE),用电化学聚合法将L-半胱氨酸(L-Cys)聚合在rGO/Nafion/GCE表面,得到Poly-L-Cys/rGO/Nafion/GCE。采用伏安法研究了芦丁在该修饰电极上的电化学行为及其影响因素。结果表明,L-Cys的电聚合圈数对修饰电极的电化学性能具有一定的影响。在最优条件下,芦丁的峰电流与其浓度在2.0×10~(-8)~1.0×10~(-5) mol/L内呈现好的线性关系,检出限(S/N=3)为1.0×10~(-8) mol/L。  相似文献   

5.
合成了一种新型的导电聚合物纳米粒子-多聚亚甲基蓝纳米粒子(PMBNPs),以扫描电镜、紫外光谱及荧光光谱对PMBNPs进行了表征。将PMBNPs固定化在MWVCNTs/Nafion修饰电极表面,制备了PMBNPs/MWCNTs/Nafion修饰电极。通过循环伏安法和电化学阻抗谱对其电化学性质进行了表征,结果表明较之亚甲基蓝溶液和电化学聚合的亚甲基蓝,由多个亚甲基蓝分子组成的纳米粒子制备成的修饰电极具有良好的电活性,可以实现检测信号的放大。据此,将PMBNPs/MWCNTs/Nafion修饰电极用于利血平的电化学检测。  相似文献   

6.
为了提高电化学检测NADH的分析性能,制备了硫堇/Nafion/石墨烯修饰的玻碳电极(GCE),利用Nifion的强离子交换能力将硫堇修饰在电极表面,形成硫堇/Nafion/石墨烯复合电极.与裸玻碳电极相比,在NADH的反应中观察到了电位明显降低和电流响应显著增大.证实了硫堇/Nafion/石墨烯复合电极对NADH有协同的电催化能力.为构造有效地检测NADH的电化学传感器提供一个良好的应用平台.  相似文献   

7.
使用多壁碳纳米管(MWCNTs)和Nafion溶液制备了多壁碳纳米管-Nafion膜修饰的铂电极。运用扫描电子显微镜(SEM)对多壁碳纳米管、Nafion膜、多壁碳纳米管-DMF膜和多壁碳纳米管-Nafion膜进行了形貌表征。通过电化学系统研究了铁氰化钾在多壁碳纳米管-Nafion膜修饰电极、多壁碳纳米管-DMF修饰电极以及未修饰铂电极的表面电化学行为。结果显示,多壁碳纳米管-Nafion膜修饰的电极对铁氰化钾有显著的电化学增强作用,于0.185 V处形成了一个尖锐的还原特征峰,比未修饰的铂电极还原峰增强近8.7倍;在0.231 V处形成了一个较强的氧化特征峰,比未修饰的铂电极氧化峰增强近2.7倍。由于多壁碳纳米管的比表面积大,利用其与Nafion修饰的电极能增强电子传输效率,使测定的峰电流增大,从而提高灵敏度,有助于检测低浓度物质。进一步研究发现,铁氰化钾在未修饰的铂电极表面反应为可逆反应,而在MWCNTsNafion膜修饰后的电极表面反应为不可逆反应。  相似文献   

8.
多巴胺在聚茶碱/Nafion双层修饰玻碳电极上的电化学行为   总被引:14,自引:0,他引:14  
研究聚茶碱/Nafion双层修饰玻碳电极的制备和其电化学性质,并用于测定多巴胺(DA)。在pH7.4的PBS缓冲溶液中,DA在聚茶碱/Nafion双层修饰玻碳电极上产生一灵敏的氧化峰。峰电流与DA浓度在1×10-7~4×10-4mol/L范围内呈良好线性关系,检出限为5×10-8mol/L。该双层膜对DA有增敏作用,对抗坏血酸(AA)有排斥作用,重现性良好,可用于DA的测定。  相似文献   

9.
通过电化学聚合法制备了聚N,N-双水杨醛乙二胺合钴[polyCo(Salen)]修饰超微电极,研究了该修饰电极的电催化性质及其在一氧化氮(NO)测定中的应用.实验结果表明,polyCo(Salen)修饰超微电极对NO的测定有高的灵敏度,NO的浓度在2.0×10-8~2.8×10-6mol/L范围内,电流与浓度呈良好的线性关系,线性相关系数为0.9998,检出限为1.0×10-8mol/L;该电极进一步修饰Nafion后,生物体中常见的物质如抗坏血酸、儿茶酚胺类神经递质的代谢物、NO的氧化产物NO-2等不干扰测定.本传感器可以满足NO在体分析的需要.  相似文献   

10.
本文采用电化学性能独特的联吡啶钌(Ru(bpy)32+)、氮掺杂石墨烯(NG)和Nafion膜构建了一种新型的盐酸异丙嗪电化学传感器。采用红外光谱和扫描电子显微镜对氮掺杂石墨烯的形貌进行了表征。在Nafion膜中添加导电性好、比表面积大的氮掺杂石墨烯可以增加电子传递速度并且可以防止联吡啶钌扩散到Nafion膜的非电活性区域而增加电极使用寿命。在p H 7.0的磷酸盐缓冲溶液中,盐酸异丙嗪在Ru(bpy)32+/NG/Nafion修饰电极上的循环伏安曲线表明,与单一的裸玻碳电极、Ru(bpy)32+/Nafion修饰电极以及NG/Nafion修饰电极相比,该修饰电极使盐酸异丙嗪得氧化峰电流显著增加,而峰电位明显负移,表明采用Ru(bpy)32+/NG/Nafion膜制备的复合修饰电极对盐酸异丙嗪呈现出较强的电化学催化作用。优化实验条件后,发现在1.0×10-6mol·L-1~1.0×10-4mol·L-1.浓度范围内,盐酸异丙嗪的氧化峰电流与其浓度呈良好的线性关系,检测限为3.6×10-7mol·L-1。而且该电极的重现性、稳定性和选择性良好,采用标准加入法可成功用于商业盐酸异丙嗪注射液中盐酸异丙嗪的测定。  相似文献   

11.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

12.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

13.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

14.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

15.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

16.
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.  相似文献   

17.
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.  相似文献   

18.
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.  相似文献   

19.
20.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.  相似文献   

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