Three-dimensional CdS@Carbon Fiber Networks - ACS Publications

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Letter

Three-dimensional CdS@Carbon Fiber Networks: Innovative Synthesis and Application as a General Platform for Photoelectrochemical Bioanalysis Yuan-Cheng Zhu, Yi-Tong Xu, Yi Xue, Gao-Chao Fan, Panke Zhang, Wei-Wei Zhao, Jing-Juan Xu, and Hong-Yuan Chen Anal. Chem., Just Accepted Manuscript • Publication Date (Web): 29 Apr 2019 Downloaded from http://pubs.acs.org on April 29, 2019

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Analytical Chemistry

Three-dimensional CdS@Carbon Fiber Networks: Innovative Synthesis and Application as a General Platform for Photoelectrochemical Bioanalysis Yuan-Cheng Zhu,1 Yi-Tong Xu,1 Yi Xue,1 Gao-Chao Fan,2 Pan-Ke Zhang,1,* Wei-Wei Zhao1,* Jing-Juan Xu,1 Hong-Yuan Chen,1,* 1State

Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry and

Chemical Engineering, Nanjing University, Nanjing 210023, China 2Shandong

Key Laboratory of Biochemical Analysis, College of Chemistry and Molecular

Engineering, Qingdao University of Science and Technology, Qingdao 266042, China *To whom correspondence should be addressed. *E-mail: [email protected] *E-mail: [email protected] *E-mail: [email protected]

1 ACS Paragon Plus Environment

Analytical Chemistry 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

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ABSTRACT: This Letter reports a novel synthetic methodology for the fabrication of three-dimensional (3D) nanostructured CdS@carbon fiber (CF) networks and the validation

of

its

feasibility

for

application

as

a

general

platform

for

photoelectrochemical (PEC) bioanalysis. Specifically, 3D architectures are currently attracted increasing attention in various fields due to their intriguing properties, while CdS has been most widely utilized for PEC bioanalysis application due to its narrow band gap, proper conduction band and stable photocurrent generation. Using CdS as a representative material, this work realized the innovative synthesis of 3D CdS@CF networks via a simple solvothermal process. Exemplified by sandwich immunoassay of fatty-acid-binding protein (FABP), the as-fabricated 3D CdS@CF networks exhibited superior properties and the assay demonstrated good performance in terms of sensitivity and selectivity. This work features novel fabrication of 3D CdS@CF networks that can serve as a general platform for PEC bioanalysis. The methodology reported here is expected to inspire new interest for fabrication other 3D nanostructured Cd-chalcogenide (S, Se, Te)@ CF networks for wide applications in biomolecular detection and beyond. KEYWORDS: Photoelectrochemical, Bioanalysis, Three-dimensional, CdS, Carbon fiber, Immunoassay


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Recently, three-dimensional (3D) architectures are of considerable attention in various fields because their unique structures allow the design and implementation of sophisticated and versatile platforms with intriguing properties.1-5 For example, 3D catalysts have been intensively developed by incorporating active species into 3D scaffolds such as graphene4 or nickel foam,6 which resulted in a significant enhancement of their catalytic activity owing to the higher catalyst loading and better electrode contact.7-9 In the field of photoelectrochemical (PEC) bioanalysis,10-17 3D architectures also have unparalleled prospect due to their high specific surface areas for accommodating functional biomolecules whilst the numerous porosity guarantees the accessibility of the electrolyte to the electrode surface.18-20 Besides, the excellent mechanical strength and outstanding electronic conductivity further favor the charge transfer and diffusion kinetics for solution-solubilized species. Despite their great potential, 3D architectures are rarely studied in PEC bioanalysis.18 Among various semiconductors, CdS has been most widely utilized for PEC bioanalysis due to its narrow band gap, proper conduction band, as well as efficient and stable photocurrent generation.21-26 Herein, this Letter reports the innovative synthesis of 3D nanostructured CdS@carbon fiber (CF) networks and its application as a general platform for PEC immunoassay application, which to our knowledge has not been reported.15 RESULTS AND DISCUSSION Scheme 1. Schematic Illustration for the Synthesis of 3D Nanostructured CdS@CF Networks and Its Application for PEC Bioanalysis 3 ACS Paragon Plus Environment


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Experimentally, as shown in Scheme 1, a typical 3D CdS@CF network can be easily prepared by directing the CF paper to a solvothermal process, and the applicability of as-fabricated 3D CdS@CF networks was exemplified by a sandwich immunoassay thereon with the fatty-acid-binding protein (FABP) as a model target. In the assay, with the aid of biocatalytic precipitation (BCP) strategy,27,28 sandwich protein binding would surface confine the enzyme label of horseradish peroxidase (HRP) to efficiently initiate BCP onto the 3D CdS@CF networks. (See the Supporting Information for the experimental section.) As demonstrated below, the CdS formed on CFs exhibited highly porous net-like morphology that of special advantageous for the deposition of insulating BCP species, which could effectively impede the interfacial mass and electron transfer and thus render the BCP-dependent suppression of the photocurrent signal. In such a protocol, the photocurrent response


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was correlated to the HRP-controlled BCP, which in turn depended on the amount of target FABP. As compared to current state-of-the-art PEC bioanalysis, this work features the innovative synthesis and use of a 3D CdS@CF networks as a potential general PEC bioanalysis platform.

Figure 1. (a-b) SEM images of pristine CFs and as-fabricated CdS@CF networks. Insets: the corresponding magnified images. (c) HR-SEM image of CdS@CF network electrode. (d) TEM image of as-fabricated composite. Inset: HR-TEM of a single CdS NWs. (e) STEM image of CdS@CF and EDX elemental mapping images of C, Cd and S. (f) Operational stability test of the CFs (black) and composite (red). The PEC tests were performed in 0.01 M PBS (pH 7.4) solution containing 0.1 M AA with 0.0 V applied voltage and 410 nm excitation light.

The morphological change from the pristine CF paper to the 3D CdS@CF networks were tracked by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). As shown in Figure 1a and inset, the unprocessed one consists of randomly-overlapped CFs with very smooth surface. However, as shown in Figure 1b and inset, after the processing, CdS grew densely on the CFs with a net-like morphology. The high-resolution SEM image and the elemental mapping 5 ACS Paragon Plus Environment


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were shown in Figure 1c and Figure S1, respectively. Obviously, such a nanostructure with large surface area and porosity could offer an excellent adsorption microenvironment for the BCP in subsequent procedure. For better clarity, the sample was characterized by TEM as shown in Figure 1d and inset. As shown, the net-like CdS was consisted of crossing-linking CdS nanowires (NWs) that closely distributed on CFs with a nanoporous structure, and the single CdS NWs was of ca. 5 nm in diameter with a crystal lattice spacing of 0.336 nm that corresponding to the (111) facet of CdS.29,30 The existence of the porosity enables the composite to form a nanoporous 3D structure with abundant internal space and large surface area. Generally, for application in various PEC directions such as, such unique morphology can expose more active sites, accommodate more guest species, and also facilitate connection between internal active material and electrolyte. Figure 1e shows the scanning transmission electron microscopy (STEM) image and corresponding energy dispersive X-ray spectroscopy (EDX) elemental mapping, which proved the uniform distribution of Cd and S elements in the net-like CdS and the results agreed well with the surface chemical composition survey by X-ray photoelectron spectroscopy (XPS), as shown in Figure S2 and Figure S3. To study its PEC property, Figure 1f demonstrates the chronoamperometric i−t curves probed by photocurrent action spectra. As shown, the pristine CF paper had no response (black curve), whereas the as-fabricated 3D CdS@CF networks exhibited fast and strong photocurrent generation upon illumination (red curve), indicating not only the good PEC property of the CdS and also the excellent contact between the formed CdS and the CFs as the current 6 ACS Paragon Plus Environment

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collector. With repeated on/off illumination cycles over 300s, the current signal kept reproducible responses revealing the high mechanical and photophysical stability of the electrode. Incidentally, as shown in Figure S4, linear sweep voltammograms (LSVs) of the 3D CdS@CF photoelectrode were also collected in the dark and upon illumination with a scan rate of 10 mV s−1. The as-fabricated 3D CdS@CF networks were then applied for the quantitative detection of FABP, a kind of biomarker of acute myocardial infarction (AMI). FABP mainly expresses by myocytes, which possesses important significance in the onset of AMI, and the normal concentration of FABP in healthy human plasma or serum is below 5 ng ml-1.31 Upon intermittent light irradiation by chronoamperometric i−t technique, Figure 2a recorded the stepwise transient photocurrent responses during the immunoassay development corresponding to 100 ng mL−1 FABP. As shown, CdS@CF electrode exhibited obvious PEC response (curve i), while the immunoassay development resulted in gradual decrease of the signal (curves ii-v). Upon the introduction of BCP, the signal was further depressed obviously (curve vi). During this process, the interface properties of electrode were also characterized by electrochemical impedance spectroscopy (EIS). As depicted in Figure 2b, both bare CF and CdS@CF exhibited small semicircle in the EIS Nyquist plot. Subsequently, with the formation of protein sandwich, the diameter of the resistance-circle was increased, which revealed the increasing charge-transfer resistance (Rct) at the electrode/solution interface. Consistently, using Fe(CN)63−/4− as the electrochemical probe, the cyclic voltammetry (CV) was also conducted as presented in Figure 2c. As 7 ACS Paragon Plus Environment


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shown, it exhibited a pair of well-defined redox peaks with a small peak-to-peak separation (Δ Ep) at the CdS@CF electrode. Along with the immunocomplexing and introduction of BCP on the electrode, ΔEp increased and the redox peak current decreased, suggesting the diminished electron transfer rate that in accordance with the tendency of EIS. These experimental phenomena were due to that the nonconductive properties of the proteins and the insoluble precipitation layer could progressively obstruct the mass transport and electron transfer so that the hindrance and insulation effect elevated on the electrode surface. Because the extent of signal reduction depended upon the target concentration, a sensitive PEC FABP immunoassay can be achieved. Figure 2d shows the variation of photocurrent signal corresponding to variable FABP concentration. Figures 2e demonstrated that the photocurrent increment linearly increased with the target concentrations from 10 pg mL-1 to 10 ng mL-1 and 50 ng mL-1 to 1 μg mL-1, and the lowest detection limit was experimentally found as 10 pg mL-1, which was comparable to those obtained detection methods, as shown in Table S1. A relative standard deviation (RSD) of 5.7 % was obtained by testing five electrodes at the concentration of 100 ng mL-1, suggesting the good reproducibility of the system. To verify the selectivity, as shown in Figure 2f, cardiac troponin T (cTnT), p53, lipoprotein phospholipase a2 (LpPLA2), prostatic specific antigen (PSA), carcinoembryonic antigen (CEA), immunoglobulin G (IgG) and creatine kinase isoenzymes (CK-MB) were investigated as interference. The concentration of interfering agents were 10-fold excess in comparison with the target FABP and the photocurrent responses were very close to the blank test, demonstrating 8 ACS Paragon Plus Environment

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the favorable selectivity. These results proved the feasibility of the proposed PEC immunoassay and also confirmed the great potential of 3D CdS@CF networks-based PEC bioanalysis.

Figure 2. (a) Photocurrent responses of the CdS@CF electrode (curve i), CdS@CF/Ab1 (curve ii), CdS@CF/Ab1/BSA (curve iii), CdS@CF/Ab1/BSA/FABP (curve iv), CdS@CF/Ab1/BSA /FABP/Ab2 (curve v) and after BCP reaction (curve vi). (b) EIS and (c) CVs of stepwise modified electrodes in 5.0 mM Fe(CN)63−/4− containing 0.1 M KCl. (d) Plot of the photocurrent variation vs different FABP concentrations. (e) The corresponding derived calibration curve. (f) The selectivity of the immunoassay to FABP with 10 ng mL-1 by comparing to the interfering proteins at 100 ng mL−1 level: cTnT, p53, LpPLA2, PSA, CEA, IgG and CK-MB. ΔI is the photocurrent decrement corresponding to the variable FABP concentrations. The PEC tests were performed in 0.01 M PBS (pH 7.4) solution containing 0.1 M AA with 0.0 V applied voltage and 410 nm excitation light.

CONCLUSIONS In short, this work has developed an innovative method for the facile fabrication of 3D nanostructured CdS@CF networks, which was then characterized by various techniques including SEM, TEM, XPS and electrochemical characterizations. Especially,

the

transient

state

photocurrent

characterization

by

the



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chronoamperometric i−t tests demonstrated the favorable PEC performance of the 3D CdS@CF networks, indicating that it can be a competitive platform for the general development of PEC bioanalysis. Exemplified by FABP as a model target, such a potential was clearly demonstrated by a BCP-supported sandwich immunoassay event and the as-developed assay possessed good performance in terms of sensitivity and selectivity. This work not only featured the novel synthesis of 3D CdS@CF networks for general PEC bioanalysis application but also offered a new perspective for the preparation of other 3D semiconductor networks for innovative applications in this field. We further expect the implementation of these materials in the broad PEC field and beyond, e.g. photocatalytic H2 evolution, CO2 reduction, degradation of pollutants, and biohazard disinfection. ASSOCIATED CONTENT Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.analchem…. Experimental section, Elemental mapping of CdS@CF network electrode, XPS spectra of CFs before and after CdS deposition, High-resolution XPS spectra of Cd 3d and S 2p, LSVs of the CdS@CF network electrode in the dark and upon illumination, Comparison of Different Methods for FABP Determination (PDF) AUTHOR INFORMATION Corresponding Author *E-mail: [email protected] *E-mail: [email protected]


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*E-mail: [email protected] ORCID Wei-Wei Zhao: 0000-0002-8179-4775 Notes The authors declare no competing financial interest. ACKNOWLEDGMENT This work was supported by the Science and Technology Ministry of China (Grant No. 2016YFA0201200), National Natural Science Foundation of China (Grant nos. 21327902 and 21675080) and the Natural Science Foundation of Jiangsu Province (Grant BK20170073). REFERENCES (1) Chaudhari, N. K.; Jin, H.; Kim, B.; Lee, K. Nanostructured materials on 3D nickel foam as electrocatalysts for water splitting. Nanoscale 2017, 9, 12231–12247. (2) Ciornii, D.; Riedel, M.; Stieger, K. R.; Feifel, S. C.; Hejazi, M.; Lokstein, H.; Zouni, A.; Lisdat, F. Bioelectronic circuit on a 3D electrode architecture: Enzymatic catalysis interconnected with photosystem I. J. Am. Chem. Soc. 2017, 139, 16478–16481. (3) Hou, Y.; Qiu, M.; Nam, G.; Kim, M. G.; Zhang, T.; Liu, K.; Zhuang, X.; Cho, J.; Yuan, C.; Feng, X. Integrated hierarchical cobalt sulfide/nickel selenide hybrid nanosheets as an efficient three-dimensional electrode for electrochemical and photoelectrochemical water splitting. Nano Lett. 2017, 17, 4202–4209. (4) Peurifoy, S. R.; Castro, E.; Liu, F.; Zhu, X. Y.; Ng, F.; Jockusch, S.; Steigerwald, M. L.; Echegoyen, L.; Nuckolls, C.; Sisto, T. J. Three-dimensional graphene nanostructures. J. Am. Chem. Soc. 2018, 140, 9341–9345. (5) Zhu, C.; Li, H.; Fu, S.; Du, D.; Lin, Y. Highly efficient nonprecious metal catalysts towards oxygen reduction reaction based on three-dimensional porous carbon nanostructures. Chem. Soc. Rev. 2016, 45, 517–531. (6) Tang, C.; Cheng, N.; Pu, Z.; Xing, W.; Sun, X. NiSe nanowire film supported on nickel foam: An efficient and stable 3D bifunctional electrode for full water splitting. Angew. Chem. Int. Ed. 2015, 54, 9351–9355.



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