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A sensitive label-free impedimetric DNA biosensor based on silsesquioxane-functionalized gold nanoparticle for Zika Virus detection Marines Steinmetz, Dhésmon Lima, Adriano Viana, Sérgio Toshio Fujiwara, Christiana Andrade Pess?a, Rafael Mazer Etto, Karen WohnrathSupplementary MaterialContentsPage TOC \o "1-3" \h \z \u S1Experimental Section PAGEREF _Toc9376917 \h 3S1.1 ZIKV DNA biosensor preparation PAGEREF _Toc9376918 \h 3S2Characterization of AuNPs-SiPy nanohybrid PAGEREF _Toc9376919 \h 4S3Electrochemical characterization of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] PAGEREF _Toc9376920 \h 9S4Optimization steps of ZIKV DNA Biosensor PAGEREF _Toc9376921 \h 13S5ZIKV DNA Biosensor characterization PAGEREF _Toc9376922 \h 16S6Redox marker effect on ZIKV DNA biosensor PAGEREF _Toc9376923 \h 17S7AuNPs-SiPy influence PAGEREF _Toc9376924 \h 18S8Microscopy characterization of the biosensor PAGEREF _Toc9376925 \h 19S9 Analytical curve PAGEREF _Toc9376926 \h 20S10 Stability of ox-GCE-[AuNPs-SiPy]/ZIKV1 PAGEREF _Toc9376927 \h 21References for the Supplementary Data section PAGEREF _Toc9376928 \h 22Figure Summary TOC \h \z \c "Figure" Figure S2.1: UV-Vis absorption spectra of HAuCl4.3H2O, NaBH4, SiPy and AuNPs-SiPy suspension obtained in aqueous solution. PAGEREF _Toc9376961 \h 4Figure S2.2: (A) Hydrodinamic diameter distribution of the AuNPs-SiPy. (B) Stability study of AuNPs-SiPy for one year. PAGEREF _Toc9376962 \h 5Figure S2.3: FTIR spectra of SiPy and lyophilized AuNPs-SiPy obtained on KBr pellets. PAGEREF _Toc9376963 \h 6Figure S2.4: Raman spectra of solid SiPy and lyophilized AuNPs-SiPy at = 632,8 nm. PAGEREF _Toc9376964 \h 7Figure S2.5: XRD diffraction pattern of solid SiPy and lyophilized AuNps-SiPy. PAGEREF _Toc9376965 \h 8 TOC \h \z \c "Figure: S3.1" Figure S3.1: Cyclic voltammograms of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] obtained in 0.5 mol L-1 H2SO4 at 50.0 mVs?1. PAGEREF _Toc9376977 \h 9Figure S3.2: Stability study of ox-GCE-[AuNPs-SiPy] platform analyzed in terms of (A) Ipc and (B) Epc in relation to the numbers of voltammetric cycles. PAGEREF _Toc9376978 \h 9Figure S3.3: Cyclic voltammograms obtained in 0.15 mol L-1 PBS buffer (pH 7.4) for the bare GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] (scan rate = 50.0 mVs?1). PAGEREF _Toc9376979 \h 10Figure S3.4: (A) Cyclic voltammograms (50.0 mV s-1) and (B) electrochemical impedance spectra (open circuit potential (OCP); frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy], in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6. PAGEREF _Toc9376980 \h 10Figure S3.5: Cyclic voltammograms of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] in 0.5 mol L?1 PBS buffer solution (pH 7.4) containing 5,0 mmol L?1 Ru(NH3)2+/3+. PAGEREF _Toc9376981 \h 11 TOC \h \z \c "Figure S4.1" Figure S4.1: Effect of the amount of AuNPs-SiPy in the biosensor response. PAGEREF _Toc9376991 \h 13Figure S4.2: Pareto chart for the effects resultant of the variable optimization by 32 full factorial design (95% confidence level). PAGEREF _Toc9376992 \h 14Figure S4.3: Effect of the temperature on the ZIKV2 hybridization on ox-GCE-[AuNPs-SiPy]/ZIKV1 biosensor. PAGEREF _Toc9376993 \h 15 TOC \h \z \c "Figure S5.1" Figure S5.1: Electrochemical impedance spectra (OCP; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) of ox-GCE-[AuNPs-SiPy]/cystamine in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L-1 K4Fe(CN)6/K3Fe(CN)6 (cystamine concentration: 1 mmol L-1). PAGEREF _Toc9376999 \h 16 TOC \h \z \c "Figure S6.1" Figure S6.1: Electrochemical impedance spectra (OPC; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) obtained before and after the interaction between the ox-[AuNPs-SiPy] surface and the [Fe(CN)6]3-/4- redox marker (2 h and 2 h 50 min), in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6. PAGEREF _Toc9377007 \h 17 TOC \h \z \c "Figure S7.1" Figure S7.1: Electrochemical impedance spectra (OPC; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) obtained using three different configurations (A) ox-ECV/ZIKV1, (B) ox-ECV-[SiPy]/ZIKV1 e (C) ox-ECV-[AuNPs-SiPy] to hybridize the ZIKV2 ssDNA target in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6. PAGEREF _Toc9377016 \h 18Figure S8.1: AFM images of (A) ox-GCE, (B) ox-GCE-[AuNPs-SiPy], (C) ox-GCE-[AuNPs-SiPy]/ZIKV1, (D) ox-GCE-[AuNPs-SiPy]/ZIKV1/ZIKV2 and (E) ox-ECV-[AuNPs-SiPy]/ZIKV1/No-ZIKV2 (negative control). PAGEREF _Toc9377017 \h 19 TOC \h \z \c "Figure 8.1" Figure S10.1: Long-term stability of the proposed biosensor. PAGEREF _Toc9377041 \h 21Table Summary TOC \h \z \c "Tabela" Table S2.1: Vibrations modes and respective wavenumber values of SiPy and lyophilized AuNPs-SiPy obtained in KBr pellets. PAGEREF _Toc9377260 \h 6 TOC \h \z \c "Table S3.1" Table S3.1: Values of Ipa, Ipc, ΔIp, Epa, Epc, ΔEp, Rs, Rct and Rct error obtained in the CV and EIS measurements for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6. PAGEREF _Toc9377119 \h 11Table S3.2: Values of Ipa, Ipc, ΔIp, Epa, Epc e ΔEp obtained by CV for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy], obtained in presence of 5.0 mmol L?1 Ru(NH3)2+/3+. PAGEREF _Toc9377120 \h 12 TOC \h \z \c "Table S4.1" Table S4.1: Results obtained in the 32 full factorial design for the optimization of the variables involved in the preparation of the ZIKV DNA biosensor. PAGEREF _Toc9377125 \h 14Table S4.2: ANOVA results of the quadratic model for ZIKV DNA biosensor optimization. PAGEREF _Toc9377126 \h 15 TOC \h \z \c "Table S5.1" Table S5.1: Values of Ipa, Ipc, ΔIp, ΔEp, Rs, Rct, ΔRct, Rct error, Cdl and W obtained by CV and EIS at each stage of ox-GCE-[AuNPs-SiPy]/ZIKV1 biossensor construction. PAGEREF _Toc9377130 \h 16 TOC \h \z \c "Table S9.1" Table S9.1: Concentration range of RNA copies present in 1 mL of body fluid in symptomatic patients. PAGEREF _Toc9377202 \h 20S1Experimental SectionS1.1 ZIKV DNA biosensor preparationGCE were first cleaned in concentrated H2SO4 for 2 min, and then thoroughly washed with ultra-pure water water. A mechanical polishing in alumina/water slurry (0.3 μm) on microcloth pads, washed and sonicated in absolute ethanol for 5 min. After an electrochemical treatment in 0.5 mol L-1 H2SO4 (30 voltammetric scans at 100 mV s-1 in the range of -0.3 to 1.5 V (vs. Ag/AgCl)), the oxidized surface of the GCE was modified by dropping 5 ?L of AuNPs-SiPy and allowed to dry for 24 h at room temperature. For the DNA biosensor construction, 15 ?L of ZIKV1 ssDNA probe (5 ?mol L-1) were dropped on the ox-GCE-[AuNPs-SiPy] and incubated for 2 h for Au-S covalent bond formation. The surface was then washed with sterile PBS buffer (pH 7.4) to remove physicaly adsorbed oligonucleotides for 6 s. To the detection of the target sequence or to evaluate the DNA hybridization specificity, 15 ?L of either ZIKV2 ssDNA target (5 ?mol L-1) or No-ZIKV2 ssDNA no target (5 ?mol L-1), respectively, was incubated with the biossensor ox-GCE-[AuNPs-SiPy]/ZIKV1 during 50 min at 37 ?C. After that, the biosensor was rinsed again with PBS buffer (Scheme 1).S2Characterization of AuNPs-SiPy nanohybridUV-Vis spectra of the precursors and the nanohybrid AuNPs-SiPy were obtained (Figure S2.1). The NaBH4 absorption spectrum showed no band in the ultraviolet visible region. The SiPy polymer displayed one absorption band at 259 nm related to π → π* transitions of pyridinium groups ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10971-018-4706-y","ISSN":"1573-4846","author":[{"dropping-particle":"","family":"Ribicki","given":"A. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Chemin","given":"B. G.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Haandel","given":"V. J.","non-dropping-particle":"Van","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Winiarski","given":"J. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rozada","given":"T. de C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Estrada","given":"R. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fiorin","given":"B. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Sol-Gel Science and Technology","id":"ITEM-1","issued":{"date-parts":[["2018"]]},"publisher":"Springer US","title":"Sol gel synthesis of 3- n -propyl ( 4-aminomethyl ) pyridinium silsesquioxane chloride and the enhanced electrocatalytic activity of LbL films","type":"article-journal"},"uris":[""]}],"mendeley":{"formattedCitation":"(Ribicki et al., 2018)","plainTextFormattedCitation":"(Ribicki et al., 2018)","previouslyFormattedCitation":"(Ribicki et al., 2018)"},"properties":{"noteIndex":0},"schema":""}(Ribicki et al., 2018). The [AuCl4]- precursor complex showed a strong absorption at 299 nm, which was ascribed to the ligand-to-metal charge transfer transition between gold and chloride ligands. This band was absent in the spectrum of AuNPs-SiPy, which suggest that the all [AuCl4]- were reduced to AuNPs. Furthermore, the spectrum of AuNPs-SiPy displayed the typical surface plasmon resonance band at 525 nm, suggesting the existence of colloidal AuNPs with sizes lower than 20 nm ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.14219/jada.archive.1988.0050","ISSN":"0003-2697","PMID":"9750129","abstract":"In a companion article we present the idea that submicroscopic light-scattering particles, such as gold and silver particles, can be used as fluorescent analog tracers in biological and clinical applications. The light-emitting power and scattered light color of the particles can be adjusted by changing particle composition or diameter. Using Rayleigh and Mie light-scattering theory, we calculated the absorbance and light-scattering properties and power of particles of different diameters and selected compositions and compared them to the properties of fluorophores. In the present article, we evaluate experimentally the optical properties of particles of selected compositions and sizes and compare the results with the theoretically calculated values. We also discuss the methods which we use to measure the light-scattering properties of particles in suspension and to view individual particles by light microscopy. We also outline examples which demonstrate the use of light-scattering particles as fluorescent analogs in biological and clinical applications.","author":[{"dropping-particle":"","family":"Yguerabide","given":"J.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Yguerabide","given":"E. E.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Analytical Biochemistry","id":"ITEM-1","issued":{"date-parts":[["1988"]]},"page":"137-156","title":"Light-scattering submicroscopic particles as highly fluorescent analogs and their use as tracer labels in clinical and biological applications","type":"article-journal","volume":"262"},"uris":[""]}],"mendeley":{"formattedCitation":"(Yguerabide and Yguerabide, 1988)","manualFormatting":"(Yguerabide and Yguerabide 1988","plainTextFormattedCitation":"(Yguerabide and Yguerabide, 1988)","previouslyFormattedCitation":"(Yguerabide and Yguerabide, 1988)"},"properties":{"noteIndex":0},"schema":""}(Yguerabide and Yguerabide 1988; ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s11051-012-1081-4","ISSN":"13880764","abstract":"We describe the preparation of platinum nanoparticles (PtNPs) using the 3-n-propylpyridinium silsesquioxane chloride (SiPy+Cl-) as a nanoreactor and stabilizer. The formation of PtNPs was monitored by UV-Vis spectroscopy by measuring the decrease in the intensity of the band at 375 nm, which is attributed to the electronic absorption of PtCl62-ions. TEM images of Pt-SiPy+Cl-nanohybrid indicated an average size of 3-40 nm for PtNPs. The Pt-SiPy+Cl-was used as a polycation in the preparation of layerby- layer films (LbL) on a glass substrate coated with fluorine-doped tin oxide (FTO) alternating with the polyanion poly(vinyl sulfonic acid) (PVS). The films were electrochemically tested in sulfuric acid to confirm the deposition of Pt-SiPy+Cl-onto the LbL films, observing the adsorption and desorption of hydrogen (Epa= 0.1 V) and by the redox process of formation for PtO with Epa= 1.3 V and Epc= 0.65 V. FTIR and Raman spectra confirmed the presence of the PVS and Pt-SiPy+Cl-in the LbL films. A linear increase in the absorbance in the UV- Vis spectra of the Pt-SiPy+Cl-at 258 nm (φ → φ transition of the pyridine groups) with a number of Pt- SiPy+Cl-/PVS or PVS/SiPy+Cl-bilayers (R = 0.992) was observed. These LbL films were tested for the determination of dopamine (DA) in the presence of ascorbic acid (AA) with a detection limit (DL) on the order of 2.6 x 10-6mol L-1and a quantification limit (QL) of 8.6 x 10-6mol L-1. The films exhibited a good repeatability and reproducibility, providing a potential difference of 550 mV for the oxidation of DA with AA interferent. ? Springer Science+Business Media B.V. 2012.","author":[{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Jesus","given":"C. G.","non-dropping-particle":"De","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Canestraro","given":"C. D.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Zucolotto","given":"V.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Nanoparticle Research","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2012"]]},"title":"Platinum nanoparticles incorporated in silsesquioxane for use in LbL films for the simultaneous detection of dopamine and ascorbic acid","type":"article-journal","volume":"14"},"uris":[""]}],"mendeley":{"formattedCitation":"(Dos Santos et al., 2012)","manualFormatting":"Dos Santos et al. 2012)","plainTextFormattedCitation":"(Dos Santos et al., 2012)","previouslyFormattedCitation":"(Dos Santos et al., 2012)"},"properties":{"noteIndex":0},"schema":""}Dos Santos et al. 2012).Figure S2. SEQ Figure \* ARABIC 1: UV-Vis absorption spectra of HAuCl4.3H2O, NaBH4, SiPy and AuNPs-SiPy suspension obtained in aqueous solution.Zeta potential analysis suggested that the obtained nanohybrid had positively charged groups and formed a stable colloidal suspension (= +35.3 mV). Dynamic light scattering (DLS) showed a small hydrodynamic diameter size distribution of 13.0 ± 3.7 nm (Figure S2.2 (A)), which is in good agreement with the literature ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1016/j.electacta.2017.07.185","ISSN":"00134686","abstract":"This paper reports the electrocatalytic properties of layer by layer (LbL) films formed by gold nanoparticles stabilized in propylpyridinium silsesquioxane polymer (AuNPs-SiPy+) as polycation, and prussian blue nanoparticles (PB) as polyanion with synergistic effect in the H2O2reduction. Under optimized synthesis conditions by factorial design, the TEM images of gold nanoparticles showed spherical shape with diameter ranging from 2 to 35 nm. All modified electrodes with inorganic materials were explored by spectroscopy (UV-Vis and FTIR) and electrochemical techniques (Cyclic Voltammetry, Chronoamperometry and Electrochemical Impedance Spectroscopy). We demonstrated that the presence of gold nanoparticles greatly enhanced the electroactive properties of the multilayer films providing interesting electrochemical features and excellent sensitivity in the electrocatalytic reduction of hydrogen peroxide, compared to electrode containing only the silsesquioxane polymer as cationic polyelectrolyte.","author":[{"dropping-particle":"","family":"Cala?a","given":"Giselle Nathaly","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Erdmann","given":"Cristiane Andreia","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Soares","given":"Ana Letícia","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pess?a","given":"Christiana Andrade","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"Sergio Toshio","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"Jarem Raul","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Vidotti","given":"Marcio","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"Karen","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Electrochimica Acta","id":"ITEM-1","issued":{"date-parts":[["2017"]]},"page":"104-112","publisher":"Elsevier Ltd","title":"Layer-by-Layer AuNPs-SiPy+/prussian blue nanoparticles modified electrodes: characterization and electrocatalytic effects","type":"article-journal","volume":"249"},"uris":[""]}],"mendeley":{"formattedCitation":"(Cala?a et al., 2017)","plainTextFormattedCitation":"(Cala?a et al., 2017)","previouslyFormattedCitation":"(Cala?a et al., 2017)"},"properties":{"noteIndex":0},"schema":""}(Cala?a et al., 2017). The colloidal suspension did not present aggregates nor color variation for one year, evidencing the fact that the SiPy polymer consists in an efficient stabilizing agent (Figure S2.2 (B)). Figure S2. SEQ Figure \* ARABIC 2: (A) Hydrodinamic diameter distribution of the AuNPs-SiPy. (B) Stability study of AuNPs-SiPy for one year.The FTIR spectra of the SiPy polymer and the AuNPs-SiPy are shown in Figure S2.3. The bands at 1636 and 1487 cm-1 correspond to the stretching (ν) of the pyridinium ring, whereas the absorption at 680 cm-1 was ascribed to the bending mode (δ) of the Si-H group and those at 1087 and 768/460 cm-1 were attributed to the Si-O-Si asymmetric and symmetric stretching, respectively, of the SiPy structure ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10971-018-4706-y","ISSN":"1573-4846","author":[{"dropping-particle":"","family":"Ribicki","given":"A. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Chemin","given":"B. G.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Haandel","given":"V. J.","non-dropping-particle":"Van","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Winiarski","given":"J. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rozada","given":"T. de C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Estrada","given":"R. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fiorin","given":"B. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Sol-Gel Science and Technology","id":"ITEM-1","issued":{"date-parts":[["2018"]]},"publisher":"Springer US","title":"Sol gel synthesis of 3- n -propyl ( 4-aminomethyl ) pyridinium silsesquioxane chloride and the enhanced electrocatalytic activity of LbL films","type":"article-journal"},"uris":[""]}],"mendeley":{"formattedCitation":"(Ribicki et al., 2018)","manualFormatting":"(Ribicki et al., 2018","plainTextFormattedCitation":"(Ribicki et al., 2018)","previouslyFormattedCitation":"(Ribicki et al., 2018)"},"properties":{"noteIndex":0},"schema":""}(Ribicki et al., 2018; ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10800-014-0703-1","ISSN":"0021891X","abstract":"This paper describes the construction, evaluation, and application of an electrochemical sensor for the determination of dopamine (DA) in the presence of ascorbic acid (AA) and uric acid (UA). Satisfactory results were achieved for the simultaneous determination of DA and UA, it was verified that it is possible to detect AA in the presence of DA, but high concentrations of AA interfere in detection of DA. The sensor was constructed using the layer-by-layer (LbL) technique with the modification of the surface of indium tin oxide coated glass (ITO) substrate with nanostructured films comprising a 3-n-propylpyridinium silsesquioxane polymer (SiPy+Cl-) and nickel(II) tetrasulfophthalocyanine (NiTsPc). Using the square wave voltammetry technique (SWV), the LbL modified electrodes produced at different pHs (pH 2 and 8) were used to determine DA in the presence UA, and the electrochemical responses of the electrodes were compared. It was observed that the electrodes with the highest concentration of monomeric species showed the highest current intensity and the lowest peak potential for the DA and UA analytes in analysis of DA and UA, individually and simultaneously, with peak potential separation of 460 mV versus Ag/AgCl. Applying SWV, a linear dynamic range of 10-99 μmol L -1 and 100-900 μmol L-1 with detection limit of 16.8 μmol L-1 and 58.3 μmol L-1 was obtained for DA and UA, respectively. The method has good selectivity and sensitivity, and it was successfully applied to the simultaneous determination of DA and UA in spiked human urine sample. ? 2014 Springer Science+Business Media Dordrecht.","author":[{"dropping-particle":"","family":"Santos","given":"C. S.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Ferreira","given":"R. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Calixto","given":"C. M. F.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rufino","given":"J. L.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Applied Electrochemistry","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2014"]]},"page":"1047-1058","title":"The influence of organization of LbL films containing a silsesquioxane polymer on the electrochemical response of dopamine","type":"article-journal","volume":"44"},"uris":[""]}],"mendeley":{"formattedCitation":"(Santos et al., 2014)","manualFormatting":"Santos et al. 2014)","plainTextFormattedCitation":"(Santos et al., 2014)","previouslyFormattedCitation":"(Santos et al., 2014)"},"properties":{"noteIndex":0},"schema":""}Santos et al. 2014). The spectrum of AuNPs-SiPy was similar to the SiPy spectrum, and some shifts in the absorption bands were observed (Table S2.1). This behavior suggests the existence of interactions between the AuNPs and the SiPy polymer ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1149/2.1001609jes","ISSN":"0013-4651","abstract":"We report the first attempt to use a naturally occurring biopolymer, such as humic acid (HA), as modifiers to prepare a new organicinorganic composite film with the 3-n-propylpyridiniumsilsesquioxane chloride Pt nanoparticles (Pt-SiPy+Cl-). By using layer-by-layer (LbL) technique, we have constructed multilayered films, (HA/Pt-SiPy+Cl-)(n) and (Pt-SiPy+Cl-/HA)(n), with adjustable thickness due to negatively charged macromolecule HA, which assists the electrostatic interaction with the positively charged of the Pt-SiPy+Cl- nanohybrid. The combination of these partially charged polyelectrolytes in the LbL film was explored by spectroscopic and electrochemical techniques. The formation of the film (HA/Pt-SiPy+Cl-)(n) is more efficient, since the presence of the macromolecule in the inner layer provides a greater number of anchoring sites for the hybrid, ensuring a more linear and uniform growth of the LbL films. This film also presented a better electroanalytical response for oxidation of 17 alpha-ethynylestradiol, EE2, indicating that the Pt nanoparticles strongly influences the electrochemical oxidation of estrogen. The analytical curve for EE2 was linear in the concentration range of 1.37 to 21.4 mu mol L-1 (R = 0.998), with a detection limit of 1.10 mu mol L-1 and quantification limit of 3.68 mu mol L-1. The obtained results showed that the synergism between HA and Pt-SiPy+Cl- improves the electroactive properties of the sensor. (C) 2016 The Electrochemical Society. All rights reserved.","author":[{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wrobel","given":"E. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Quináia","given":"S. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pess?a","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Scheffer","given":"E. W. O.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of The Electrochemical Society","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2016"]]},"page":"B499-B506","title":"Development of an electrochemical sensor based on LbL films of Pt nanoparticles and humic acid","type":"article-journal","volume":"163"},"uris":[""]}],"mendeley":{"formattedCitation":"(dos Santos et al., 2016)","manualFormatting":"(Dos Santos et al. 2016)","plainTextFormattedCitation":"(dos Santos et al., 2016)","previouslyFormattedCitation":"(dos Santos et al., 2016)"},"properties":{"noteIndex":0},"schema":""}(Dos Santos et al. 2016). The AuNPs-SiPy spectrum also demonstrated an apparent decrease in the intensity of the bands, indicating that the stabilization of AuNPs causes a hindrance in the vibrational modes of the polymeric structure, decreasing the degrees of freedom ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1016/j.snb.2017.06.001","ISSN":"09254005","abstract":"In this paper, the 3-n-propylpyridinium silsesquioxane chloride (SiPy+Cl?) polymer was used as a stabilizing agent for the synthesis of gold nanoparticles (AuNps). The formation of AuNPs-SiPy+Cl?was confirmed by UV–vis spectroscopy from the plasmon band at 521 nm, which showed good distribution with size of about 5.0 nm, observed by transmission electron microscopy (TEM) and good stability (ζ = + 38.5 mV) obtained by zeta potential experiments. The surface of the glassy carbon electrode (GCE) was modified with gold nanoparticles (AuNPs-SiPy+Cl?) and subsequent formation of thiolactic acid (TLA) self-assembled monolayer (SAM). For the biosensor construction, horseradish peroxidase (HRP) was covalently immobilized on the surface modified with SAM. The steps of the formation of this biosensor was confirmed by electrochemical impedance spectroscopy (EIS) and field-effect scanning electron microscopy (SEM-FEG). The GCE/AuNps/TLA/HRP biosensor was applied for the detection of cathecol (CT). Under optimized experimental conditions, the biosensor showed an excellent electrocatalytic activity for CT in presence of 0.03 mmol L?1 H2O2in the range of 6.0 at 46.0 μmol L?1, with a low detection limit (LOD = 0.852 μmol L?1) and good sensitivity (0.026 μA.mol L?1). The modified electrode displayed good reproducibility for the determination of catechol and long-term stability of approximately 25 days. The formation of a TLA monolayer on the gold nanoparticles modifying GCE provided a suitable, simple, and low cost platform that could effectively be used to immobilize different enzymes.","author":[{"dropping-particle":"","family":"Mossanha","given":"R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Erdmann","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"C. S.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Sensors and Actuators, B: Chemical","id":"ITEM-1","issued":{"date-parts":[["2017"]]},"page":"747-756","publisher":"Elsevier B.V.","title":"Construction of a biosensor based on SAM of thiolactic acid on gold nanoparticles stabilized by silsesquioxane polyelectrolyte for cathecol determination","type":"article-journal","volume":"252"},"uris":[""]}],"mendeley":{"formattedCitation":"(Mossanha et al., 2017)","plainTextFormattedCitation":"(Mossanha et al., 2017)","previouslyFormattedCitation":"(Mossanha et al., 2017)"},"properties":{"noteIndex":0},"schema":""}(Mossanha et al., 2017). Figure S2. SEQ Figure \* ARABIC 3: FTIR spectra of SiPy and lyophilized AuNPs-SiPy obtained on KBr pellets.Table S2. SEQ Tabela \* ARABIC 1: Vibrations modes and respective wavenumber values of SiPy and lyophilized AuNPs-SiPy obtained in KBr pellets.Vibration modesWavenumber (cm-1)Ref.SiPyAuNPs-SiPyRef.? (pyridinium ring)163614871631148916331486ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1149/2.1001609jes","ISSN":"0013-4651","abstract":"We report the first attempt to use a naturally occurring biopolymer, such as humic acid (HA), as modifiers to prepare a new organicinorganic composite film with the 3-n-propylpyridiniumsilsesquioxane chloride Pt nanoparticles (Pt-SiPy+Cl-). By using layer-by-layer (LbL) technique, we have constructed multilayered films, (HA/Pt-SiPy+Cl-)(n) and (Pt-SiPy+Cl-/HA)(n), with adjustable thickness due to negatively charged macromolecule HA, which assists the electrostatic interaction with the positively charged of the Pt-SiPy+Cl- nanohybrid. The combination of these partially charged polyelectrolytes in the LbL film was explored by spectroscopic and electrochemical techniques. The formation of the film (HA/Pt-SiPy+Cl-)(n) is more efficient, since the presence of the macromolecule in the inner layer provides a greater number of anchoring sites for the hybrid, ensuring a more linear and uniform growth of the LbL films. This film also presented a better electroanalytical response for oxidation of 17 alpha-ethynylestradiol, EE2, indicating that the Pt nanoparticles strongly influences the electrochemical oxidation of estrogen. The analytical curve for EE2 was linear in the concentration range of 1.37 to 21.4 mu mol L-1 (R = 0.998), with a detection limit of 1.10 mu mol L-1 and quantification limit of 3.68 mu mol L-1. The obtained results showed that the synergism between HA and Pt-SiPy+Cl- improves the electroactive properties of the sensor. (C) 2016 The Electrochemical Society. All rights reserved.","author":[{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wrobel","given":"E. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Quináia","given":"S. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pess?a","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Scheffer","given":"E. W. O.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of The Electrochemical Society","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2016"]]},"page":"B499-B506","title":"Development of an electrochemical sensor based on LbL films of Pt nanoparticles and humic acid","type":"article-journal","volume":"163"},"uris":[""]}],"mendeley":{"formattedCitation":"(dos Santos et al., 2016)","plainTextFormattedCitation":"(dos Santos et al., 2016)","previouslyFormattedCitation":"(dos Santos et al., 2016)"},"properties":{"noteIndex":0},"schema":""}(dos Santos et al., 2016)?s (Si-O-Si)774460770466768470ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1016/j.electacta.2017.07.185","ISSN":"00134686","abstract":"This paper reports the electrocatalytic properties of layer by layer (LbL) films formed by gold nanoparticles stabilized in propylpyridinium silsesquioxane polymer (AuNPs-SiPy+) as polycation, and prussian blue nanoparticles (PB) as polyanion with synergistic effect in the H2O2reduction. Under optimized synthesis conditions by factorial design, the TEM images of gold nanoparticles showed spherical shape with diameter ranging from 2 to 35 nm. All modified electrodes with inorganic materials were explored by spectroscopy (UV-Vis and FTIR) and electrochemical techniques (Cyclic Voltammetry, Chronoamperometry and Electrochemical Impedance Spectroscopy). We demonstrated that the presence of gold nanoparticles greatly enhanced the electroactive properties of the multilayer films providing interesting electrochemical features and excellent sensitivity in the electrocatalytic reduction of hydrogen peroxide, compared to electrode containing only the silsesquioxane polymer as cationic polyelectrolyte.","author":[{"dropping-particle":"","family":"Cala?a","given":"Giselle Nathaly","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Erdmann","given":"Cristiane Andreia","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Soares","given":"Ana Letícia","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pess?a","given":"Christiana Andrade","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"Sergio Toshio","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"Jarem Raul","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Vidotti","given":"Marcio","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"Karen","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Electrochimica Acta","id":"ITEM-1","issued":{"date-parts":[["2017"]]},"page":"104-112","publisher":"Elsevier Ltd","title":"Layer-by-Layer AuNPs-SiPy+/prussian blue nanoparticles modified electrodes: characterization and electrocatalytic effects","type":"article-journal","volume":"249"},"uris":[""]}],"mendeley":{"formattedCitation":"(Cala?a et al., 2017)","plainTextFormattedCitation":"(Cala?a et al., 2017)","previouslyFormattedCitation":"(Cala?a et al., 2017)"},"properties":{"noteIndex":0},"schema":""}(Cala?a et al., 2017)ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10971-018-4706-y","ISSN":"1573-4846","author":[{"dropping-particle":"","family":"Ribicki","given":"A. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Chemin","given":"B. G.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Haandel","given":"V. J.","non-dropping-particle":"Van","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Winiarski","given":"J. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rozada","given":"T. de C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Estrada","given":"R. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fiorin","given":"B. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Sol-Gel Science and Technology","id":"ITEM-1","issued":{"date-parts":[["2018"]]},"publisher":"Springer US","title":"Sol gel synthesis of 3- n -propyl ( 4-aminomethyl ) pyridinium silsesquioxane chloride and the enhanced electrocatalytic activity of LbL films","type":"article-journal"},"uris":[""]}],"mendeley":{"formattedCitation":"(Ribicki et al., 2018)","plainTextFormattedCitation":"(Ribicki et al., 2018)","previouslyFormattedCitation":"(Ribicki et al., 2018)"},"properties":{"noteIndex":0},"schema":""}(Ribicki et al., 2018) ?ass (Si-O-Si)114210871133104911301054ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s11051-012-1081-4","ISSN":"13880764","abstract":"We describe the preparation of platinum nanoparticles (PtNPs) using the 3-n-propylpyridinium silsesquioxane chloride (SiPy+Cl-) as a nanoreactor and stabilizer. The formation of PtNPs was monitored by UV-Vis spectroscopy by measuring the decrease in the intensity of the band at 375 nm, which is attributed to the electronic absorption of PtCl62-ions. TEM images of Pt-SiPy+Cl-nanohybrid indicated an average size of 3-40 nm for PtNPs. The Pt-SiPy+Cl-was used as a polycation in the preparation of layerby- layer films (LbL) on a glass substrate coated with fluorine-doped tin oxide (FTO) alternating with the polyanion poly(vinyl sulfonic acid) (PVS). The films were electrochemically tested in sulfuric acid to confirm the deposition of Pt-SiPy+Cl-onto the LbL films, observing the adsorption and desorption of hydrogen (Epa= 0.1 V) and by the redox process of formation for PtO with Epa= 1.3 V and Epc= 0.65 V. FTIR and Raman spectra confirmed the presence of the PVS and Pt-SiPy+Cl-in the LbL films. A linear increase in the absorbance in the UV- Vis spectra of the Pt-SiPy+Cl-at 258 nm (φ → φ transition of the pyridine groups) with a number of Pt- SiPy+Cl-/PVS or PVS/SiPy+Cl-bilayers (R = 0.992) was observed. These LbL films were tested for the determination of dopamine (DA) in the presence of ascorbic acid (AA) with a detection limit (DL) on the order of 2.6 x 10-6mol L-1and a quantification limit (QL) of 8.6 x 10-6mol L-1. The films exhibited a good repeatability and reproducibility, providing a potential difference of 550 mV for the oxidation of DA with AA interferent. ? Springer Science+Business Media B.V. 2012.","author":[{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Jesus","given":"C. G.","non-dropping-particle":"De","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Canestraro","given":"C. D.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Zucolotto","given":"V.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Nanoparticle Research","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2012"]]},"title":"Platinum nanoparticles incorporated in silsesquioxane for use in LbL films for the simultaneous detection of dopamine and ascorbic acid","type":"article-journal","volume":"14"},"uris":[""]}],"mendeley":{"formattedCitation":"(Dos Santos et al., 2012)","plainTextFormattedCitation":"(Dos Santos et al., 2012)","previouslyFormattedCitation":"(Dos Santos et al., 2012)"},"properties":{"noteIndex":0},"schema":""}(Dos Santos et al., 2012)ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10800-014-0703-1","ISSN":"0021891X","abstract":"This paper describes the construction, evaluation, and application of an electrochemical sensor for the determination of dopamine (DA) in the presence of ascorbic acid (AA) and uric acid (UA). Satisfactory results were achieved for the simultaneous determination of DA and UA, it was verified that it is possible to detect AA in the presence of DA, but high concentrations of AA interfere in detection of DA. The sensor was constructed using the layer-by-layer (LbL) technique with the modification of the surface of indium tin oxide coated glass (ITO) substrate with nanostructured films comprising a 3-n-propylpyridinium silsesquioxane polymer (SiPy+Cl-) and nickel(II) tetrasulfophthalocyanine (NiTsPc). Using the square wave voltammetry technique (SWV), the LbL modified electrodes produced at different pHs (pH 2 and 8) were used to determine DA in the presence UA, and the electrochemical responses of the electrodes were compared. It was observed that the electrodes with the highest concentration of monomeric species showed the highest current intensity and the lowest peak potential for the DA and UA analytes in analysis of DA and UA, individually and simultaneously, with peak potential separation of 460 mV versus Ag/AgCl. Applying SWV, a linear dynamic range of 10-99 μmol L -1 and 100-900 μmol L-1 with detection limit of 16.8 μmol L-1 and 58.3 μmol L-1 was obtained for DA and UA, respectively. The method has good selectivity and sensitivity, and it was successfully applied to the simultaneous determination of DA and UA in spiked human urine sample. ? 2014 Springer Science+Business Media Dordrecht.","author":[{"dropping-particle":"","family":"Santos","given":"C. S.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Ferreira","given":"R. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Calixto","given":"C. M. F.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rufino","given":"J. L.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Applied Electrochemistry","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2014"]]},"page":"1047-1058","title":"The influence of organization of LbL films containing a silsesquioxane polymer on the electrochemical response of dopamine","type":"article-journal","volume":"44"},"uris":[""]}],"mendeley":{"formattedCitation":"(Santos et al., 2014)","plainTextFormattedCitation":"(Santos et al., 2014)","previouslyFormattedCitation":"(Santos et al., 2014)"},"properties":{"noteIndex":0},"schema":""}(Santos et al., 2014)δ Si-H680685610ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1149/2.1001609jes","ISSN":"0013-4651","abstract":"We report the first attempt to use a naturally occurring biopolymer, such as humic acid (HA), as modifiers to prepare a new organicinorganic composite film with the 3-n-propylpyridiniumsilsesquioxane chloride Pt nanoparticles (Pt-SiPy+Cl-). By using layer-by-layer (LbL) technique, we have constructed multilayered films, (HA/Pt-SiPy+Cl-)(n) and (Pt-SiPy+Cl-/HA)(n), with adjustable thickness due to negatively charged macromolecule HA, which assists the electrostatic interaction with the positively charged of the Pt-SiPy+Cl- nanohybrid. The combination of these partially charged polyelectrolytes in the LbL film was explored by spectroscopic and electrochemical techniques. The formation of the film (HA/Pt-SiPy+Cl-)(n) is more efficient, since the presence of the macromolecule in the inner layer provides a greater number of anchoring sites for the hybrid, ensuring a more linear and uniform growth of the LbL films. This film also presented a better electroanalytical response for oxidation of 17 alpha-ethynylestradiol, EE2, indicating that the Pt nanoparticles strongly influences the electrochemical oxidation of estrogen. The analytical curve for EE2 was linear in the concentration range of 1.37 to 21.4 mu mol L-1 (R = 0.998), with a detection limit of 1.10 mu mol L-1 and quantification limit of 3.68 mu mol L-1. The obtained results showed that the synergism between HA and Pt-SiPy+Cl- improves the electroactive properties of the sensor. (C) 2016 The Electrochemical Society. All rights reserved.","author":[{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wrobel","given":"E. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Quináia","given":"S. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pess?a","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Scheffer","given":"E. W. O.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Wohnrath","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of The Electrochemical Society","id":"ITEM-1","issue":"9","issued":{"date-parts":[["2016"]]},"page":"B499-B506","title":"Development of an electrochemical sensor based on LbL films of Pt nanoparticles and humic acid","type":"article-journal","volume":"163"},"uris":[""]}],"mendeley":{"formattedCitation":"(dos Santos et al., 2016)","plainTextFormattedCitation":"(dos Santos et al., 2016)","previouslyFormattedCitation":"(dos Santos et al., 2016)"},"properties":{"noteIndex":0},"schema":""}(dos Santos et al., 2016)as = symmetrical, bass = asymmetricalRaman scattering spectra of SiPy and AuNPs-SiPy (Figure S2.4) revealed two bands at 1028 and 647 cm-1, which indicates, respectively, the breathing mode of pyridine ring and the ring in-plane deformation ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s11051-012-1081-4","ISSN":"13880764","abstract":"We describe the preparation of platinum nanoparticles (PtNPs) using the 3-n-propylpyridinium silsesquioxane chloride (SiPy+Cl-) as a nanoreactor and stabilizer. The formation of PtNPs was monitored by UV-Vis spectroscopy by measuring the decrease in the intensity of the band at 375 nm, which is attributed to the electronic absorption of PtCl62-ions. TEM images of Pt-SiPy+Cl-nanohybrid indicated an average size of 3-40 nm for PtNPs. The Pt-SiPy+Cl-was used as a polycation in the preparation of layerby- layer films (LbL) on a glass substrate coated with fluorine-doped tin oxide (FTO) alternating with the polyanion poly(vinyl sulfonic acid) (PVS). The films were electrochemically tested in sulfuric acid to confirm the deposition of Pt-SiPy+Cl-onto the LbL films, observing the adsorption and desorption of hydrogen (Epa= 0.1 V) and by the redox process of formation for PtO with Epa= 1.3 V and Epc= 0.65 V. FTIR and Raman spectra confirmed the presence of the PVS and Pt-SiPy+Cl-in the LbL films. A linear increase in the absorbance in the UV- Vis spectra of the Pt-SiPy+Cl-at 258 nm (φ → φ transition of the pyridine groups) with a number of Pt- SiPy+Cl-/PVS or PVS/SiPy+Cl-bilayers (R = 0.992) was observed. These LbL films were tested for the determination of dopamine (DA) in the presence of ascorbic acid (AA) with a detection limit (DL) on the order of 2.6 x 10-6mol L-1and a quantification limit (QL) of 8.6 x 10-6mol L-1. The films exhibited a good repeatability and reproducibility, providing a potential difference of 550 mV for the oxidation of DA with AA interferent. ? Springer Science+Business Media B.V. 2012.","author":[{"dropping-particle":"","family":"Santos","given":"V.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Jesus","given":"C. G.","non-dropping-particle":"De","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Santos","given":"M.","non-dropping-particle":"Dos","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Canestraro","given":"C. D.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Zucolotto","given":"V.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Garcia","given":"J. R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. 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R.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fateley","given":"W. G.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Benteley","given":"F. F.","non-dropping-particle":"","parse-names":false,"suffix":""}],"id":"ITEM-1","issued":{"date-parts":[["1991"]]},"number-of-pages":"443","publisher":"Wiley-Inter-science","publisher-place":"New York","title":"Characteristic raman frequencies of organic compounds","type":"book"},"uris":[""]}],"mendeley":{"formattedCitation":"(Dollish et al., 1991)","manualFormatting":"Dollish, Fateley and Bentley, 1991)","plainTextFormattedCitation":"(Dollish et al., 1991)","previouslyFormattedCitation":"(Dollish et al., 1991)"},"properties":{"noteIndex":0},"schema":""}Dollish, Fateley and Bentley, 1991). Similarly to the FTIR result, the presence of the AuNPs in the polymer structure resulted in a decrease in the intensity and broadening of these bands, indicating new vibrational modes generated by the interaction between the AuNPs and the polymer.Figure S2. SEQ Figure \* ARABIC 4: Raman spectra of solid SiPy and lyophilized AuNPs-SiPy at = 632,8 nm.The crystalline nature of SiPy and AuNPs-SiPy was confirmed by XRD analysis (Figure S2.5). The SiPy diffractogram exhibited two broad peaks at 5.08? and 22.50?, which were attributed to the intramolecular periodic chain-to-chain distance and the periodic arrangement of Si-O-Si, respectively. However, AuNPs-SiPy diffractogram presented less intense peaks in 3.07? and 22.50?, confirming the incorporation of the AuNPs in the SiPy polymeric structure ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1007/s10971-018-4706-y","ISSN":"1573-4846","author":[{"dropping-particle":"","family":"Ribicki","given":"A. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Chemin","given":"B. G.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Haandel","given":"V. J.","non-dropping-particle":"Van","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Winiarski","given":"J. P.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Rozada","given":"T. de C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Pessoa","given":"C. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Estrada","given":"R. A.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fiorin","given":"B. C.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Fujiwara","given":"S. T.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Journal of Sol-Gel Science and Technology","id":"ITEM-1","issued":{"date-parts":[["2018"]]},"publisher":"Springer US","title":"Sol gel synthesis of 3- n -propyl ( 4-aminomethyl ) pyridinium silsesquioxane chloride and the enhanced electrocatalytic activity of LbL films","type":"article-journal"},"uris":[""]}],"mendeley":{"formattedCitation":"(Ribicki et al., 2018)","plainTextFormattedCitation":"(Ribicki et al., 2018)","previouslyFormattedCitation":"(Ribicki et al., 2018)"},"properties":{"noteIndex":0},"schema":""}(Ribicki et al., 2018). The diffractogram also presents other four characteristic diffraction peaks, at 30.06?, 44.20?, 64.70?, and 77.30?, which were ascribed to (111), (200), (220) and (311) planes, respectively, related to the face centered cubic (fcc) crystalline structure of gold. The higher intensity of (111) diffraction peak reveals that the nanocrystals are mainly oriented along this plane. The lattice constant calculated for (111) diffraction peak was 4.0910 ? for AuNPs-SiPy, which is in close agreement with the value described in the literature (a = 4.0786 ?) ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1016/j.carbpol.2012.08.058","ISBN":"0144-8617","ISSN":"01448617","PMID":"23121940","abstract":"Gold nanoparticles were synthesized by reducing chloroauric acid with a glucan, isolated from an edible mushroom Pleurotus florida, cultivar Assam Florida. Here, glucan acts as reducing as well as stabilizing agent. The synthesized gold nanoparticles were characterized by UV-visible spectroscopy, HR-TEM, XRD, SEM, and FT-IR analysis. The results indicated that the size distribution of gold nanoparticles (Au NPs) changed with the change in concentration of chloroauric acid (HAuCl4). The resulting Au NPs-glucan bioconjugates function as an efficient heterogeneous catalyst in the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP), in the presence of sodium borohydride. The reduction of 4-nitrophenol with Au NPs-glucan bioconjugates followed pseudo-first-order kinetics. The effect of particle size and gold loading on reduction rate of 4-NP was studied with Au NPs-glucan bioconjugates prepared with different concentrations of HAuCl4. The synthesis of catalytically active Au NPs using a pure mushroom polysaccharide of known structure is reported for the first time. ? 2012 Elsevier Ltd.","author":[{"dropping-particle":"","family":"Sen","given":"I. K.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Maity","given":"K.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Islam","given":"S. S.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Carbohydrate Polymers","id":"ITEM-1","issue":"2","issued":{"date-parts":[["2013"]]},"page":"518-528","publisher":"Elsevier Ltd.","title":"Green synthesis of gold nanoparticles using a glucan of an edible mushroom and study of catalytic activity","type":"article-journal","volume":"91"},"uris":[""]}],"mendeley":{"formattedCitation":"(Sen et al., 2013)","plainTextFormattedCitation":"(Sen et al., 2013)","previouslyFormattedCitation":"(Sen et al., 2013)"},"properties":{"noteIndex":0},"schema":""}(Sen et al., 2013).Others six sharps peaks were related to the presence of NaCl, whose crystals were probably formed during the lyophilization process of the AuNPs-SiPy suspension. The presence of Na+ ions could be justified by the addition of the reducing agent NaBH4 and the Cl- is possibly originated from the reduction process of the gold precursor complex ([AuCl4]- + 3e- Au0 + 4 Cl-) or by the solubilization of the polymer SiPy. Figure S2. SEQ Figure \* ARABIC 5: XRD diffraction pattern of solid SiPy and lyophilized AuNps-SiPy.S3Electrochemical characterization of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy]The electrochemical behavior of the bare GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] was investigated by CV measurements in 0.5 mol L-1 H2SO4.Figure S3. SEQ Figure:_S3.1 \* ARABIC 1: Cyclic voltammograms of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] obtained in 0.5 mol L-1 H2SO4 at 50.0 mVs?1.Stability study of the ox-GCE-[AuNPs-SiPy] platform, performed by applying successive potential scans between 0.2 to 1.6 V (around 22 cycles).Figure S3. SEQ Figure:_S3.1 \* ARABIC 2: Stability study of ox-GCE-[AuNPs-SiPy] platform analyzed in terms of (A) Ipc and (B) Epc in relation to the numbers of voltammetric cycles.Cyclic voltammograms of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] obtained in 0.15 mol L-1 PBS buffer (pH 7.4) in the absence of the redox marker [Fe(CN)6]3-/4-.Figure S3. SEQ Figure:_S3.1 \* ARABIC 3: Cyclic voltammograms obtained in 0.15 mol L-1 PBS buffer (pH 7.4) for the bare GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] (scan rate = 50.0 mVs?1).Electrochemical measurements (CV and EIS) for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] platforms (Figure S3.4 and Table S3.1) performed in 0.15 mol L-1 PBS buffer (pH 7.4) in the presence of 5.0 mmol L-1 Fe(CN)63-/4-.Figure S3. SEQ Figure:_S3.1 \* ARABIC 4: (A) Cyclic voltammograms (50.0 mV s-1) and (B) electrochemical impedance spectra (open circuit potential (OCP); frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy], in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6.Table S3. SEQ Table_S3.1 \* ARABIC 1: Values of Ipa, Ipc, ΔIp, Epa, Epc, ΔEp, Rs, Rct and Rct error obtained in the CV and EIS measurements for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6.Electrode(a)Ipa (?A)Ipc (?A)ΔIp (?A)Epa (mV)Epc (mV)ΔEp (mV)Rs (Ω)Rct (Ω)Error Rct(b) (%)1103.4-102.4102.90.20.20.298.550.21.8268.3-75.872.00.30.10.2104.5851.81.9385.5-99.392.40.30.20.2102.2502.31.7474.6-122.398.40.30.10.2101.3402.62.0 (a) 1: GCE; 2: ox-GCE; 3: ox-GCE-[SiPy]; 4: ox-GCE-[AuNPs-SiPy].(b) Rct errors correspond to the percent error that resulted from the fit of EIS data to the equivalent circuit.Electrochemical measurements for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] platforms (Figure S3.5 and Table S3.2) performed in the presence of 5.0 mmol L?1 Ru(NH3)2+/3+, as positive redox probe.Figure S3. SEQ Figure:_S3.1 \* ARABIC 5: Cyclic voltammograms of GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy] in 0.5 mol L?1 PBS buffer solution (pH 7.4) containing 5,0 mmol L?1 Ru(NH3)2+/3+.Table S3. SEQ Table_S3.1 \* ARABIC 2: Values of Ipa, Ipc, ΔIp, Epa, Epc e ΔEp obtained by CV for GCE, ox-GCE, ox-GCE-[SiPy] and ox-GCE-[AuNPs-SiPy], obtained in presence of 5.0 mmol L?1 Ru(NH3)2+/3+.Electrode(a)Ipa (?A)Ipc (?A)ΔIp (?A)Epa (mV)Epc (mV)ΔEp (mV)186.6-146.3116.6-0.1-0.2-0.2243.8-83.563.7-0.1-0.2-0.2351.6-104.478.0-0.1-0.2-0.2478.9-135.9107.4-0.1-0.2-0.2(a) 1: GCE; 2: ox-GCE; 3: ox-GCE-[SiPy]; 4: ox-GCE-[AuNPs-SiPy].S4Optimization steps of ZIKV DNA BiosensorThe amount of AuNPs-SiPy was optimized by using a univariate process, which showed an increase in ΔRct values until 5 ?L and then a sequential decrease with the increase in the amount of AuNPs-SiPy deposited on ox-GCE.Figure S4. SEQ Figure_S4.1 \* ARABIC 1: Effect of the amount of AuNPs-SiPy in the biosensor response.The multivariate optimization of the variables [ZIKV1] and timeinc involved in the preparation of the ZIKV DNA biosensor was carried out by using a 32 full factorial design (central point assayed in triplicate).Table S4. SEQ Table_S4.1 \* ARABIC 1: Results obtained in the 32 full factorial design for the optimization of the variables involved in the preparation of the ZIKV DNA biosensor.timeinc[ZIKV1]?Rct (%)--239.45+-213.73-+226.43++238.4900287.2300286.2400288.940-254.360+242.71-0252.51+0256.80Figure S4. SEQ Figure_S4.1 \* ARABIC 2: Pareto chart for the effects resultant of the variable optimization by 32 full factorial design (95% confidence level).The statistical validity of the obtained quadratic model was tested by applying analysis of variance (ANOVA) at 95% confidence level.Table S4. SEQ Table_S4.1 \* ARABIC 2: ANOVA results of the quadratic model for ZIKV DNA biosensor optimization.FactorSum of squareDegrees of freedomMean of squareFp[ZIKV1]1308.911308.9701.60.001timeinc2075.412075.41112.40.001[ZIKV1]*timeinc620.74155.283.20.012Lack of fit14.627.33.90.203Pure error3.721.9Total6331.610Maximum explainable variation: R2 = 0.9971; explained variation: Adj-R2 = 0.9927. The temperature of hybridization between the ZIKV1 and ZIKV2 strands was optimized by using a univariate process.Figure S4. SEQ Figure_S4.1 \* ARABIC 3: Effect of the temperature on the ZIKV2 hybridization on ox-GCE-[AuNPs-SiPy]/ZIKV1 biosensor.S5ZIKV DNA Biosensor characterizationTable S5. SEQ Table_S5.1 \* ARABIC 1: Values of Ipa, Ipc, ΔIp, ΔEp, Rs, Rct, ΔRct, Rct error, Cdl and W obtained by CV and EIS at each stage of ox-GCE-[AuNPs-SiPy]/ZIKV1 biossensor construction.Step(a)Ipa (?A)Ipc (?A)ΔIp (?A)ΔEp (mV)Rs (Ω)Rct (Ω)ΔRct (Ω)Error Rct(b) (%)Cdl (?F sn-1)W (?F sn-1)198.4-99.899.10.298.550.2-1.8211.71.7268.3-75.872.10.2104.5851.81596.81.940.21.2369.2-112.690.90.2101.3419.7-103.02.1104.01.3442.4-90.065.20.2105.91003.5139.21.638.71.0526.6-55.140.80.2120.443994.5298.12.028.00.8640.5-84.560.50.2108.91410.128.81.735.20.9 (a) 1: GCE; 2: ox-GCE; 3: ox-GCE-[AuNPs-SiPy]; 4: ox-GCE-[AuNPs-SiPy]/ZIKV1; 5: ox-GCE-[AuNPs-SiPy]/ZIKV1/ZIKV2; 6: ox-GCE-[AuNPs-SiPy]/ZIKV1/No-ZIKV2.(b) Rct errors correspond to the percent error that resulted from the fit of EIS data to the equivalent circuit.The immobilization of cystamine (C4H12N2S2) onto the ox-GCE-[AuNPs-SiPy] surface was carried out in order to confirm the formation of the Au-S covalent bond.Figure S5. SEQ Figure_S5.1 \* ARABIC 1: Electrochemical impedance spectra (OCP; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) of ox-GCE-[AuNPs-SiPy]/cystamine in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L-1 K4Fe(CN)6/K3Fe(CN)6 (cystamine concentration: 1 mmol L-1). S6Redox marker effect on ZIKV DNA biosensor In order to verify the interaction of the [Fe(CN)6]4-/3- redox marker on the ox-GCE-[AuNPs-SiPy] surface, EIS measurements were performed.Figure S6. SEQ Figure_S6.1 \* ARABIC 1: Electrochemical impedance spectra (OPC; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) obtained before and after the interaction between the ox-[AuNPs-SiPy] surface and the [Fe(CN)6]3-/4- redox marker (2 h and 2 h 50 min), in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6.S7AuNPs-SiPy influenceIn order to justify the use of the AuNPs-SiPy for the covalent binding (S-Au) of the thiolate ZIKV1 ssDNA probe EIS measurements were performed. Figure S7. SEQ Figure_S7.1 \* ARABIC 1: Electrochemical impedance spectra (OPC; frequency range: 10.0 kHz to 0.1 Hz; amplitude: 10 mV) obtained using three different configurations (A) ox-ECV/ZIKV1, (B) ox-ECV-[SiPy]/ZIKV1 e (C) ox-ECV-[AuNPs-SiPy] to hybridize the ZIKV2 ssDNA target in 0.15 mol L-1 PBS buffer solution (pH 7.4) containing 5.0 mmol L?1 K4Fe(CN)6/K3Fe(CN)6.S8Microscopy characterization of the biosensor AFM images were obtained for each step of biosensor construction.Figure S8. SEQ Figure_S7.1 \* ARABIC 1: AFM images of (A) ox-GCE, (B) ox-GCE-[AuNPs-SiPy], (C) ox-GCE-[AuNPs-SiPy]/ZIKV1, (D) ox-GCE-[AuNPs-SiPy]/ZIKV1/ZIKV2 and (E) ox-ECV-[AuNPs-SiPy]/ZIKV1/No-ZIKV2 (negative control).S9 Analytical curve Table S9. SEQ Table_S9.1 \* ARABIC 1: Concentration range of RNA copies present in 1 mL of body fluid in symptomatic patients.Body fluidsRNA copies mL-1Ref.Blood7.3 x 106 – 9.3 x 108ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"DOI":"10.1128/CMR.00072-15.Address","ISBN":"1080-6040","ISSN":"0028-4793","PMID":"24983096","abstract":"Zika virus is rapidly spreading throughout the Americas and the Caribbean. The association with microcephaly has led the WHO to declare a public health emergency. 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This review describes our current understanding of the characteristics of Zika virus infection.","author":[{"dropping-particle":"","family":"Musso","given":"D.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Gubler","given":"D.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"American Society for Microbiology","id":"ITEM-1","issue":"1","issued":{"date-parts":[["2016"]]},"page":"10-20","title":"Zika virus","type":"article-journal","volume":"11"},"uris":[""]}],"mendeley":{"formattedCitation":"(Musso and Gubler, 2016)","plainTextFormattedCitation":"(Musso and Gubler, 2016)","previouslyFormattedCitation":"(MUSSO; GUBLER, 2016)"},"properties":{"noteIndex":0},"schema":""}(Musso and Gubler, 2016)ADDIN CSL_CITATION {"citationItems":[{"id":"ITEM-1","itemData":{"author":[{"dropping-particle":"","family":"Besnard","given":"M.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Lastènere","given":"S.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Cao-Lormeau","given":"V. M.","non-dropping-particle":"","parse-names":false,"suffix":""},{"dropping-particle":"","family":"Musso","given":"D.","non-dropping-particle":"","parse-names":false,"suffix":""}],"container-title":"Eurosurveillance","id":"ITEM-1","issue":"13","issued":{"date-parts":[["2014"]]},"title":"Evidance of perinatal transmission of Zika virus, French Polynesia, December 2013 and February 2014","type":"article-journal","volume":"19"},"uris":[""]}],"mendeley":{"formattedCitation":"(Besnard et al., 2014)","plainTextFormattedCitation":"(Besnard et al., 2014)","previouslyFormattedCitation":"(BESNARD et al., 2014)"},"properties":{"noteIndex":0},"schema":""}(Besnard et al., 2014)*N = NewbornS10 Stability of ox-GCE-[AuNPs-SiPy]/ZIKV1The long-term stability of the ox-GCE-[AuNPs-SiPy]/ZIKV1 biosensor was evaluated by EIS towards ZIKV2 hybridization detection for 90 days. There was not a significant loss in the biosensor response even after this time interval. Figure S10. SEQ Figure_8.1 \* ARABIC 1: Long-term stability of the proposed biosensor.References for the Supplementary Data sectionADDIN Mendeley Bibliography CSL_BIBLIOGRAPHY Besnard, M., Lastènere, S., Cao-Lormeau, V.M., Musso, D., 2014. Eurosurveillance 19.Cala?a, G.N., Erdmann, C.A., Soares, A.L., Pess?a, C.A., Fujiwara, S.T., Garcia, J.R., Vidotti, M., Wohnrath, K., 2017. Electrochim. Acta 249, 104–112. , F.R., Fateley, W.G., Benteley, F.F., 1991. Characteristic raman frequencies of organic compounds. Wiley-Inter-science, New York.dos Santos, M., Wrobel, E.C., dos Santos, V., Quináia, S.P., Fujiwara, S.T., Garcia, J.R., Pess?a, C.A., Scheffer, E.W.O., Wohnrath, K., 2016. J. Electrochem. Soc. 163, B499–B506. Santos, V., De Jesus, C.G., Dos Santos, M., Canestraro, C.D., Zucolotto, V., Fujiwara, S.T., Garcia, J.R., Pessoa, C.A., Wohnrath, K., 2012. J. Nanoparticle Res. 14. , C., Cadar, D., Schlaphof, A., Neddersen, N., Günther, S., Schmidt-Chanasit, J., Tappe, D., 2016. 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