Highly accurate detection of poisonous arsenic and mercury ions in human blood serum samples based on AgTiO3/PVA/BN nanocomposite immobilized glassy carbon electrode

Abstract

Silver titanate (AgTiO3) blend with polyvinyl acrylate (PVA) decorated boron nitride (BN) nanocomposite immobilized glassy carbon electrode (GCE) is fabricated for an accurate detection of poisonous arsenic as well as mercury ions in blood serum samples by amperometric technique. The as-synthesized AgTiO3/PVA/BN nanocomposite material is well characterized by spectral, analytical, and electrochemical studies. The developed electrochemical sensor provided enhanced electrochemical sensing properties owing to its excellent surface area, lower electron transfer resistance, and catalytic property as compared to reported electrodes. The developed AgTiO3/PVA/BN immobilized GCE electrochemical sensor exhibited a highly selective detection of AsIII and HgII ions at pH-7.4. The developed sensor showed a wide linear range of response (1 µM -100 µM) and the limit of detections (LOD) are found to be 0.033 µM and 0.022 µM for AsIII and HgII ions respectively. The developed AgTiO3/PVA/BN immobilized GCE sensor exhibited excellent stability, sensitivity, selectivity, and reproducibility. It was utilized to successfully detect real-world human blood serum samples for AsIII and HgII ions.

Specification

Description:FIELD OF INVENTION
[001] The field of invention in patent applications refers to sensing biotechnology. In this, a developed AgTiO3/PVA/BN immobilized GCE sensor is utilized to detect AsIII and HgII ions in human blood serum samples by amperometric technique.
BACKGROUND AND PRIOR ART
[002] The accumulation of arsenic and mercury for a prolonged period in the human body will damage our kidneys, liver, and central nervous system and create cancer. From a clinical point of view detection of the poisonous metal ions receives much attention nowadays. Various methods of detection of poisonous metal ions such as flame atomic absorption spectroscopy (FASS), inductively coupled plasma/mass spectroscopy (ICP-MS), graphite furnace atomic absorption spectroscopy (GFAAS), inductively coupled plasma/atomic emission spectroscopy (ICP-AES), hybrid generation atomic absorption spectroscopy (HG-AAS), Plasmon resonance sensor (PRS), atomic fluorescence spectrometry (AFS) exist however, these are highly sophisticated and highly cost instrumentation techniques. Electrochemical sensing techniques are emerging and highly reliable for the accurate detection of analyte samples within a second. To date, Au (111)-like polycrystalline gold electrode, GCE/AuNP Bentonite clay, AuNPs/CeO2/ZrO2/GCE, Fe3O4-RTIL/SPCE, Au NPs/GCE, MWCNT/ArO/GCE, SrTiO3/β-CD immobilized GCE, Pt nanoparticles deposited on Si modified electrode, etc were employed for detection of poisonous metal ions using different electrochemical techniques. But this is the first work we have used a developed AgTiO3/PVA/BN immobilized GCE sensor for highly sensitive (0.0024 µM & 0.0032 µM) detection of both AsIII and HgII ions in human blood serum samples by amperometric technique at pH-7.4. The evaluated values of detection limit, wide linear range of response, and sensitivity are found to be better as compared to the reported electrodes for AsIII and HgII ions.
SUMMARY OF THE INVENTION
[003] The AgTiO3/PVA/BN nanocomposite material is synthesized using the sonochemical method and analyzed by UV-vis, FT-IR, SEM, EDX, HR-TEM and SEAD, CV, DPV, EIS, and amperometric techniques. The developed AgTiO3/PVA/BN immobilized GCE sensor is applied for the accurate detection of AsIII and HgII ions in blood serum samples and it is monitored by electrochemical techniques. In this work, the LOD, sensitivity, and linear range of response are achieved to be 0.033 µM & 0.022 µM, 0.0024 µAµM/cm2 & 0.0032 µAµM/cm2, and 1 µM -100 µM for the detection of AsIII and HgII ions at pH-7.4 respectively. The AgTiO3/PVA/BN immobilized GCE sensor paves the way for the detection of heavy metal ions not only in blood serum samples but also in water samples, and urine samples hence, it may be used for clinical, forensic, and diagnostic applications in future under optimized environment conditions.
BRIEF DESCRIPTIONS OF DRAWINGS:
[004] Fig.1: AgTiO3 nanomaterial is synthesized in the first step by hydrothermal method, 10 mg/mL AgTiO3 is added in 10 mg/mL of boron nitride (BN) dropwise and dispersed in 50 mL of deionized water in a 100 mL beaker in the second step under ultrasonication for 30 min at room temperature. In the third step, 5mg/mL of polyvinyl acrylate (PVA) is added and ultrasonicated for 15 min. The resultant product is filtered using Whatman filter paper, purified with anhydrous ethanol and deionized water several times, and dried at 80 °C for 2 h in a hot air oven. The final nanocomposite is mixed with ethanol and then immobilized on the surface of the glassy carbon electrode (GCE) by drop cost method dried at room temperature and used as a working electrode for the electrochemical detection of poisonous metal ions in this study.
[005] Fig.2. Amperometric selectivity response of 1 µM of a). AsIII and b). HgII ions at AgTiO3/PVA/BN immobilized GCE with 100-fold excess concentrations of hazardous interferents such as c). CrIII, d) PbII, (e) CdII and (f) CuII in 0.01 M phosphate buffer containing human blood serum samples at pH -7.4.
DETAILED DESCRIPTION OF THE INVENTION
[006] The amperometric technique is one of the advanced techniques in electrochemical sensing. The amperometric i-t curve method for the detection of poisonous metal ions such as AsIII and HgII ions are injected with regular 30 sec time intervals using a conventional three-electrode system ie. AgTiO3/PVA/BN immobilized GCE as a working electrode, Ag/AgCl in 0.1 M KCl as a reference electrode, and platinum wire used as a counter electrode in 0.01 M phosphate buffer (pH-7.4) at an applied potential of -0.18 V. A wide linear range of response is observed while increasing the concentration of AsIII and HgII ions in human blood serum samples from 1 µM to 100 µM with correlation coefficient (R2) are estimated to be 0.9982 & 0.9958 and the values of limit of detection are achieved to be 0.033 µM & 0.022 µM respectively. The sensitivity values are estimated to be 0.0024 µAµM/cm2 & 0.0032 µAµM/cm2. The limit of detection values is calculated using the LOD = 3.3S/b formula. The selectivity of the poisonous metal ions such as AsIII, and HgII ions are also analyzed even in the presence of 100-fold excess concentrations of various hazardous interferents in human blood serum samples as shown in Fig.2. , C , Claims:This work claims the as-synthesized electrode material, developed electrode and its applications for accurate detection of poisonous metal ions in common and arsenic and mercury in particular. The applications of amperometric detection of arsenic and mercury in human blood serum samples and their selectivity are also claims as a novel aspect in this patent.

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