Carbon Nanotube Based Sensor For Simultaneous Determination Of Acetaminophen And Ascorbic Acid Exploiting Multiple Response Optimization And Measures In The Presence Of Surfactant

A simple procedure for the simultaneous determination of acetaminophen (AC) and ascorbic acid (AA) by differential pulse voltammetry (DPV) using a carbon nanotube paste electrode exploiting measures in cetylpyridinium bromide (CPB) medium is described. Under the best instrumental parameters of DPV, optimized by means of factorial design, the calibration plots in the range 100.0-700.0μmolL-1 (r=0.993) and 39.4-146.3μmolL-1 (r=0.995) with limits of detection of 7.1 and 2.1μmolL-1, were achieved for AA and AC, respectively. The developed method was successfully applied for the AC and AA determination in pharmaceutical formulations, whose accuracy was attested by comparison with HPLC method. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.241222912301Goyal, R.N., Singh, S.P., (2006) Electrochim. Acta, 51, p. 3008Fan, Y., Liu, J.-H., Lu, H.-T., Zhang, Q., (2011) Colloids Surf. B, 85, p. 289Özcan, L., Şahin, Y.S., (2007) Sens. Actuators B, 127, p. 362Goyal, R.N., Gupta, V.K., Oyama, M., Bachheti, N., (2005) Electrochem. Commun., 7, p. 803Kachoosangi, R.T., Wildgoose, G.G., Compton, R.G., (2008) Anal. Chim. Acta, 618, p. 54Shankaran, D.R., Iimura, K., Kato, T., (2003) Sens. Actuators B, 94, p. 73Padayatty, S.J., Katz, A., Wang, Y., Eck, P., Kwon, O., Lee, J.-H., Chen, S., Levine, M., (2003) J. Am. Coll. Nutr., 22, p. 18Tsvetkova, B., Pencheva, I., Zlatkov, A., Peikov, P., (2012) Afr. J. Pharm. Pharmacol., 6, p. 1332Sarakbi, A., Aydogmus, Z., Sidali, T., Gokce, G., Kauffamann, J., (2011) Electroanalysis, 23, p. 29Atta, N.F., El-Kady, M.F., (2009) Talanta, 79, p. 639Nair, S.S., John, S.A., Sagara, T., (2009) Electrochim. Acta, 54, p. 6837Atta, N.F., El-Kady, M.F., Galal, A., (2010) Anal. Biochem., 400, p. 78DosSantos, W.T.P., DeAlmeira, E.G.N., Ferreira, H.E.A., Gimenes, D.T., Richter, E.M., (2008) Electroanalysis, 20, p. 1878Rodovan, C., Cofan, C., Cinghita, D., (2008) Electroanalysis, 20, p. 1353Cofan, C., Rodavan, C., (2008) Sensor, 8, p. 3952Jacobs, C.B., Peairs, M.J., Venton, B.J., (2010) Anal. Chim. Acta, 662, p. 105Agüí, L., Yáñez-Sedeño, P., Pingaron, J.M., (2008) Anal. Chim. Acta, 622, p. 11Ionescu, M.I., Zhang, Y., Li, R., Sun, X., Abou-Rachid, H., Lussier, L.S., (2011) Appl. Surf. Sci., (6843), p. 257Menezes, V.M.D., Rocha, A.R., Zanella, I., Mota, R., Fazzio, A., Fagan, S.B., (2011) Chem. Phys. Lett., (233), p. 506Sharokhian, S., Asadian, E., (2010) Electrochim. Acta, 55, p. 666Ensafi, A.A., Karimi-Maleh, H., Mallakpour, S., (2012) Electroanalysis, 24, p. 666Habibi, B., Jahanbakhshi, M., Pournaghi-Azar, M.H., (2011) Anal. Biochem., 411, p. 167P.R. Dalmasso, M.L. Pedano, G.A. Rivas, Sens. Actuators B 2012, 173, 732Havens, N., Trihn, P., Kim, D., Luna, M., Wanekaya, A.K., Mugweru, A., (2010) Electrochim. Acta, 55, p. 2186Juan, P., Zuo-Ning, G., (2006) Anal. Bioanal. Chem., 384, p. 1525DosReis, A.P., Tarley, C.R.T., Kubota, L.T., (2005) Talanta, 67, p. 829DosReis, A.P., Tarley, C.R.T., Mello, L.D., Kubota, L.T., (2008) Anal. Sci., 24, p. 1569DosReis, A.P., Tarley, C.R.T., Kubota, L.T., (2008) J. Braz. Chem. Soc., 19, p. 1567Jain, R., Rather, J.A., (2011) Colloids Surf. B, 83, p. 340Wen, X.-L., Jia, Y.-H., Liu, Z.-L., (1999) Talanta, 50, p. 1027Atta, N.F., Darwish, S.A., Khalil, S.E., Galal, A., (2007) Talanta, 72, p. 1438Li, C., (2007) Colloids Surf. B, 55, p. 77Wang, X.-G., Wu, Q.-S., Liu, W.-Z., Ding, Y.-P., (2006) Electrochim. Acta, 52, p. 589Tarley, C.R.T., Silveira, G., DosSantos, W.N., Matos, G.D., DaSilva, E.G., Bezerra, M.A., Miro, M., Ferreira, S.L., (2009) Microchem. J., 92, p. 58Korany, M.A., Fahmy, O.T., Mahgoub, H., Maher, H.M., (2011) J. Adv. Res., 2, p. 121Santos, V.S., Santos, W.J.R., Kubota, L.T., Tarley, C.R.T., (2009) J. Pharm. Biomed. Anal., 50, p. 151Derringer, G., Suich, R., (1980) J. Quality Technol., 12, p. 214Goyal, R.N., Gupta, V.K., Chatterjee, S., (2010) Sens. Actuators B, 149, p. 252Weast, R.C., (1984) CRC Handbook of Chemistry and Physics, , CRC Press, FloridaLiu, L., Zhao, F., Xiao, F., Zeng, B., (2009) Int. J. Electrochem. Sci., 4, p. 525Bard, A.J., Faulkner, L.R., (2001) Electrochemical Methods, Fundamentals and Applications, , Wiley, New YorkB.B. Neto, I.S. Scarminio, R.E. Bruns, Como Fazer Experimentos: Pesquisa e Desenvolvimento na Ciência e na Indústria, Bookman, Porto Alegre 2010Long, G.L., Winefordner, J.D., (1983) Anal. Chem., 55, p. 71

Improved Selective Cholesterol Adsorption By Molecularly Imprinted Poly(methacrylic Acid)/silica (pmaa-sio2) Hybrid Material Synthesized With Different Molar Ratios

The present paper describes the synthesis of molecularly imprinted polymer - poly(methacrylic acid)/silica and reports its performance feasibility with desired adsorption capacity and selectivity for cholesterol extraction. Two imprinted hybrid materials were synthesized at different methacrylic acid (MAA)/tetraethoxysilane (TEOS) molar ratios (6:1 and 1:5) and characterized by FT-IR, TGA, SEM and textural data. Cholesterol adsorption on hybrid materials took place preferably in apolar solvent medium, especially in chloroform. From the kinetic data, the equilibrium time was reached quickly, being 12 and 20 min for the polymers synthesized at MAA/TEOS molar ratio of 6:1 and 1:5, respectively. The pseudo-second-order model provided the best fit for cholesterol adsorption on polymers, confirming the chemical nature of the adsorption process, while the dual-site Langmuir-Freundlich equation presented the best fit to the experimental data, suggesting the existence of two kinds of adsorption sites on both polymers. The maximum adsorption capacities obtained for the polymers synthesized at MAA/TEOS molar ratios of 6:1 and 1:5 were found to be 214.8 and 166.4 mg g- 1, respectively. The results from isotherm data also indicated higher adsorption capacity for both imprinted polymers regarding to corresponding non-imprinted polymers. Nevertheless, taking into account the retention parameters and selectivity of cholesterol in the presence of structurally analogue compounds (5-α-cholestane and 7-dehydrocholesterol), it was observed that the polymer synthesized at the MAA/TEOS molar ratio of 6:1 was much more selective for cholesterol than the one prepared at the ratio of 1:5, thus suggesting that selective binding sites ascribed to the carboxyl group from MAA play a central role in the imprinting effect created on MIP. © 2014 Elsevier B.V.4499108Gupta, R., Kumar, A., Synthesis and characterization of sol-gel-derived molecular imprinted polymeric materials for cholesterol recognition (2011) J. Sol-Gel Sci. Technol., 58, pp. 182-194Puocci, F., Iemma, F., Cirillo, G., Muzzalupo, R., Spizzirri, U.G., Trombino, S., Cassano, R., Molecularly imprinted polymers based on amidic functional monomers for selective recognition of cholesterol in aqueous media (2006) Macromol. 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Study Of Cross-linked Poly(methacrylic Acid) And Polyvinylimidazole As Selective Adsorbents For On-line Preconcentration And Redox Speciation Of Chromium With Flame Atomic Absorption Spectrometry Determination

A redox speciation and preconcentration study of Cr(III) and Cr(VI) using a flow injection system with dual mini-columns prepared from cross-linked polymers-poly(methacrylic acid) and polyvinylimidazole was developed. Characterization of organic polymers was performed by using FTIR, SEM, TG, C:H:N and BET measurements. The equilibrium data obtained from Cr(III) adsorption on poly(methacrylic acid) and Cr(VI) on polyvinylimidazole were fitted very well to the dual site Langmuir-Freundlich model, suggesting the presence homogeneous and heterogeneous binding site and providing maximum adsorption capacities of 1.42 and 3.24mgg-1, respectively. The adsorption kinetics data were described by the pseudo-second-order model for both polymers, thus corroborating to isotherm data. The on-line preconcentration/speciation system was operated by loading 18.0mL of a solution containing Cr(III) and Cr(VI) at pH4.0 through the dual mini-columns at a flow rate of 3.0mLmin-1, where Cr(III) was selectively retained on poly(methacrylic acid), while Cr(VI) was retained on polyvinylimidazole. The limits of detection were found to be 0.84 and 1.58μgL-1 for Cr(III) and Cr(VI), respectively. The preconcentration factor (PF), consumptive index (CI) and concentration efficiency (CE) were found to be 47.3/8.6, 0.38/2.1mL and 7.88/1.43min-1 for Cr(III) and Cr(VI), respectively. The developed method was successfully applied to the speciation of chromium in different kinds of water samples. Satisfactory recovery values ranging from 89.9 to 108.3% were obtained. © 2014 Elsevier B.V.1171826Idris, S.A., Alotaibi, K., Peshkur, T.A., Anderson, P., Gibson, L.T., Preconcentration and selective extraction of chromium species in water samples using amino modified mesoporous silica (2012) J. 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Grafting 3-mercaptopropyl Trimethoxysilane On Multi-walled Carbon Nanotubes Surface For Improving On-line Cadmium(ii) Preconcentration From Water Samples

In the present study, the performance of multi-walled carbon nanotubes (MWCNTs) grafted with 3-mercaptopropyltrimethoxysilane (3-MPTMS), used as a solid phase extractor for Cd2+ preconcentration in a flow injection system coupled to flame atomic absorption spectrometry (FAAS), was evaluated. The procedure involved the preconcentration of 20.0mL of Cd2+ solution at pH 7.5 (0.1molL-1 buffer phosphate) through 70mg of 3-MPTMS-grafted MWCNTs packed into a minicolumn at 6.0mLmin-1. The elution step was carried out with 1.0molL-1 HCl. Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were used to estimate the extent of the MWCNT chemical modification. The 3-MPTMS-grafted MWCNTs provided a 1.68 times improvement in the sensitivity of the Cd2+ FAAS determination compared to the unsilanized oxidized MWCNTs. 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Ion Imprinted Polymers: Fundamentals, Preparation Strategies And Applications In Analytical Chemistry [polímeros Impressos Com íons: Fundamentos, Estratégias De Preparo E Aplicações Em Química Analítica]

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Evaluation Of Boron-doped Diamond Electrode For Simultaneous Voltammetric Determination Of Hydrochlorothiazide And Losartan In Pharmaceutical Formulations

A method for the simultaneous determination of hydrochlorothiazide (HCTZ) and losartan (LOS) in pharmaceutical formulations using differential-pulse voltammetry (DPV) was developed. Two very well-resolved and reproducible oxidation peaks of HCTZ and LOS, with separation of 0.23 V, were obtained in Britton-Robinson (BR) buffer (pH 9.5) using an anodically pretreated boron-doped diamond electrode. Under the optimum analytical experimental conditions, the voltammetric method exhibited linear responses for simultaneous determination of HCTZ and LOS in the concentration range 3.0 × 10-6 to 7.4 × 10-5 mol L-1 for both compounds, with detection limits of 1.2 × 10-6 mol L-1 and 9.5 × 10 -7 mol L-1, respectively. The proposed method was successfully applied in the simultaneous determination of LOS and HCTZ content in pharmaceutical formulations, whose accuracy was attested by good agreement of the results (paired t-test at a 95% confidence level) with those obtained using high performance liquid chromatography (HPLC). © 2013 Published by Elsevier B.V.188263270Hardman, J.G., Limbird, L.E., Gilman, A.G., (1996) Goodman & Gilman's - The Pharmacological Basis of Therapeutics, , 9th ed. 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of hydrochlorothiazide and several angiotensin-II-receptor antagonists by capillary electrophoresis (2003) Journal of Pharmaceutical and Biomedical Analysis, 31 (2), pp. 329-339. , DOI 10.1016/S0731-7085(02)00643-X, PII S073170850200643XLastra, O.C., Lemus, I.G., Sanchez, H.J., Perez, R.F., Development and validation of an UV derivative spectrophotometric determination of Losartan potassium in tablets (2003) Journal of Pharmaceutical and Biomedical Analysis, 33 (2), pp. 175-180. , DOI 10.1016/S0731-7085(03)00347-9Ansari, M., Kazemipour, M., Baradaran, M., Jalalizadeh, H., Derivative spectrophotometric method for determination of losartan in pharmaceutical formulations (2004) Iranian Journal of Pharmacology and Therapeutics, 3, pp. 21-25Rossini, P.O., Felix, F.S., Angnes, L., A simple and precise conductometric method for the determination of losartan in pharmaceutical products (2012) Central European Journal of Chemistry, 10, pp. 1842-1849(2009) United States Pharmacopoeia, , United 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pharmaceutical products (2008) Portugaliae Electrochimica Acta, 26, pp. 315-2324Razak, O.A., Electrochemical study of hydrochlorothiazide and its determination in urine and tablets (2004) Journal of Pharmaceutical and Biomedical Analysis, 34 (2), pp. 433-440. , DOI 10.1016/S0731-7085(03)00497-7Rezaei, B., Damiri, S., Multiwalled carbon nanotubes modified electrode as a sensor for adsorptive stripping voltammetric determination of hydrochlorothiazide (2008) IEEE Sensors Journal, 8, pp. 1523-1528Karimi-Maleh, H., Ensafi, A.A., Ensafi, H.R., Ferrocenedicarboxylic acid modified carbon paste electrode: A sensor for electrocatalytic determination of hydrochlorothiazide (2009) Journal of the Brazilian Chemical Society, 20, pp. 880-887Dos Santos, S.X., Cavalheiro, E.T.G., Evaluation of the potentialities of a carbon nanotubes/silicone rubber composite electrode in the determination of hydrochlorothiazide (2012) Analytical Letters, 45, pp. 1454-1466Pecková, K., Musilová, J., Barek, J., The use 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Enhanced Selectivity And Sensitivity For Flow Injection Spectrophotometric Determination Of Cobalt Using Solid Phase Extraction With A 2d Ion-imprinted Adsorbent

The present work reports the effectiveness of a 2D imprinting method based on a surface imprinting technique for the development of a selective and sensitive flow sorbent preconcentration system for Co2+ ion determination. Cobalt ions were determined by UV-vis spectrophotometry exploiting the complexation with 1-(2-piridylazo)-2-naphtol (PAN). Based on a coefficient of relative selectivity (k'), the ion-imprinted amino-functionalized silica gel sorbent (ISG), compared with modified but non-imprinted sorbent (MSG) and silica gel (SG), showed a very high selectivity. A limit of detection of 0.51 μg L-1 and precision (n = 10) as a relative standard deviation of 2.63 and 1.50% for Co2+ concentration of 10.0 and 90.0 μg L-1, respectively, were achieved. A comparison of the proposed method with other previously published methods shows advantages in terms of sample consumption, sample throughput, and limit of detection. The application of the present method was successfully performed for the direct determination of Co2+ content in urine and environmental water samples without any interference and without sample preparation, with satisfactory results. © Taylor & Francis Group, LLC.4401/03/15216231Andaçu, M., Ozyapi, E., Senel, S., Say, R., Denizli, A., Ion-selective imprinted beads for aluminum removal from aqueous solutions (2006) Ind. Eng. Chem. Res., 45, pp. 1780-1786Bellamy, L.J., (1958) The Infra-red Spectra of Complex Molecules, , 2nd ed. London: John Wiley & SonsBi, X., Lau, R.J., Yang, K., Preparation of ion-imprinted silica gels functionalized with glycine, diglycine, and triglycine and their adsorption properties for copper ions (2007) Langmuir, 23, pp. 8079-8086Carlosena, A., Gallego, M., Valcárcel, M., Evaluation of various sample preparation produces for the determination of chromium, cobalt and nickel in vegetables (1997) J. Anal. At. 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Enhanced Sorption Of Mn2+ Ions From Aqueous Medium By Inserting Protoporphyrin As A Pendant Group In Poly(vinylpyridine) Network

The main goal of the present work was to evaluate the effect of protoporphyrin (PP) (as pendant group) incorporated into a poly(vinylpyridine) [poly(VPY)] polymer network on the sorption of Mn2+ ions from an aqueous medium. The sorbent materials - poly(PP-co-VPY) and poly(VPY) - were characterized by SEM, FTIR, elemental analysis and nitrogen adsorption-desorption measurements (BET - Barrett-Joyner-Halenda and BJH - Brunauer-Emmett-Teller). It was observed that the pseudo-second-order kinetic model fitted the experimental data very well (R2=0.9967), confirming that the Mn2+ sorption onto poly(PP-co-VPY) took place via chemical reactions (chemisorption). To describe the equilibrium between the Mn2+ ions and sorbents and estimate the maximum sorption capacity, different models, including Langmuir, Freundlich, Dubinin-Radushkevich and dual-site non-linear Langmuir-Freundlich equations, were applied to the experimental data. The dual-site Langmuir-Freundlich model provided the best fit for poly(PP-co-VPY) and poly(VPY), yielding the maximum sorption capacity of 5.0 and 1.79mgg-1, respectively. These findings suggest the presence of homogeneous and heterogeneous binding sites able to sorb Mn2+ ions. Binary solutions of Mn2+/Zn2+, Mn2+/Pb2+ and Mn2+/Fe3+ were submitted to competitive sorption in the polymers. The results obtained for these systems demonstrated 4.75, 18.24 and 388-fold increases in the rate of the Mn2+ sorption onto poly(PP-co-VPY), when compared with poly(VPY). 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