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1.
功能聚间苯二胺膜用于免疫传感器分析   总被引:1,自引:1,他引:0  
陈瑞川  万桢 《应用化学》1998,15(6):25-28
以电化学聚合法在石墨电极上获得聚间苯二胺膜(PMPD),并建立了快速、灵敏的膜质量检验方法:辣根过氧化物酶(HRP)标记PMPD膜-邻苯二胺(OPD)反应法,对聚合、活化等条件作了研究;进一步制成了检测乙肝表面抗原(HBsAg)和检测鼠免疫蛋白(MIgG)的免疫电极,对血清样品作了检测.结果表明:2.5V电池电压下,于含0.12mol/LMPD的1.2mol/LH2SO4中聚合20min,再以30g/L浓度的戊二醛活化4h,所得HRP标记电极及免疫电极重现性好;检测HB-sAg和MIgG的线性范围分别为0.1~3.2mg/L及0.1~10mg/L  相似文献   

2.
王升富  杜丹  邹其超 《分析化学》2002,30(2):178-182
制备了磷钼杂多酸-L-半胱氨酸自组装超分子膜电极(P2Mo18-L-Cys/Au)。采用水平衰减全反射(ATR-FTIR)光谱表征了膜的组成。研究了该膜电极的电化学性质,发现它在1.0 mol/L H2SO4溶液中,于0.0~0.7V(vs.SCE)间CV扫描出现两对稳定、可逆的氧化还原峰,其中峰电位分别为Em1=0.334 V,Em2=0.188V,对应着P2Mo18O_(62)~(6-)的两步2电子-2质子反应;计时库仑法计算了薄膜内的电子传递系数D为5.01 × 10~(-8)cm2·s~(-1)。该膜电极对酸性溶液中的NO_2~-有明显的电催化还原作用,初步探讨了电催化机理。用差分脉冲伏安法(DPV)测定其还原峰电流与NO_2~-的浓度在2.0 ×10~(-6)~2.0 × 10~(-4)mol/L范围内呈良好的线性关系,相关系数为0.9953,检测限5.0×10~(-7)mol/L。该电极用于模拟水样中NO_2~-的测定,结果满意。  相似文献   

3.
巯基钴卟啉自组装膜的表征及催化性能   总被引:4,自引:0,他引:4  
卢小泉  靳军  朱开梅  张焱  康敬万 《分析化学》2001,29(10):1178-1180
用自制的新型尾式巯基钴(Ⅱ)卟啉在金电极上制成自组装单分子膜,并用XPS,SEM和电化学的方法进行了表征。该膜对抗坏血酸具有良好的催化作用,其氧化过电位较裸金电极上降低了140 mV,响应电流与抗坏血酸(AA)的浓度在 7.8 × 10-5mol/L~1.0×10-2mol/L的范围内具有良好的线性关系,相关系数为 0.9981;检测下限为 1.3 × 10-8mol/L(富集 10min)。  相似文献   

4.
报道了两种9-冠-3衍生物的合成,并以合成的化合物作载体研制了对锂离子响应的PVC膜电极。以乙基-9-冠-3为载体的锂离子电极的能斯特响应为10×10-1~52×10-5mol/L,斜率为(574±03)mV/p[Li](25℃),检测下限为24×10-5mol/L。电极具有良好的稳定性和重现性,用于实际样品测定,结果满意  相似文献   

5.
氯化十六烷基二甲基苄基铵PVC膜糖精离子选择电极的研制   总被引:1,自引:0,他引:1  
本文以氯化十六烷基二甲基苄基铵为活性材料研制成PVC碳棒涂膜式糖精电极。其线性响应范围为5.0×10 ̄-5~1.0×l0 ̄-1mol/L,响应斜率53.2mV/pc。将电极用于饮料中糖精含量测定,回收率在90%~110/范围内。  相似文献   

6.
一种新的适合低pH范围的中性载体PVC膜电极的研究   总被引:2,自引:0,他引:2  
设计并合成了N-十八烷基水杨醛亚胺(ODSAI),N-十八烷基苯甲醛亚胺(ODBAI)两种新的亚胺化合物,并以此为中性载体,制成了PVC膜PH电极。此电极在PH0.6-8.5的范围内,对氢离子呈现很的能斯响应,电极斜率为52mV/pH。  相似文献   

7.
系统地研究了碱性条件下(pH8~10.8)As3+,As5+,MA,DMA和AB等砷化合物在PRP-X100阴离子交换柱上的保留行为。用火焰原子吸收光谱(FAAS)测定从HPLC分离的砷化合物,即通过一根1m×0.23mmi.d.不锈钢毛细管,将HPLC柱出口与FAAS的雾化器连接起来,采用乙炔/空气火焰,在193.7nm处测定。具体研究了两个流动相(20mmol/LNH4HCO3和2.5mmol/L对-羟基苯甲酸-1.0mmol/L苯甲酸水溶液),并系统研究了pH值和缓冲液浓度对上述5个砷化合物的保留时间的影响,发现对于20mmol/LNH4HCO3体系,在pH8.7时,AB,As3+,DMA可以得到完全分离,通过梯度洗提(pH8.7到9.8,流速1.65mL/min),在15min内上述5个砷化合物可以得到良好分离;对于2.5mmol/L对-羟基苯甲酸-1.0mmol/L苯甲酸体系,在pH9.0及流速1.5mL/min时,可以在12min内将上述5个砷化合物分离。  相似文献   

8.
刘焕云  周清泽 《分析化学》1998,26(3):275-278
以碱性染料为活性物质制备20余种不同组分PVC膜Au(CN)2^-电极,确定较佳膜组成为乙基紫0.99%,邻苯二甲酸二丁酯69.2%,PVC粉29.8%。该电极对Au(CN)2^-浓度在5.0×10^-7 ̄1.0×10^-2mol/L范围内接近能斯特响应;斜率为55.7mV(30℃)。稳定性与选择性较好。该电极制备简单,使用方便,已成功用于氰化镀金液中金的测定。  相似文献   

9.
以2-(2-吡啶偶氮)-5-二乙氨基苯酚(PADAP)为柱前衍生试剂,在含0.1%酒石酸的10mmo1/L(pH3.5)HAc-NaAc缓冲溶液的甲醇/水(50∶50,V/V)中(580nm检测),在C18柱上于11min内实现了V、Nb、Ta的同时分离及测定,检出限(S/N=3)为0.34、0.29、7.30ng/mL。该法灵敏度高,用于矿样分析所得结果与推荐值相符,标准加入回收率为99.0%~101.1%。  相似文献   

10.
以2-(2-吡啶偶氮0-5-二乙氨基苯酚(PADAP)为柱前衍生试剂,在含0.1%酒石酸的10mmol/L(pH3.5)HAc-NaAc缓冲溶液的甲醇/水(50∶50,V/V)中(580nm检测),在C18柱上于11min内实现了V、Nb、Ta的同时分离及测定,检出限(S/N=3)杰0.34、0.29、7.30ng/mL.该法灵敏度高,用于矿样分析所得民推荐值相行,标准加入回收率为99.0%~10  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.
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   

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.
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   

19.
20.
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%).  相似文献   

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