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Screening metal nanoparticles using boron-doped diamond microelectrodes

Ivandini Tribidasari A., Rangkuti Prasmita K., Einaga Yasuaki

2016年04月

Boron-doped diamond (BDD) microelectrodes were used to observe the correlation between electrocatalytic currents caused by individual Pt nanoparticle (Pt-np) collisions at the electrode. The BDD microelectrodes, ∼20 μm diameter and ∼2 μm particle size, were fabricated at the surface of tungsten wires. Pt-np with a size of 1 to 5 nm with agglomerations up to 20 nm was used for observation. The electrolytic currents were observed via catalytic reaction of 15 mM hydrazine in 50 mM phosphate buffer solution at Pt-np at 0.4 V when it collides with the surface of the microelectrodes. The low current noise and wider potential window in the measurements using BDD microelectrode produced a better results, which represents a better correlation to the TEM result of the Pt-np, compared to when gold microelectrodes was used.

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Zanamivir immobilized magnetic beads for voltammetric measurement of neuraminidase at gold-modified boron doped diamond electrode

Wahyuni Wulan Tri, Ivandini Tribidasari A., Saepudin Endang, Einaga Yasuaki

2016年04月

Biomolecule modified magnetic beads has been widely used in separation and sensing process. This study used streptavidin modified magnetic beads to immobilize biotin modified zanamivir. Biotin-streptavidin affinity facilitates immobilization of zanamivir on magnetic beads. Then interaction of zanamivir and neuraminidase was adopted as basic for enzyme detection. Detection of neuraminidase was performed at gold modified BDD using cyclic voltammetry technique. The measurement was carried out based on alteration of electrochemical signals of working electrode as neuraminidase response. The result showed that zanamivir was successfully immobilized on magnetic beads. The optimum amount of magnetic beads for zanamivir immobilization was 120 ug. Linear responses of neuraminidase were detected in concentration range of 0-15 mU. Detection limit (LOD) of measurement was 2.32 mU (R2 = 0.959) with precision as % RSD of 1.41%. Measurement of neuraminidase on magnetic beads could be also performed in the presence of mucin matrix. The linearity range was 0-8 mU with LOD of 0.64 mU (R2 = 0.950) and % RSD of 7.25%.

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Electroreduction of CO₂ using copper-deposited on boron-doped diamond (BDD)

Panglipur Hanum Sekar, Ivandini Tribidasari A., Wibowo Rahmat, Einaga Yasuaki

2016年04月

Electroreduction of CO₂ was studied at copper-modified boron-doped diamond (Cu-BDD) electrodes as the working electrode. The Cu-BDD electrodes were prepared by electrochemical reduction with various concentrations of CuSO₄ solutions. FE-SEM was utilized to characterize the electrodes. At Cu-BDD electrodes, a reduction peak at around-1.2 V (vs Ag/AgCl) attributtable to CO₂ reductions could be observed by cyclic voltammetry technique of CO₂ bubbled in water containing 0.1M NaCl. Accordingly, electroreduction of CO₂ was conducted at-1.2 V (vs Ag/AgCl) using amperometry technique. The chemical products of the electroreduction analyzed by using HPLC showed the formation of formaldehyde, formic acid, and acetic acid at Cu-BDD electrodes.

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Dose-escalation study for the targeting of CD44v⁺ cancer stem cells by sulfasalazine in patients with advanced gastric cancer (EPOC1205)

Shitara Kohei, Doi Toshihiko, Nagano Osamu, Imamura Chiyo K., Ozeki Takeshi, Ishii Yuya, Tsuchihashi Kenji, Takahashi Shunji, Nakajima Takako E., Hironaka Shuichi, Fukutani Miki, Hasegawa Hiromi, Nomura Shogo, Sato Akihiro, Einaga Yasuaki, Kuwata Takeshi, Saya Hideyuki, Ohtsu Atsushi

Gastric Cancer 1 - 9 2016年04月

ISSN 1436-3291

Background: Cancer stem cells (CSCs) have enhanced mechanisms of protection from oxidative stress. A variant form of CD44 (CD44v), a major CSC marker, was shown to interact with xCT, a subunit of cystine–glutamate transporter, which maintains high levels of intracellular reduced glutathione (GSH) which defend the cell against oxidative stress. Sulfasalazine (SSZ) is an inhibitor of xCT and was shown to suppress the survival of CD44v-positive stem-like cancer cells both in vitro and in vivo. To find the dose of SSZ which can safely reduce the population of CD44v-positive cells in tumors, a dose-escalation study in patients with advanced gastric cancer was conducted. Methods: SSZ was given four times daily by oral administration with 2 weeks as one cycle. Tumor biopsies were obtained before and after 14 days of administration of SSZ to evaluate expression of CD44v and the intratumoral level of GSH. Results: Eleven patients were enrolled and received a dosage from 8 to 12 g/day. Safety was confirmed up to a dosage of 12 g/day, which was considered the maximum tolerated dose. Among the eight patients with CD44v-positive cells in their pretreatment biopsy samples, the CD44v-positive cancer cell population appeared to be reduced in the posttreatment biopsy tissues of four patients. Intratumoral GSH levels were also decreased in two patients, suggesting biological effectiveness of SSZ at 8 g/day or greater. Conclusions: This is the first study of SSZ as an xCT inhibitor for targeting CSCs. Reduction of the levels of CD44v-positive cells and GSH was observed in some patients, consistent with the mode of action of SSZ in CSCs.

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Development of neuraminidase detection using gold nanoparticles boron-doped diamond electrodes

Wahyuni Wulan T., Ivandini Tribidasari A., Saepudin Endang, Einaga Yasuaki

Analytical Biochemistry 497 68 - 75 2016年03月

ISSN 0003-2697

Gold nanoparticles-modified boron-doped diamond (AuNPs-BDD) electrodes, which were prepared with a self-assembly deposition of AuNPs at amine-terminated boron-doped diamond, were examined for voltammetric detection of neuraminidase (NA). The detection method was performed based on the difference of electrochemical responses of zanamivir at gold surface before and after the reaction with NA in phosphate buffer solution (PBS, pH 5.5). A linear calibration curve for zanamivir in 0.1 M PBS in the absence of NA was achieved in the concentration range of 1 × 10^-6 to 1 × 10^-5 M (R² = 0.99) with an estimated limit of detection (LOD) of 2.29 × 10^-6 M. Furthermore, using its reaction with 1.00 × 10^-5 M zanamivir, a linear calibration curve of NA can be obtained in the concentration range of 0-12 mU (R² = 0.99) with an estimated LOD of 0.12 mU. High reproducibility was shown with a relative standard deviation (RSD) of 1.14% (n = 30). These performances could be maintained when the detection was performed in mucin matrix. Comparison performed using gold-modified BDD (Au-BDD) electrodes suggested that the good performance of the detection method is due to the stability of the gold particles position at the BDD surface.

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A New Family of Anionic Fe^III Spin Crossover Complexes Featuring a Weak-Field N₂O₄ Coordination Octahedron

Takahashi Kazuyuki, Kawamukai Kiko, Okai Mitsunobu, Mochida Tomoyuki, Sakurai Takahiro, Ohta Hitoshi, Yamamoto Takashi, Einaga Yasuaki, Shiota Yoshihito, Yoshizawa Kazunari

Chemistry - A European Journal 22 （ 4 ） 1253 - 1257 2016年01月

ISSN 0947-6539

Unprecedented anionic Fe^III spin crossover (SCO) complexes involving a weak-field O,N,O-tridentate ligand were discovered. The SCO transition was evidenced by the temperature variations in magnetic susceptibility, Mössbauer spectrum, and coordination structure. The DFT calculations suggested that larger coefficients on the azo group in the HOMO-1 of a ligand might contribute to the enhancement of a ligand-field splitting energy. The present anionic SCO complex also exhibited the light- induced excited-spin-state trapping effect. Photoinduced spin transition: Unprecedented anionic spin crossover (SCO) complexes involving a weak-field Fe^IIIN₂O₄ coordination sphere were discovered. The tetramethylammonium salt of the depicted SCO anion exhibited the light-induced excited-spin-state trapping effect, which is quite rare in Fe^III SCO complexes (see scheme).

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Microfluidic platform for environmental contaminants sensing and degradation based on boron-doped diamond electrodes

Medina-Sánchez Mariana, Mayorga-Martinez Carmen C., Watanabe Takeshi, Ivandini Tribidasari A., Honda Yuki, Pino Flavio, Nakata Azuya, Fujishima Akira, Einaga Yasuaki, Merkoçi Arben

Biosensors and Bioelectronics 75 365 - 374 2016年01月

ISSN 0956-5663

We have developed a lab-on-a-chip (LOC) platform for electrochemical detection and degradation of the pesticide atrazine (Atz). It is based on boron-doped diamond (BDD) electrodes and a competitive magneto-enzyme immunoassay (EIA) that enables high sensitivity. To detect the enzymatic reaction, we employed a BDD electrode modified with platinum nanoparticles (PtNPs), as a highly conductive catalytic transducer. Chronoamperometry revealed a limit of detection (LOD) of 3.5pM for atrazine, which, to the best of our knowledge, is one of the lowest value published to date. Finally, we degraded Atz in the same platform, using a bare BDD electrode that features remarkable corrosion stability, a wide potential window, and much higher O<inf>2</inf> overvoltage as compared to conventional electrodes. These characteristics enable the electrode to produce a greater amount of HO• on the anode surface than do conventional electrodes and consequently, to destroy the pollutant more rapidly. Our new LOC platform might prove interesting as a smart system for detection and remediation of diverse pesticides and other contaminants.

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Surface Termination Effect of Boron-Doped Diamond on the Electrochemical Oxidation of Adenosine Phosphate

Asai Kai, Ivandini Tribidasari A., Falah Muhammad M., Einaga Yasuaki

Electroanalysis 28 （ 1 ） 177 - 182 2016年01月

ISSN 1040-0397

Electrochemical oxidation of adenosine phosphates, including adenosine 5'-monophosphate (AMP), adenosine 5'-diphosphate (ADP), and adenosine 5'-triphosphate (ATP), have been studied using boron-doped diamond (BDD) electrodes. Cyclic voltammograms in phosphate buffer solution pH7.4 showed a typical oxidation peak at the potential of around +1.3V (vs. Ag/AgCl) attributable to the oxidation of adenine base moiety. This peak appears at both cathodically and anodically treated BDD. However, investigation at low pH showed, whereas the oxidation peak could be well observed for the oxidation of each AMP, ADP, and ATP at cathodically treated BDD, it was only found for the oxidation of AMP at anodically-treted BDD electrodes. Linear calibration curve can be achieved in the concentration range of 20 to 200μM with an average detection limit of 2μM (S/N=3). Furthermore, cathodic treatment has demonstrated its ability to maintain the electrode surface from biofouling, resulting in the excellent stability of current responses.

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Development of electrochemical oxygen demand measurement cells using a diamond electrode

Kondo Takeshi, Hoshin Masaki, Watanabe Takeshi, Aikawa Tatsuo, Yuasa Makoto, Einaga Yasuaki

Analytical Sciences 32 （ 12 ） 1381 - 1384 2016年

ISSN 0910-6340

Electrolytic cells for electrochemical oxygen demand (ECOD) measurements based on total electrolytic decomposition at a boron-doped diamond (BDD) electrode were developed for rapid measurement of organic pollutants at low concentrations. Using improved electrolytic cells designed for efficient mass transfer, the ECOD for 10 μM potassium hydrogen phthalate (theoretical ECOD: 2.3 mg-O₂ L^-1) was determined in a relatively short electrolysis time. Thus, ECOD measurements using these cells would be useful for estimating organic water pollution in industrial waste and lake water.

Co-Fe Prussian Blue analogue intercalated into diamagnetic Mg-Al layered double hydroxides

Zhang Cuijuan, Yamamoto Takashi, Einaga Yasuaki

Nanomaterials and Nanotechnology 6 （ 1 ） 2016年

A heterostructure of diamagnetic magnesium-aluminium layered double hydroxides (Mg-Al LDHs) and photomagnetic cobalt-iron Prussian Blue analogue (Co-Fe PBA) was designed, synthesized and then designated as LDH-PB. The cyanide-bridged Co-Fe PBA was two-dimensionally intercalated into the Mg-Al LDH template by the stepwise anion exchange method. LDH-PB showed ferrimagnetic properties with in-plane antiferromagnetic exchange interactions, as well as small photo-induced magnetization by visible light illumination due to the low dimensional structures and the characteristic photo-induced electronic states of the mixed valence of Fe^III(low spin, S = 1/2)-CN-Co^II(high spin, S = 3/2)-NC-Fe^II (low spin, S = 0).

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Preparation of dihydroquinazoline carbohydrazone Fe(II) complexes for spin crossover

Shen Fu Xing, Huang Wei, Yamamoto Takashi, Einaga Yasuaki, Wu Dayu

New Journal of Chemistry 40 （ 5 ） 4534 - 4542 2016年

ISSN 1144-0546

Dihydroquinazoline Fe^II complexes, namely [Fe(pq-R)₂](X)₂·xCH₃OH·yCH₃CN·zH₂O (R = 2-py: X = ClO₄ ^-, x = 1, y = 0, z = 2 (1), BF₄ ^-, x = 0, y = 2, z = 1.75 (2), CF₃SO₃ ^-, x = 1, y = 1, z = 0 (3); and X = ClO₄ ^-: R = 2-OCH₃, x = 0, y = 0, z = 1 (4), R = 3-OCH₃, x = 0, y = 0, z = 1 (5)), were prepared and the effects of the solvent, counteranion and ligand substituent on spin crossover properties were discussed. Comparison of X-ray diffraction data for these complexes revealed the sole presence of high-spin Fe^II at 298 K and the bond distances around the Fe^II center at low temperature fall much closer to those at high temperature, which is consistent with variable-temperature dc magnetic susceptibility data. However, the loss of solvent induced a significant change in the spin state of complexes 1 and 2. Moreover, fits to magnetic data of the desolvated samples provide crossover temperatures of T_1/2 = 182.9(6), 157.0(8) and 138.3(5) K for 1-des (ClO₄ ^-), 2-des (BF₄ ^-) and 3-des (CF₃SO₃ ^-), respectively, indicative of the anion-dependent transition temperature. The cooperativity operating in the complexes is thought to be mainly from the intermolecular π⋯π interactions between dihydroquinazoline rings on the neighboring molecules. The ligand substituent effect was also investigated on Fe^II SCO properties. This work revealed the spin crossover properties of new types of dihydroquinazoline Fe(ii) complexes, including the transition temperature, the degree of completion and the cooperative nature of the transition, which can be optimally designed when developing new spin-crossover materials.

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Recovery of copper from dilute cupric sulfate solution by electrodeposition method using boron-doped diamond electrodes

Natsui Keisuke, Yamaguchi Chizu, Einaga Yasuaki

Physica Status Solidi (A) Applications and Materials Science 2016年

ISSN 1862-6300

The recovery of copper from wastewater is a key issue for environmental and economic aspects. The wastewater treatment containing copper ions has been carried out by various techniques. Among them, the electrodeposition is the "clean" method that is able to achieve the recovery of copper without requiring addition of chemicals and generating sludge or secondary wastes. However, the current efficiency would tend to decrease especially in a dilute solution, because hydrogen evolution and oxygen reduction reaction would occur as competition reaction. In this article, we study on the recovery of copper from dilute cupric sulfate solution as a model wastewater by an electrodeposition method using boron-doped diamond electrodes which have relatively higher hydrogen overpotential. Two types of boron-doped diamond electrodes were prepared with different boron doping level. The boron-doped diamond electrodes could achieve the recovery of copper with higher current efficiency because of inhibiting hydrogen evolution reaction, compared with glassy carbon electrode.

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Charge-Transfer Phase Transition of a Cyanide-Bridged Fe^II/Fe^III Coordination Polymer

Zhang Kuirun, Kang Soonchul, Yao Zi shuo, Nakamura Kazusa, Yamamoto Takashi, Einaga Yasuaki, Azuma Nobuaki, Miyazaki Yuji, Nakano Motohiro, Kanegawa Shinji, Sato Osamu

Angewandte Chemie - International Edition 2016年

ISSN 1433-7851

Heterometallic Prussian blue analogues are known to exhibit thermally induced charge transfer, resulting in switching of optical and magnetic properties. However, charge-transfer phase transitions have not been reported for the simplest FeFe cyanide-bridged systems. A mixed-valence Fe^II/Fe^III cyanide-bridged coordination polymer, ([Fe(Tp)(CN)₃]₂Fe(bpe)5H₂O)_n, which demonstrates a thermally induced charge-transfer phase transition, is described. As a result of the charge transfer during this phase transition, the high-spin state of the whole system does not change to a low-spin state. This result is in contrast to FeCo cyanide-bridged systems that exhibit charge-transfer-induced spin transitions.

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Enhancement of the coercivity in Co-Ni layered double hydroxides by increasing basal spacing

Zhang Cuijuan, Tsuboi Tomoya, Namba Hiroaki, Einaga Yasuaki, Yamamoto Takashi

Dalton Transactions 45 （ 34 ） 13324 - 13331 2016年

ISSN 1477-9226

The magnetic properties of layered double hydroxides (LDH) containing transition metal ions can still develop, compared with layered metal hydroxide salts which exhibit structure-dependent magnetism. In this article, we report the preparation of a hybrid magnet composed of Co-Ni LDH and n-alkylsulfonate anions (Co-Ni-CnSO₃ LDH). As Co-Ni LDH is anion-exchangeable, we can systematically control the interlayer spacing by intercalating n-alkylsulfonates with different carbon numbers. The magnetic properties were examined with temperature- and field-dependent magnetization measurements. As a result, we have revealed that the coercive field depends on the basal spacing. It is suggested that increasing the basal spacing varies the competition between the in-plane superexchange interactions and long-range out-of-plane dipolar interactions. Moreover, a jump in the coercive field at around 20 Å of the basal spacing is assumed to be the modification of the magnetic ordering in Co-Ni-CnSO₃ LDH.

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Selective production of methanol by the electrochemical reduction of CO₂ on boron-doped diamond electrodes in aqueous ammonia solution

Jiwanti Prastika K., Natsui Keisuke, Nakata Kazuya, Einaga Yasuaki

RSC Advances 6 （ 104 ） 102214 - 102217 2016年

ISSN 2046-2069

The electrochemical reduction of CO₂ was investigated in an aqueous ammonia solution using boron-doped diamond electrodes. Methanol was mainly produced by reduction at a potential of -1.3 V (vs. Ag/AgCl) with a faradaic efficiency as high as 24.3%. Also, even in an aqueous ammonium bicarbonate solution (pH 7.9) without CO₂ bubbling, methanol was produced, while no methanol production was observed at higher (10.6) and lower pH (3.38). These observations suggest that the selectivity for methanol production in aqueous ammonia solutions is due to the electrochemical reduction of bicarbonate ions which are formed by the reaction between ammonia and CO₂. Moreover, we present the important role of ammonia as an electrolyte for the selective production of methanol by electrochemical reduction of CO₂.

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Fabrication of a Microfluidic Device with Boron-doped Diamond Electrodes for Electrochemical Analysis

Watanabe Takeshi, Shibano Shuhei, Maeda Hideto, Sugitani Ai, Katayama Michinobu, Matsumoto Yoshinori, Einaga Yasuaki

Electrochimica Acta 2015年09月

ISSN 0013-4686

A prototype microfluidic device using boron-doped diamond (BDD) electrodes patterned on an alumina chip was designed and fabricated. Electrochemical microfluidic devices have advantages in that the amount of sample required is small, the measurement throughput is high, different functions can be integrated on a single device, and they are highly durable. In using the device for the flow injection analysis of oxalic acid, the application of a brief conditioning step ensured that the reproducibility of the current signal was excellent.Furthermore, the fabricated system also performed as a prototype of "elimination-detection flow system", in which interfering species are eliminated using "elimination electrodes" prior to the species reaching the "detection electrode". The fabricated device reduced the current due to interfering species by 78%. Designs of devices to improve this efficiency are also discussed.

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Novel Fe(II) spin crossover complexes involving a chalcogen-bond and π-stacking interactions with a paramagnetic and nonmagnetic M(dmit)<inf>2</inf> anion (M = Ni, Au; Dmit = 4,5-dithiolato-1,3-dithiole-2-thione)

Okai Mitsunobu, Takahashi Kazuyuki, Sakurai Takahiro, Ohta Hitoshi, Yamamoto Takashi, Einaga Yasuaki

Journal of Materials Chemistry C 3 （ 30 ） 7858 - 7864 2015年08月

ISSN 2050-7534

To introduce both an inter-sulphur atom and π-stacking interaction between a spin crossover (SCO) cation and paramagnetic anion, we designed and synthesised two novel Fe(ii) SCO compounds involving a terpyridine-type thiazole containing ligand with the paramagnetic Ni(dmit)<inf>2</inf> and nonmagnetic Au(dmit)<inf>2</inf> anion (dmit = 4,5-dithiolato-1,3-dithiole-2-thione). The temperature variations of magnetic susceptibility and Mössbauer spectroscopy revealed that both complexes exhibited an almost complete SCO conversion, and moreover, the Ni(dmit)<inf>2</inf> anion was in a paramagnetic state down to 2 K. The crystal structures for the Ni(dmit)<inf>2</inf> complex at 213 and 400 K indicated that the chalcogen-bond and π-stacking interaction would be enhanced by the electrostatic interaction between the cation and anion, preventing the π-radicals from dimerising. The light-induced excited spin state trapping effect was observed at 5 K.

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Electrochemical behavior of zanamivir at gold-modified boron-doped diamond electrodes for an application in neuraminidase sensing

Wahyuni Wulan Tri, Ivandini Tribidasari A., Jiwanti Prastika K., Saepudin Endang, Gunlazuardi Jarnuzi, Einaga Yasuaki

Electrochemistry 83 （ 5 ） 357 - 362 2015年05月

ISSN 1344-3542

This study emphasizes the electrochemical detection of Neuraminidase (NA) based on NA inhibition by Zanamivir. The detection method was developed based on the difference of electrochemical responses of Zanamivir in the presence and the absence of NA in phosphate buffer solution (pH 5.5). Gold and gold-modified boron-doped diamond was used as the working electrode and the measurement was conducted using cyclic voltammetry method. A linear calibration curve of Zanamivir was observed in the concentration range of 5 × 10^-6-1 × 10^-4 mol/L (R² = 0.991), with the estimated limit of detection (LOD) of 1.49 × 10^-6 mol/L. The presence of NA increases the peak current of gold oxidation and reduction with linear calibration curves were monitored in the concentration range of 0-15mU (R² = 0.996). An estimated LOD of 0.25mU NA and an excellent reproducibility of the detection with an RSD of 1.18% can be achieved. Application of a real sample was successfully demonstrated for NA detection in the presence of mucin, suggested that the method is promising for pharmaceutical or medical application.

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Crystal structure of 5,5′-dibromo-3,3′-di-tert-butyl-6,6′-dimethylbiphenyl-2,2′-diol

Obata Rika, Ohba Shigeru, Einaga Yasuaki, Nishiyama Shigeru, Stoeckli-Evans H.

Acta Crystallographica Section E: Structure Reports Online 71 （ 5 ） o278 - o279 2015年05月

ISSN 1600-5368

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Anodic stripping voltammetry of gold nanoparticles at boron-doped diamond electrodes and its application in immunochromatographic strip tests

Ivandini Tribidasari A., Wicaksono Wiyogo P., Saepudin Endang, Rismetov Bakhadir, Einaga Yasuaki

Talanta 134 136 - 143 2015年03月

ISSN 0039-9140

Anodic stripping voltammetry (ASV) of colloidal gold-nanoparticles (AuNPs) was investigated at boron-doped diamond (BDD) electrodes in 50 mM HClO₄. A deposition time of 300 s at-0.2 V (vs. Ag/AgCl) was fixed as the condition for the ASV. The voltammograms showed oxidation peaks that could be attributed to the oxidation of gold. These oxidation peaks were then investigated for potential application in immunochromatographic strip tests for the selective and quantitative detection of melamine, in which AuNPs were used as the label for the antibody of melamine. Linear regression of the oxidation peak currents appeared in the concentration range from 0.05-0.6 μg/mL melamine standard, with an estimated LOD of 0.069 μg/mL and an average relative standard deviation of 8.0%. This indicated that the method could be considered as an alternative method for selective and quantitative immunochromatographic applications. The validity was examined by the measurements of melamine injected into milk samples, which showed good recovery percentages during the measurements.

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