Applications Of Qcm, Eis And Spr In The Investigation Of Surfaces And Interfaces For The Development Of (bio)sensors [aplicações De Qcm, Eis E Spr Na Investigação De Superfícies E Interfaces Para O Desenvolvimento De (bio)sensores]

The use of the quartz crystal microbalance process, electrochemical impedance spectroscopy and surface plasmon resonance for characterizing thin films and monitoring interfaces is presented. The theorical aspects of QCM, EIS and SPR are introduced and the main application areas are outlined. Future prospects of the combined applications of QCM, EIS and SPR methods in the studies of interfacial processes at surfaces are also discussed.276970979Valcárcel, M., Rios, A., (1999) Anal. Chim. Acta, 400, p. 425Zhang, S., Wright, G., Yang, Y., (2000) Biosens. Bioelectron., 15, p. 273Thévenot, D.R., Toth, K., Durst, R.A., Wilson, G.S., (2001) Biosens. Bioelectron., 16, p. 121Fraser, D., (1997) Biosensors in the Body: Continuous in Vivo Monitoring, , Wiley: New YorkJacobson, G.A., Winkeler, M., (2000) Mater. 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Development Of A Sensor Based On Tetracyanoethylenide (litcne)/poly-l- Lysine (pll) For Dopamine Determination

The catalytic oxidation of dopamine (DA) at a LiTCNE (lithium tetracyanoethylenide) film modified electrode is studied by electrochemical approaches. The immobilization of LiTCNE was performed by a polymer (poly-l-lysine) to prepare this modified electrode and its application for dopamine (DA) determination is described in detail. The modified electrode showed a high activity for the electrooxidation of dopamine (DA) at E p = 0.20 V versus SCE. The modified electrode presented a wide linear response range for DA from 0.01 up to 10 μmol l-1 by differential pulse voltammetry (DPV) with a detection limit of 0.5 nmol l-1. The repeatability of the proposed sensor evaluated in term of relative standard deviation was 3.2% for n = 10. The sensor was applied for the determination of dopamine in pharmaceutical formulations and the average recovery for these samples was 101.9 (±0.1)%. © 2004 Elsevier Ltd. All rights reserved.501326752683Cooper, J.R., Bloom, F.E., Roth, R.H., (1982) The Biochemical Basis of Neuropharmacology, , Oxford University Press Oxford, UKDamier, P., Hirsch, E.C., Agid, Y., Graybiel, A.M., (1999) Brain, 122, p. 1437Michael, D.J., Wightman, R.M., (1999) J. Pharm. Biomed. Anal., 19, p. 33Wighman, R.M., May, L.J., Michael, A.C., (1988) Anal. Chem., 60, pp. 769ALane, R.F., Blaha, C.D., (1990) Langmuir, 6, p. 56Janata, J., (1992) Anal. Chem., 64, pp. 196RYe, J., Baldwin, R.P., (1988) Anal. Chem., 60, p. 1979Murray, R.W., (1984) Electroanalytical Chemistry, p. 191. , A.J. Bard Marcel Dekker New YorkRedepenning, J.G., (1987) Trends Anal. Chem., 6, p. 18Damos, F.S., Sotomayor, M.D.T., Kubota, L.T., Tanaka, S.M.C.N., Tanaka, A.A., (2003) Analyst, 128, p. 255Marzal, P.C., Chumbimuni-Torres, K.Y., Hoehr, N.F., Neto, G.O., Kubota, L.T., (2004) Sens. Actuators, 100, p. 333Miura, T., Masaki, Y., (1994) Tetrahedron Lett., 35, p. 7961Miura, T., Masaki, Y., (1994) J. Chem. Soc., Perkin Trans., 1, p. 1659Luz, R.C.S., Damos, F.S., Oliveira, A.B., Beck, J., Kubota, L.T., (2004) Talanta, 64, p. 935Khoo, S.B., Foley, J.K., Pons, S., (1986) J. Electroanal. Chem., 215, p. 273Sttephan, S., Maenz, K., Stadermann, D., (1992) Liebigs Ann. Chem., p. 1033Pereira, A.C., Santos, A.S., Kubota, L.T., (2002) Quim. Nova, 25, p. 1012Oyama, N., Anson, F.C., (1979) J. Am. Chem. Soc., 101, p. 3450Oyama, N., Anson, F.C., (1980) Anal. Chem., 52, p. 1192Shigehara, K., Oyama, N., Anson, F.C., (1981) Inorg. Chem., 20, p. 518Aleman, C., Zanuy, D., Casanovas, J., (2003) J. Phys. Chem., 107, p. 4151Muthukuma, M., (2004) J. Chem. Phys., 120, p. 9343Moreira, J.C., Zhao, R., Fogg, A.G., (1990) Analyst, 115, p. 1565Anson, F.C., Ohsaka, T., Saveant, J.M., (1983) J. Phys. Chem., 87, p. 640Webster, O.W., Mahler, W., Benson, R.E., (1962) J. Am. Chem. Soc., 84, p. 3678Zhu, Z., Na-Qiang, L., (1998) Electroanalysis, 10, p. 643Hall, E.A.H., Skinner, N.G., Jung, C., Szunerits, S., (1995) Electroanalysis, 7, p. 830Bard, A.J., Faulkner, L.R., (1980) Electrochemical Methods, Fundamentals and Applications, , Wiley New YorkRen, X., Puckup, P.J., (1997) J. Electroanal. Chem., 420, p. 251Raj, C.R., Takeyoshi, T., Ohsaka, T., (2003) J. Electroanal. Chem., 543, p. 127Andriex, C.P., Dumas-Bouchiat, J.M., Savéant, J.M., (1982) J. Electroanal. Chem., 131, p. 1Laviron, E., (1981) J. Electroanal. Chem., 124, p. 1Richard, J.A., Whitson, P.E., Evans, D.H., (1975) J. Electroanal. Chem., 63, p. 3111Papouchado, L., Sandford, R.W., Petrie, G., Adams, R.N., (1975) J. Electroanal. Chem., 65, p. 275Wang, Q., Dong, D., Li, N., (2001) Bioelectrochemistry, 54, p. 169Ferreira, M., Dinelli, L.R., Wohnrath, K., Batista, A.A., Oliveira Jr., O.N., (2004) Thin Solid Films, 446, p. 301(1987) Analyst, 112, p. 199. , Analytical Methods CommiteeZhou, D.M., Ju, H.X., Chen, H.Y., (1996) J. Electroanal. Chem., 408, p. 219Carvalho, R.M., Oliveira, O.N., Kubota, L.T., (2000) Anal. Chim. Acta, 420, p. 109Carvalho, R.M., Kubota, L.T., Rath, S., (2003) J. Electroanal. Chem., 548, p. 19Winter, E., Carvalho, R.M., Kubota, L.T., Rath, S., (2000) J. Braz. Chem. Soc., 14, p. 564Copra, A., (2001), M.Sc. Thesis, University of Sarajevo, Sarajev

Adsorption Kinetic And Properties Of Self-assembled Monolayer Based On Mono(6-deoxy-6-mercapto)-β-cyclodextrin Molecules

The kinetic of the assembly and adsorption processes of mono(6-deoxy-6-mercapto)-β-cyclodextrin (βCDSH) on gold surfaces in situ and in real time have been investigated by surface plasmon resonance technique (SPR). The film thickness, dielectric constant and its coverage capability were determined by SPR with one-wavelength approach. To unambiguously determine the film parameters avoiding multi-layer adsorption as well as an underestimation of the binding constants of the adsorption process, the influence of the mass transport of βCDSH was investigated and controlled. Under flow regime the SPR angle was monitored in several concentrations of thiol and the data were fitted by using a two-step adsorption model based on a fast adsorption of the thiol molecules in a first step followed by its slow rearrangement on the gold surface. Finally, the selectivity of the host-guest property of the βCDSH monolayer was investigated using [Fe(CN)6]3-/4- and ferrocenemonocarboxylic acid as redox probes. © 2006 Elsevier B.V. All rights reserved.60101/02/15181193Atwoods, J.L., Lehn, J.-M., (1996) Comprehensive Supramolecular Chemistry, 3, pp. 1-78. , Szejtli J., and Osa T. (Eds), Pergamon, Oxford, UKKhan, A.R., Forgo, P., Stine, K.J., D'Souza, V.T., (1998) Chem. Rev., 98, pp. 1977-1996Cszejtli, J., (1998) Chem. Rev., 98, pp. 1743-1754Martin Del Valle, E.M., (2004) Process Biochem., 39, pp. 1033-1046Singh, M., Sharma, R., Banerjee, U.C., (2002) Biotechnol. Adv., 20, pp. 341-359D'Souza, V.T., Lipkowitz, K.B., (1998) Chem. Rev., 98, pp. 1741-1742Pospisil, L., Svestka, M.J., (1994) J. Electroanal. Chem., 366, pp. 295-302Rojas, M.T., Koniger, R., Stoddart, J.F., Kaifer, A.E., (1995) J. Am. Chem. Soc., 117, pp. 336-343Ferancova, A., Labuda, J., Kutner, W., (2001) Electroanalysis, 13, pp. 1417-1423Parker, D., Kataky, R., (1997) Chem. Commun., 21, pp. 141-145Ferancova, A., Korgova, E., Miko, R., Labuda, J., (2000) J. Electroanal. Chem., 492, pp. 74-77Busse, S., DePaoli, M., Wenz, G., Mittler, S., (2001) Sensors Actuat. B, 80, pp. 116-124Wang, Y., Kaifer, A.E., (1998) J. Phys. Chem. B, 102, pp. 9922-9927Karpovich, D.S., Blanchardt, G.J., (1994) Langmuir, 10, pp. 3315-3322Subramaniam, R., Lakshminarayanan, V., (2000) Electrochim. Acta, 45, pp. 4501-4509Peterlinz, K.A., Georgiadis, R., (1996) Langmuir, 12, pp. 4731-4740Henke, C., Stenem, C., Janshoff, A., Steffen, G., Luftmann, H., Sieber, M., Galla, H.-J., (1996) Anal. Chem., 68, pp. 3158-3165Fujita, K., Ueda, T., Imoto, T., Tabushi, I., Toh, N., Koga, T., (1982) Bioorg. Chem., 11, pp. 72-84Kretschmann, E., (1971) Z. Phys., 241, pp. 313-324Damos, F.S., Luz, R.C.S., Kubota, L.T., (2005) Langmuir, 21, p. 602Caide, X., Sui, S.-F., (2000) Sensors Actuat. B, 66, pp. 174-177Peterlinz, K.A., Georgiadis, R., (1996) Opt. Commun., 130, pp. 260-266Bruijn, H.E., Kooyman, R.P.H., Greve, J., (1990) Appl. Opt., 29, pp. 1974-1978Bruijn, H.E., Altenburg, B.S.F., Kooyman, R.P.H., Greve, J., (1991) Opt. Commun., 82, pp. 425-432Love, J.C., Estroff, L.A., Kriebel, J.K., Nuzzo, R.G., Whitesides, G.M., (2005) Chem. Rev., 105, pp. 1103-1169DeBonno, R.F., Loucks, G.D., Manna, D.D., Krull, U., (1995) Can. J. Chem., 74, pp. 677-688Azzam, R.M.A., Bashara, N.M., (1977) Ellipsometry and Polarized Light, , Elsevier Science, Amsterdam, The Netherlands p. 359Hu, K., Bard, A.J., (1998) Langmuir, 14, pp. 4790-4794Morton, T.A., Myska, D.G., Charken, I.M., (1995) Anal. Biochem., 227, pp. 176-185Camillone III, N., (2004) Langmuir, 201, pp. 1199-1206Kim, Y.T., McCarley, R.L., Bard, A.J., (1993) Langmuir, 9, pp. 1941-1944Glaser, R.W., (1993) Anal. Biochem., 213, pp. 152-161Adamson, A.W., (1982) Physical Chemistry of Surfaces, , John Wiley & Sons, New YorkUlman, A., (1991) An Introduction to Ultrathin Organic Films, , Academic Press Inc., New YorkDijksma, M., Boukamp, B.A., Kamp, B., van Bennekom, W.P., (2002) Langmuir, 18, pp. 3105-3112Nelles, G., Weisser, M., Back, R., Wohlfart, P., Wenz, G., Mittler-Neher, S., (1996) J. Am. Chem. Soc., 118, pp. 5039-5046Sabatini, E., Rubinstein, J., (1987) J. Phys. Chem., 91, pp. 6663-6669Finklea, H.O., Snider, D.A., Fedyk, J., (1993) Langmuir, 9, pp. 3660-3667Choi, S.-W., Jang, J.-H., Kang, Y.-G., Lee, C.-J., Kim, J.-H., (2005) Colloids Surf. A: Phys. Eng. Aspects, 257, pp. 31-36Rekharsky, N.V., Inoue, Y., (1998) Chem. Rev., 98, pp. 1875-1917Bard, A., Falkner, L.R., (1980) Electrochemical Methods: Fundamentals and Applications, , John Wiley & Sons, New Yor

Development Of A Sensor For L-dopa Based On Co(dmg) 2clpy/multi-walled Carbon Nanotubes Composite Immobilized On Basal Plane Pyrolytic Graphite Electrode

L-Dopa is the immediate precursor of the neurotransmitter dopamine, being the most widely prescribed drug in the treatment of Parkinson's disease. A sensitive and selective method is presented for the voltammetric determination of L-Dopa in pharmaceutical formulations using a basal plane pyrolytic graphite (BPPG) electrode modified with chloro(pyridine)bis(dimethylglyoximato)cobalt(III) (Co(DMG) 2ClPy) absorbed in a multi-walled carbon nanotube (MWCNT). Scanning Electron Microscopy and Fourier Transform Infrared Spectroscopy were used to characterize the materials. The electrocatalytical oxidation of L-Dopa using the Co(DMG) 2ClPy/MWCNT/BPPG electrode was investigated by cyclic voltammetry and square wave voltammetry. The parameters that influence the electrode response (the amount of Co(DMG) 2ClPy and of MWCNT, buffer solution, buffer concentration, buffer pH, frequency and potential pulse amplitude) were investigated. Voltammetric peak currents showed a linear response for L-Dopa concentration in the range of 3 to 100μM, with a sensitivity of 4.43μAcm -2/μM and a detection limit of 0.86μM. The related standard deviation for 10 determinations of 50μML-Dopa was 1.6%. The results obtained for L-Dopa determination in pharmaceutical formulations (tablets) were in agreement with the compared official method. The sensor was successfully applied for L-Dopa selective determination in pharmaceutical formulations. © 2012 Elsevier B.V.862229Fauci, A.S., Braunwald, E., Kasper, D.L., Hauser, S.L., Longo, D.L., Jameson, J.L., Loscalzo, J., (2008) Harrison's Principles of Internal Medicine, , McGraw-Hill Professional, New YorkTrevor, A.J., Katzung, B.G., Masters, S.B., (2010) Katzung & Trevor's Pharmacology, Examination and Board Review, , McGraw-Hill Medical, New YorkGrünhut, M., Centurión, M.E., Fragoso, W.D., Almeida, L.F., de Araújo, M.C.U., Band, B.S.F., Flow-batch technique for the simultaneous enzymatic determination of levodopa and carbidopa in pharmaceuticals using PLS and successive projections algorithm (2008) Talanta, 75, pp. 950-958Kaur, K., Malik, A.K., Singh, B., Godarzi, M., Simultaneous spectrophotometric determination of carbidopa and levodopa by partial least squares regression, principal component regression and least squares support vector machine methods (2009) Thai J. Pharm. Sci., 33, pp. 123-136Marques, K.L., Santos, J.L.M., Lopes, J.A., Lima, J.L.F.C., Simultaneous chemiluminometric determination of levodopa and benzerazide in a multi-pumping flow system with multivariate calibration (2008) Anal. Sci., 24, pp. 985-991Zhao, S., Bai, W., Wang, B., He, M., Determination of levodopa by capillary electrophoresis with chemiluminescence detection (2007) Talanta, 73, pp. 142-146Li, S., Wu, H., Yu, Y., Li, Y., Nie, J., Fu, H., Yu, R., Quantitative analysis of levodopa, carbidopa and methyldopa in human plasma samples using HPLC-DAD combined with second-order calibration based on alternating trilinear decomposition algorithm (2010) Talanta, 81, pp. 805-812Muzzi, C., Bertocci, E., Terzuoli, L., Porcelli, B., Ciari, I., Pagani, R., Guerranti, R., Simultaneous determination of serum concentrations of levodopa, dopamine, 3-O-methyldopa and α-methyldopa by HPLC (2008) Biomed. Pharmacother., 62, pp. 253-258Talebpour, Z., Haghgoob, S., Shamsipur, M., 1H nuclear magnetic resonance spectroscopy analysis for simultaneous determination of levodopa, carbidopa and methyldopa in human serum and pharmaceutical formulations (2004) Anal. Chim. Acta, 506, pp. 97-104Aslanoglu, M., Kutluay, A., Goktas, S., Karabulut, S., Voltammetric behaviour of levodopa and its quantification in pharmaceuticals using a β-cyclodextrine doped poly(2,5-diaminobenzenesulfonic acid) modified electrode (2009) J. Chem. Sci., 121, pp. 209-215Shahrokhian, S., Asadian, E., Electrochemical determination of L-Dopa in the presence of ascorbic acid on the surface of the glassy carbon electrode modified by a bilayer of multi-walled carbon nanotube and poly-pyrrole doped with tiron (2009) J. Electroanal. Chem., 636, pp. 40-46Ensafi, A.A., Arabzadeh, A., Karimi-Maleh, H., Sequential determination of benserazide and levodopa by voltammetric method using chloranil as a mediator (2010) J. Braz. Chem. Soc., 21, pp. 1572-1580Nematollahi, D., Rafiee, M., Fotouhi, L., Mechanistic study of homogeneous reactions coupled with electrochemical oxidation of catechols (2009) J. Iran. Chem. Soc., 6, pp. 448-476Rafiee, M., Nematollahi, D., Electrochemical oxidation of catechols in the presence of cyanoacetone and methyl cyanoacetate (2009) J. Electroanal. Chem., 626, pp. 36-41Teixeira, M.F.S., Bergamini, M.F., Marques, C.M.P., Bocchi, N., Voltammetric determination of L-Dopa using an electrode modified with trinuclear ruthenium ammine complex (Ru-red) supported on Y-type zeolite (2004) Talanta, 63, pp. 1083-1088Tu, Y., Xu, Q., Zou, Q., Yin, Z., Sun, Y., Zhao, Y., Electrochemical behavior of levodopa at multi-wall carbon nanotubes-quantum dots modified glassy carbon electrodes (2007) Anal. Sci., 23, pp. 1321-1324Yaghoubian, H., Karimi-Maleh, H., Khalilzadeh, M.A., Karimi, F., Electrocatalytic oxidation of levodopa at a ferrocene modified carbon nanotube paste electrode (2009) Int. J. 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Electrocatalytic Determination Of Reduced Glutathione In Human Erythrocytes

The determination of reduced glutathione (GSH) in human erythrocytes using a simple, fast and sensitive method employing a glassy carbon electrode modified with cobalt tetrasulfonated phthalocyanine (CoTSPc) immobilized in poly(l-lysine) (PLL) film was investigated. This modified electrode showed very efficient electrocatalytic activity for anodic oxidation of GSH, decreasing substantially the anodic overpotentials for 0.2 V versus Ag/AgCl. The modified electrode presented better performance in 0.1 mol l-1 piperazine-N,N-bis(2-ethanesulfonic acid) buffer at pH 7.4. The other experimental parameters, such as the concentration of CoTSPc and PLL in the membrane preparation, pH, type of buffer solution and applied potential, were optimized. Under optimized operational conditions, a linear response from 50 to 2,160 nmol l-1 was obtained with a high sensitivity of 1.5 nA l nmol-1 cm-2. The detection limit for GSH determination was 15 nmol l-1. The proposed sensor presented good repeatability, evaluated in terms of the relative standard deviation (1.5%) for n∈=∈10. The modified electrode was applied for determination of GSH in erythrocyte samples and the results were in agreement with those obtained by a comparative method described in the literature The average recovery for these fortified samples was 100∈±∈1)%. 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Development Of A Voltammetric Sensor For Catechol In Nanomolar Levels Using A Modified Electrode With Cu(phen)2(tcnq)2 And Pll

A sensor based on glassy carbon (GC) electrode modified with bis(1,10-phenantroline)copper(II) bis(tetracyanoquinodimethanide) [Cu(phen)2(TCNQ)2] immobilized in a poly-l-lysine (PLL) film is proposed for catechol (CA) determination with differential pulse voltammetry (DPV) technique. The modified electrode showed excellent stability as well as the ability to detect catechol in nanomolar catechol levels. A linear response range from 10 nmol l-1 up to 20 μmol l-1 with a sensitivity of 2.29 μA l μmol-1 cm-2 and detection limit of 3.0 nmol l-1 were observed in the optimized conditions. The repeatability of the mesurements with the proposed sensor was 2% evaluated in term of relative standard deviation, with n = 10 for 10 μmol l-1 CA. Cyclic voltammetry and rotating disk electrode (RDE) experiments indicated that the catechol oxidation reaction involves two-electrons and a heterogenous rate constant (k) average value of about 1.30 × 103 M-1 s-1. The catechol diffusion coefficient (Do) value was estimated as being 7.6 × 10-6 cm2 s-1. The sensor was successfully applied for CA determination in powdered guarana samples. © 2005 Elsevier B.V. All rights reserved.1171274281Solná, R., Sapelnikova, S., Skládal, P., Winther-Nielsen, M., Carlsson, C., Emnéus, J., Ruzgas, T., Multienzyme electrochemical array sensor for determination of phenols and pesticides (2005) Talanta, 65, pp. 349-357Lin, X., Gong, J., Electrocatalytic oxidation and selective detection of dopamine at a 5,5-ditetradecyl-2-(2-trimethyl-ammonioethyl)-1,3-dioxane bromide self-assembled bilayer membrane modified glassy carbon electrode (2004) Anal. Chim. 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A, 855, pp. 171-179Maurer, H.H., Bickeboeller-Friedrich, J., Kraemer, T., Gas chromatographic-mass spectrometric procedures for determination of the catechol-O-methyltransferase (COMT) activity and for detection of unstable catecholic metabolites in human and rat liver preparations after (COMT) catalyzed in statu nascendi derivatization using S-adenosylmethionine (2000) J. Chromatogr. B, 739, pp. 325-335Fiehn, O., Jekel, M., Analysis of phenolic compounds in industrial wastewater with high-performance liquid chromatography and post-column reaction detection (1997) J. Chromatogr. A, 769, pp. 189-200Sotomayor, M.D.P.T., Tanaka, A.A., Kubota, L.T., Tris (2,2′-bipyridil) copper (II) chloride complex: a biomimetic tyrosinase catalyst in the amperometric sensor construction (2003) Electrochim. Acta, 48, pp. 855-865Carvalho, R.M., Mello, C., Kubota, L.T., Simultaneous determination of phenol isomers in binary mixtures by differential pulse voltammetry using carbon fibre electrode and neural network with pruning as a multivariate calibration tool (2000) Anal. Chim. Acta, 420, pp. 109-121Mello, L.D., Stomayor, M.D.P.T., Kubota, L.T., HRP-based amperometric biosensor for the polyphenols determination in vegetables extract (2003) Sens. Actuators B: Chem., 96, pp. 636-645Murray, R.W., (1984) Electroanalytical Chemistry, , Bard A.J. (Ed), Marcel Dekker, New YorkRedepenning, J.G., Chemically modified electrodes-a general overview (1987) Tracs-Trends Anal. Chem., 6, pp. 18-22Razmi, H., Agazadeh, M., Habibi-A, B., Electrocatalytic oxidation of dopamine at aluminum electrode modified with nickel pentacyanonitrosylferrate films, synthesized by electroless procedure (2003) J. Electroanal. Chem., 547, pp. 25-33Damos, F.S., Sotomayor, M.D.T., Kubota, L.T., Tanaka, S.M.C.N., Tanaka, A.A., Iron(III) tetra-(N-methyl-4-pyridyl)-porphyrin as a biomimetic catalyst of horseradish peroxidase on the electrode surface: an amperometric sensor for phenolic compound determinations (2003) Analyst, 128, pp. 225-259Dempsey, E., Diamond, D., Collier, A., Development of a biosensor for endocrine disrupting compounds based on tyrosinase entrapped within a poly(thionine) film (2004) Biosens. Bioelectron., 20, pp. 367-377Rajesh, W., Kaneto, K., Amperometric tyrosinase based biosensor using an electropolymerized PTS-doped polypyrrole film as an entrapment support (2004) React. Funct. Polym., 59, pp. 163-169Campuzano, S., Serra, B., Pedrero, M., Villena, F.J.M., Pingarrón, J.M., Amperometric flow-injection determination of phenolic compounds at self-assembled monolayer-based tyrosinase biosensors (2003) Anal. Chim. 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Dna And Graphene As A New Efficient Platform For Entrapment Of Methylene Blue (mb): Studies Of The Electrocatalytic Oxidation Of β-nicotinamide Adenine Dinucleotide

The modification of glassy carbon (GC) electrode with deoxyribonucleic acid (DNA) and grapheneis utilized as a new efficient platform for entrapment of methylene blue (MB). Electrochemical andelectroanalytical properties of the modified electrode (DNA/graphene/MB) were investigated by cyclicvoltammetry (CV), electrochemical impedance spectroscopy (EIS) and amperometry techniques. Cyclicvoltammetric results indicated the excellent electrocatalytic activity of the resulting electrode toward oxidation of β-nicotinamide adenine dinucleotide (NADH) at reduced overpotential (0.1 V vs. Ag/AgCl).It has been found that the DNA/graphene/MB modification has significantly enhanced the effective electrode response toward NADH oxidation. Cyclic voltammetry and rotating disk electrode (RDE) exper-iments indicated that the NADH oxidation reaction involves two electrons and an electrocatalytic rateconstant (kobs) of 1.75 × 106mol-1L s-1. The electrochemical sensor presented better performance in0.1 mol L-1phosphate buffer at pH 7.0. Other experimental parameters, such as the DNA, graphene, MB concentrations and the applied potential were optimized. Under optimized conditions, a linear response range from 10 μmol L-1to 1.50 mmol L-1was obtained with a sensitivity of 12.75 μA L μmol -1. The detection and quantification limits for NADH determination were 1.0 μmol L-1and 3.3 μmol L-1, respectively.© 2013 Elsevier Ltd. All rights reserved.111543551Li, Z., Huang, Y., Chen, L., Qin, X., Huang, Z., Zhou, Y., Meng, Y., Yao, S., Amperometric biosensor for NADH and ethanol based on electroreduced graphene oxide-polythionine nanocomposite film (2013) Sens. Actuators B, 181, pp. 280-287Creanga, C., El Murr, N., Development of new disposable NADH biosensors based on NADH oxidase (2011) J. Electroanal. 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Acta, 747, pp. 84-91Sharifi, E., Salimi, A., Shams, E., Electrocatalytic activity of nickel oxide nanopar-ticles as mediatorless system for NADH and ethanol sensing at physiological pH solution (2013) Biosens. Bioelectron., 45, pp. 260-266Sun, Y., Ren, Q., Liu, X., Zhao, S., Qin, Y., A simple route to fabricate controllable and stable multilayered all-MWNTs films and their applications for the detection of NADH at low potentials (2013) Biosens. Bioelectron., 39, pp. 289-295Sosna, M., Bonamore, A., Gorton, L., Boffi, A., Ferapontova, E.E., Direct electro-chemistry and Os-polymer-mediated bioelectrocatalysis of NADH oxidation by Escherichia coli flavohemoglobin at graphiteelectrodes (2013) Biosens. Bioelectron., 42, pp. 219-224Zhaia, X., Li, Y., Liua, G., Cao, Y., Gao, H., Yue, C., Sheng, N., Electropolymerizedtoluidine blue O functionalized ordered mesoporous carbon-ionic liquid gel-modified electrode and its low-potential detection of NADH (2013) Sens. Actuators B, 178, pp. 169-175Ratinac, K.R., Yang, W., Gooding, J.J., Thordarson, P., Braet, F., Graphene and related materials in electrochemical sensing (2011) Electroanalysis, 23, pp. 803-826Shao, Y., Wang, J., Wu, H., Liu, J., Aksay, I.A., Lin, Y., Graphene based electrochemical sensors and biosensors: A review (2010) Electroanalysis, 22, pp. 1027-1036Park, S., Ruoff, R.S., Chemical methods for the production of graphenes (2009) Nat. Nanotechnol., 4, pp. 217-224Navaee, A., Salimi, A., Teymourian, H., Graphene nanosheets modified glassy car-bon electrode for simultaneous detection of heroine, morphine and noscapine (2012) Biosens. Bioelectron., 31, pp. 205-211Banhart, F., Kotakoski, J., Krasheninnikov, A.V., Structural defects in graphene (2011) ACS Nano, 5, pp. 26-41Li, D., Muller, M.B., Gilje, S., Kaner, R.B., Wallace, G.G., Processable aqueous dispersions of graphene nanosheets (2008) Nat. 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Development And Evaluation Of A Spr-based Immunosensor For Detection Of Anti-trypanosoma Cruzi Antibodies In Human Serum

Protozoan Trypanosoma cruzi is the etiological agent of Chagas disease, which needs urgent progress in its immunological diagnosis. Surface plasmon resonance (SPR) is a promising technique for the development of immunosensors with biomedical applications. In this work, a SPR-based immunosensor has been developed by the first time for real time and label free immunoassay for detection of anti-T. cruzi antibodies in serum samples. T. cruzi antigen was successfully immobilized on a SPR sensor chip via activated mixed self-assembled monolayer (SAM) of 3-mercaptopropionic acid (3-MPA) and 11-mercaptoundecanoic acid (11-MUA), by amide coupling. After the sensor construction, a pool of human sera infected with T. cruzi was added to its surface and the antibodies were detected in sera diluted up to 1280 times, indicating excellent sensitivity of the technique for detection of antigen-antibody interaction. The addition of a pool of negative human serum at dilutions lower than 1:160 to the sensor surface was accompanied by a null or very low response. Then, the following operational parameters of the immunoassay were optimized and defined: time of immobilization and antigen concentration at 20 min and 30 mg mL-1, serum dilution at 1:320, preventing of nonspecific bindings with solution of BSA 1.0% and surface regeneration by injection of SDS 1.0%. The immunoassay, here termed SPRCruzi, showed high capability in the discrimination of positive and negative sera, including those infected with other pathogens usually sources of false positives results in conventional serodiagnosis. 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