Non-enzymatic Electrochemical Glucose Research Articles

Study on the performance of MoS2/Au composites for non-enzymatic electrochemical glucose detection

Abstract Glucose concentration is considered an indicator for the diagnosis of diabetes, highlighting the importance of accurate glucose detection. Non-enzymatic electrochemical sensors have been extensively studied for glucose detection applications, with nanocomposites composed of molybdenum disulfide (MoS2) and gold nanoparticles (Au NPs) demonstrating high catalytic activity. In this study, a nanocomposite material composed of MoS2 and Au NPs (MoS2/Au) was synthesized and employed to construct a non-enzymatic electrochemical glucose biosensor. The detection limit of this sensor was explored, reaching as low as 1 mM. Additionally, compared to MoS2, the MoS2/Au nanocomposite exhibited a higher linear correlation coefficient and sensitivity, with a linear range of 1-25 mM and a sensitivity of 417.556 μA mM-1 cm-2. The sensor demonstrated excellent performance within the range of human blood glucose concentrations, showing potential for real-time monitoring and precise measurement of glucose levels. Furthermore, it exhibited good stability and reproducibility. These findings indicate the potential applications of MoS2/Au in biosensors and immunoassays.

One‐Pot Carbothermal Reduction Preparation of Cu‐BTC@Cu/C Heterostructure for Enhanced Nonenzymatic Electrochemical Glucose Sensing

AbstractA heterostructure based on MOFs with a small lattice mismatch is ideal for improving glucose‘s electrochemical sensing performance. Herein, a novel one‐pot carbothermal reduction technique to prepare Cu‐BTC@Cu/C heterostructure with intimate interfacial contact and high yield was developed, by in situ integrating Cu‐BTC (Cu3(BTC)2 ⋅ 3H2O) and its derived Cu/C nanocomposites. Structure characterizations demonstrated that Cu‐BTC@Cu/C heterostructure shows a synergistic effect in the combination of these two components, with more electrochemical active sites and lower resistance. Compared with each individual component, Cu‐BTC@Cu/C heterostructure exhibits better glucose electrooxidation performance. Under optimal condition, an extremely sensitive nonenzymatic glucose sensor with a low detection limit of 6.78 μM, sensitivity of 911.03 μA mM−1 cm−2, linear range of 0.001–2.0 mM, and anti‐interference performance is presented. Meanwhile, the newly constructed sensor was effectively employed for detecting glucose in honey sample with perfect recoveries, showing its great potential toward glucose monitoring in real sample. In addition, it has been demonstrated Cu(II) can be induced into Cu(I) by glucose in solution, while Cu(I) could be electrochemically converted to Cu(II), therefore achieving a Cu(I)/Cu(II) redox cycle. It offers a promising strategy for synthesis of advanced electrocatalysts with high efficiency and promising applications in this paper.

Graphene/PEDOT/Ni-Based electrochemical Non-Enzymatic glucose sensor

Compared to enzymatic glucose sensors, non-enzymatic glucose sensors offer significant advantages in sensitivity, stability, and cost. In this study, a green and simple electrochemical method was employed to prepare an electrochemical non-enzymatic glucose sensor based on graphene/PEDOT/Ni materials. The modified electrode was characterized using scanning electron microscopy (SEM), Raman spectroscopy, Fourier-transform infrared spectroscopy (FTIR), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The electrochemical behavior of glucose on the modified electrode was investigated, and the results indicated that the sensor exhibited a good electrochemical response to glucose. Experimental conditions were optimized, and under the optimal conditions, the sensor showed a good linear relationship with glucose concentration in the range of 0.0001 to 7 mM, with a detection limit of 0.012 μM. The sensitivity was 1561 μA·mM−1·cm−2, demonstrating excellent reliability, stability, and accuracy.

Highly stable and selective determination of glucose by a modified glassy carbon electrode based on micro-rods [Ni(HL)NCS] complex as a novel modifier

Non-enzymatic glucose sensors have acquired a lot of attention, where the modifier materials perform as an electrocatalyst instead of an enzyme on the surface of electrodes. More active sites, increased synergistic reactions, and expanded contacts between the electrolyte and the catalyst are essential to enhance catalytic performances. Numerous efforts have been made to fabricate novel non-enzymatic glucose sensors with electrode modification strategies. Herein, a non-enzymatic electrochemical glucose sensor was constructed by a modified glassy carbon electrode (GCE) based on micro-rods [Ni(HL)NCS] complex (MR-NiC/GCE) as a novel modifier for the glucose detection. In alkali media, the non-enzymatic glucose sensor showed a linear dynamic range (LDR) of 100-1100 µM with an excellent limit of detection (LOD) of 15.8 μM (S/N= 3). The proposed sensor demonstrated remarkable stability (after recording 50 continuous cycles), good reproducibility, and significant anti-interference performance toward fructose (Fru), ascorbic acid (AA), dopamine (DA), citric acid (CA), uric acid (UA) and sucrose. According to this study, complexes can be an excellent suggestion to fabricate non-enzymatic glucose sensors.

Growth of WO3 nanostructure deposited on TiO2 nanotube arrays for electrochemical enzyme-free glucose sensor

In this study, a novel WO3-TiO2 hybrid nanostructure-based electrochemical non-enzymatic glucose biosensor has been developed. The anodization method was utilized to successfully produce TiO2 nanotubes on Ti6Al4V alloy functioning as substrates and WO3 nanomaterial decorate on the surface of TiO2 nanotubes (TNTs) deposited through electrochemical technique. The incorporation of WO3 on TNTs has resulted in a high electroactive surface and more degradation resistance in comparison to pure TNTs, resulting in enhanced electron transfer rate and electrode stability. High-resolution transmission electron microscopy (HR-TEM), field emission scanning electron microscopy (FE-SEM), and X-ray diffraction were used to investigate the crystalline structure and morphology of the WO3-TiO2 nanostructure. The electrochemical properties of the hybrid electrodes were investigated employing amperometry, cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The hybrid electrode had a promising sensitivity (1228.12 μA/mM/cm2), low detection limit (0.19 mM), wide linear range (1.0–6.5 mM), and short response time (2-s). The sensors also demonstrated superior levels of reproducibility, repeatability, and stability.

One-step green synthesis of flower-like non-precious metal (Cu, Ni, Fe or Zn) doped ZIF-67 and its application as non-enzymatic electrochemical glucose sensors

Co ions and imidazolate ligands can be self-assembled into a novel metal-organic frameworks (MOFs) with zeolite-like topological structures, which is named as ZIF-67. Flower-like ZIF-67 can be precisely prepared by one-step green synthesis method under specific experimental conditions, and has excellent enzyme-like electrocatalytic activity toward glucose. Non-precious metal (Cu, Ni, Fe or Zn) can be doped into flower-like ZIF-67 while maintaining zeolite-like topological structures, which may also be an important way to enhance the electrocatalytic performances of ZIF-67. In this study, flower-like non-precious metal (Cu, Ni, Fe or Zn) doped ZIF-67 was contrastively researched by physical characterizations and electrochemical techniques, and was employed as electrocatalysts for non-enzymatic electrochemical glucose sensors. Flower-like non-precious metal (Cu, Ni, Fe or Zn) doped ZIF-67 all exhibits perfect electrocatalytic activities toward glucose, among them the performance of Fe(5 %)-ZIF-67 is the most outstanding.

Directionally Exfoliated Ni/Co Hydroxide-Organic Framework Nanosheets for Enhanced Wearable Glucose Sensing.

We report two-dimensional (2D) Ni/Co-based metal hydroxide-organic framework nanosheets (Ni/Co-MHOF NSs) for the construction of an efficient electrochemical nonenzymatic glucose sensor. The nanosheet architecture maximizes the exposure of coordinatively unsaturated metal sites, which enables a largely improved electrocatalytic performance toward the glucose oxidation reaction. The as-designed nonenzymatic sensor exhibits a high sensitivity of 235.71 μA·mM-1·cm-2 and a wide linear range of 1-3000 μM. The sensor presents excellent selectivity against several potential interferences and a short response time of 3.0 s. Of interest, a high-performance flexible sensor is developed by depositing the Ni/Co-MHOF NSs on screen-printed electrodes, which reveal decent bending stability. The designed glucose sensor patch can attach to the human body and realize noninvasive glucose monitoring in human sweat. This work may shed light on the application of novel MHOFs in the field of wearable electrochemical sensing.

Nanostructured metallic enzymes mimic for electrochemical biosensing of glucose

In many domains, the creation of nonenzymatic glucose sensors with robust electrocatalytic activity and chemical stability is indispensable. However, the design of nanoarchitecture transition metals and their nanocomposites as sensing interfaces for nonenzymatic recognition groups remains a formidable challenge. This review discusses the engineered nanoarchitecture transition metals used as non-enzymatic glucose sensors, with a particular focus on their applications characterized by low cost, high sensitivity, and long-term durability. Central to our discussion is the imperative of crafting nanostructured transition materials with expansive specific surface areas and well-defined active sites to serve as electrochemical sensing platforms. Our objective is to shed light on the enhanced electrochemical behavior toward glucose without reliance on mediators or templates. Leveraging advancements in nanotechnology, this review seeks to elucidate strategies for refining conventional nanostructures to optimize enzyme-free glucose sensing applications. Additionally, we delve into the inherent challenges and potential applications of these sensors for detecting glucose and outline ways to develop better non-enzymatic electrochemical glucose sensors.

Development of Highly Sensitive and Selective Electrochemical Glucose Sensors Based on the Modification of the Surface, Structural, and Morphological Properties of ZnO Using Vitamin-B Complexes

Non-enzymatic electrochemical glucose sensors are particularly advantageous because of their simplicity, low cost, efficiency, and long storage life. ZnO structures were modified with water-soluble vitamin B12, B9, and B6 complexes in alkaline 0.1 M NaOH solutions to enhance glucose sensing. ZnO samples were hydrothermally synthesized using 5 mg fixed masses of B12, B9, and B6 complexes. X-ray diffraction, scanning electron microscopy, UV-visible spectrometry, and Fourier transform infrared spectroscopy were used to determine crystalline properties, morphology, and optical band gap. Zinc oxide obtained from vitamin B complexes had a hexagonal structure similar to wurtzite, modified nanorods on its surface, and a reduced optical band gap. The molecular weight, size, and number of functional groups vitamins also influenced surface and structural characteristics of ZnO. Zinc oxide from the B12 complex proved excellent for non-enzymatic glucose sensing in alkaline conditions. B12-derived ZnO glucose sensors have a linear range of 0.1 to 10 mM with a detection limit of 0.005 mM. In the glucose sensing process, a satisfactory level of stability, reproducibility, and selectivity was observed. Furthermore, it was found that ZnO derived from B12 had a high electrical conductivity, which facilitated electron transfer during glucose oxidation.

Enhanced sensing performance of flexible non-enzymatic electrochemical glucose sensors using hollow Fe3O4 nanospheres of controllable morphologies

Rapid and accurate monitoring of glucose concentration is of great significance in clinical diagnosis and treatment of diabetes and hence, it is necessary to develop glucose sensors of superior electro-catalytic capacity. Most literature utilize synergistic effect of nanocomposites to enhance glucose sensing performance, whereas it suffers from crucial restriction in physical and chemical characteristics of each constituents. Morphology of nanostructures significantly affects the electro-catalytic capacity, thus it is a novel route to improve glucose sensing performance to adjust morphology of nanostructures. Herein, we presented highly sensitive non-enzymatic electrochemical sensors for rapid and accurate glucose analysis with hollow Fe3O4 nanospheres (Fe3O4NSs) of controllable morphologies decorated on flexible fibers. The morphologies of the Fe3O4NSs were evaluated with quantitative parameters like diameter, roundness, roughness, skewness, and kurtosis acquired from SEM images and image processing algorithms, and their effect on the interfacial characteristics and the electro-catalytic capacity of the glucose sensors was investigated. Owing to the unique spherical nanostructures and superior catalysis, the Fe3O4NSs exhibit desirable solid/liquid interface for mass diffusion and abundant active sites for sufficient oxidation of glucose. Moreover, much rounder and rougher Fe3O4NSs of near Gaussian surface are readily produced at a higher Fe3+ concentration and result in favorable sensing performance. Accordingly, the optimal glucose sensor shows sensitivities of 96.1 ± 5.4 μA mM−1 cm−2 and 38.2 ± 2.2 μA mM−1 cm−2 over a preferable range of 0–18.0 mM, and a lower detection limit of 19.2 μM. Besides, the glucose sensors remain acceptable response after continuous testing for 20 times and repetitive bending for 50 times, and display superior selectivity to glucose and accurate analysis to practical samples. It is a facile and effective methodology to regulate the morphologies of the Fe3O4NSs for enhanced electro-catalytic capacity of glucose sensors.

A wearable non-enzymatic sensor for continuous monitoring of glucose in human sweat

To enhance personalized diabetes management, there is a critical need for non-invasive wearable electrochemical sensors made from flexible materials to enable continuous monitoring of sweat glucose levels. The main challenge lies in developing glucose sensors with superior electrochemical characteristics and high adaptability. Herein, we present a wearable sensor for non-enzymatic electrochemical glucose analysis. The sensor was synthesized using hydrothermal and one-pot preparation methods, incorporating gold nanoparticles (AuNPs) functionalized onto aminated multi-walled carbon nanotubes (AMWCNTs) as an efficient catalyst, and crosslinked with carboxylated styrene butadiene rubber (XSBR) and PEDOT:PSS. The sensors were then integrated onto screen-printed electrodes (SPEs) to create flexible glucose sensors (XSBR-PEDOT:PSS-AMWCNTs/AuNPs/SPE). Operating under neutral conditions, the sensor exhibits a linear range of 50 μmol/L to 600 μmol/L, with a limit of detection limit of 3.2 μmol/L (S/N = 3), enabling the detection of minute glucose concentrations. The flexible glucose sensor maintains functionality after 500 repetitions of bending at a 180° angle, without significant degradation in performance. Furthermore, the sensor exhibits exceptional stability, repeatability, and resistance to interference. Importantly, we successfully monitored changes in sweat glucose levels by applying screen-printed electrodes to human skin, with results consistent with normal physiological blood glucose fluctuations. This study details the fabrication of a wearable sensor characterized by ease of manufacture, remarkable flexibility, high sensitivity, and adaptability for non-invasive blood glucose monitoring through non-enzymatic electrochemical analysis. Thus, this streamlined fabrication process presents a novel approach for non-invasive, real-time blood glucose level monitoring.

Facilely prepared Co-based MOF functionalized N, S-doped reduced graphene oxide for electrochemical non-enzymatic glucose sensing

Rational design of modified electrode materials is critical for electrochemical sensors. Metal-organic frameworks (MOFs), a novel sort of substance with porosity, has received widespread attention owing to various superior characteristics such as adjustable pore sizes, great surface area and controllable structures. Nevertheless, the poor charge transfer capability of MOFs leads to a general suppression of their electrochemical sensing performance. To solve this issue, compositing conductive substance with MOFs have been demonstrated to be an effective strategy. Herein, Co-based MOF (ZIF-67) functionalized N, S-doped reduced graphene oxide (N, S-RGO) heterostructure (ZIF-67/N, S-RGO) was fabricated through an in-situ synthesis method. The composite material was used in the modification of an electrode to construct a sensing platform for non-enzymatic glucose testing. The synergistic interaction of ZIF-67 and N, S-RGO not only provided more efficient active sites and larger surface areas, but also improved the electron transport efficiency and electrocatalytic performance. Under optimized conditions, the ZIF-67/N, S-RGO/GCE had a dynamic linear range of 1–3200 μM, with a detection limit of 0.33 μM (S/N = 3) for glucose detection. The sensing platform also provided excellent reproducibility, selectivity, and stability (70 % activity retained after 12 days). Furthermore, the sensor had the potential to apply for glucose determination in human serum. This work presented a novel strategy to the field of non-enzymatic glucose sensing and may provide effective coaching for optimizing the electrochemical sensing performance of other series of MOFs.

Electrochemical Non-Enzymatic Glucose Sensing Platform Based on Vanadium Pentoxide Film-Modified Screen Printed Gold Electrode

A screen printed gold electrode (SPGE) served as the foundation for directly depositing Vanadium pentoxide (V2O5), crafting an enzyme-free glucose sensor. Through cyclic voltammetry in an alkaline setting, the sensor's ability to drive glucose oxidation was explored. Utilizing V2O5 as an electrocatalyst, this non-enzymatic sensor exhibited an expansive linear detection range (1 mM–10 mM) and an impressively low detection limit of 0.9 μM. These results underscored V2O5's robust electrocatalytic process in facilitating glucose oxidation within alkaline solutions, unaffected notably by substances like ascorbic acid, fructose and maltose. This investigation highlights a direct and efficient method for glucose detection without reliance on enzymes.

Non-enzymatic Glucose Sensor Based on Ni(OH)2/NF Materials Using Different Pulse Voltammetry Technique

Non-enzymatic glucose sensors have gained significant attention owing to their potential for accurate and cost-effective glucose detection. Nanomaterials play a pivotal role in enhancing performance of non-enzymatic glucose sensor. In this study, a novel non-enzymatic glucose sensor based on Ni(OH)2/NF (nickel hydroxide/nickel foam) materials was developed using different pulse voltammetry technique. Chemical precipitation methods have been used to grow Ni(OH)2 nanostructures directly on a nickel foam electrode. The characterization of the synthesized materials was performed through field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDX), and X-ray diffraction (XRD). The performance of the Ni(OH)2/NF-based glucose sensor was evaluated through electrochemical measurements. Nanoscale hive-like structures of Ni(OH)2 with a diameter ranging from 450 to 530 μm and a thickness of 20 nm were formed on the NF surface. The sensor exhibited good performance, displaying a high sensitivity of 8.42mA.mM-1.cm-2 with a low detection limit of 0.84 μM. These results position the synthesized electrode as a promising contender for non-enzymatic electrochemical glucose sensors.

Tailoring the d-band center on Ru1Cu single-atom alloy nanotubes for boosting electrochemical non-enzymatic glucose sensing.

The development of cost-effective and highly efficient electrocatalysts is critical to help electrochemical non-enzymatic sensors achieve high performance. Here, a new class of catalyst, Ru single atoms confined on Cu nanotubes as asingle-atom alloy (Ru1Cu NTs), with aunique electronic structure and property, was developed to construct a novel electrochemical non-enzymatic glucose sensor for the first time. The Ru1Cu NTs with a diameter of about 24.0nm showed amuch lower oxidation potential (0.38V) and 9.0-fold higher response (66.5 μA) current than Cu nanowires (Cu NWs, oxidation potential 0.47V and current 7.4 μA) for glucose electrocatalysis. Moreover, as an electrochemical non-enzymatic glucose sensor, Ru1Cu NTs not only exhibited twofold higher sensitivity (54.9 μA mM-1cm-2) and wider linear range (0.5-8mM) than Cu NWs, but also showed alow detection limit (5.0μM), excellent selectivity, and great stability. According to theoretical calculation results, the outstanding catalytic and sensing performance of Ru1Cu NTs could be ascribed to the upshift of the d-band center that helped promote glucose adsorption. This work presents a new avenue for developing highly active catalysts for electrochemical non-enzymatic sensors.

Highly Efficient Non-Enzymatic Electrochemical Glucose Biosensor Based on Copper Metal Organic Framework Coated on Graphite Sheet

Detection of glucose is highly informative, creating a constant demand for fabricating high-precision glucose biosensors. Metal–organic frameworks, a family of porous materials renowned for their tunability, can be an excellent choice for developing such sensors. We have developed a highly-sensitive, non-enzymatic sensor for electrochemical detection of glucose fabricated using Copper Metal–Organic Framework (Cu MOF), synthesized by a simple, room-temperature stirring method using Benzene-1,3,5-tricarboxylic acid (BTC) as ligand and Copper nitrate trihydrate as precursor. The synthesized nanostructure was characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, and energy-dispersive X-ray analytical techniques. Powder X-ray diffraction study and thermogravimetric analysis were also done. Further, Brunnauer-Emmett-Teller analysis revealed the porous nature of Cu MOF. The materials exhibited strong electro-catalytic activity for glucose oxidation as revealed from cyclic voltammetry and chronoamperometric studies done under alkaline pH conditions. The Cu MOF deposited on a conducting graphite sheet electrode displayed a significantly low detection limit of 0.019 mM through a broad detection range (1–15 mM) and a strong sensitivity of 229.4 μAmM−1 cm2. Overall, the Cu MOF/GS exhibits exceptional stability, short response time (less than 1 s), and good repeatability and reproducibility, making it a promising future material for non-enzymatic glucose detection.

Ag@TiO2 nanoribbon array: a high-performance sensor for electrochemical non-enzymatic glucose detection in beverage sample

Developing an accurate, cost-effective, reliable, and stable glucose detection sensor for the food industry poses a significant yet challenging endeavor. Herein, we present a silver nanoparticle-decorated titanium dioxide nanoribbon array on titanium plate (Ag@TiO2/TP) as an efficient electrode for non-enzymatic glucose detection in alkaline environments. Electrochemical evaluations of the Ag@TiO2/TP electrode reveal a broad linear response range (0.001 mM - 4 mM), high sensitivity (19,106 and 4264 μA mM−1 cm−2), rapid response time (6 s), and a notably low detection limit (0.18 μM, S/N = 3). Moreover, its efficacy in measuring glucose in beverage samples shows its practical applicability. The impressive performance and structural benefits of the Ag@TiO2/TP electrode highlight its potential in advancing electrochemical sensors for small molecule detection.

Synergistically enhancing electrocatalysis and non-enzymatic sensing for glucose by iridium single-atom/nickel oxide/N-doped graphene.

The development of novel catalyst with high catalytic activity is important for electrochemical non-enzymatic glucose sensing. Here, iridium single-atom/nickel oxide nanoparticle/N-doped graphene nanosheet (Ir1/NiO/NG) with the loading of 1.13 wt% Ir was successfully synthesized for constructing electrochemical non-enzymatic glucose sensor for the first time. The morphology and structure of Ir1/NiO/NG were characterized by XRD, SEM, TEM, HRTEM, and XPS, and the presence of Ir SAs was confirmed by AC-HAADF-STEM. The Ir1/NiO/NG shows 65 mV lower oxidation potential and 3.3 times higher response current than Ni(OH)2/NG. In addition, Ir1/NiO/NG exhibits high sensitivity (70.09 μA mM-1 cm-2), excellent selectivity, low detection limit (2.00 μM), and great stability (91.53% current remaining after 21 days) for electrochemical non-enzymatic glucose sensing. The outstanding catalytic and sensing performance of Ir1/NiO/NG is mainly attributed to synergistic effect of Ir SAs, NiO nanoparticles, and highly conductive NG, which modulate the electronic and geometric structure of Ir1/NiO/NG. This work shows the promising potential of SACs in electrochemical sensing.

Construction of hierarchical NiCo2 S4 /2D-Carbyne nanohybrid onto nickel foam for high performance supercapacitor and non-enzymatic electrochemical glucose sensor applications.

Synthesising and designing pseudocapacitive material with good electrochemical and electrocatalytic behaviour is essential to use as supercapacitor as well as non-enzymatic glucose sensor electrode. In this work, NiCo2 S4 nanoparticles decorated onto the 2D-Carbyne nanosheets are achieved by the solvothermal process. The as-prepared NiCo2 S4 @2D-Carbyne provides rich reaction sites and better diffusion pathways. On usage as an electrode for supercapacitor application, the NiCo2 S4 @2D-Carbyne exhibits the specific capacitance of about 2507 F g-1 at 1 A g-1 . In addition, the fabricated hybrid device generates an energy density of 52.2 Wh kg-1 at a power density of 1.01 kW kg-1 . Besides, the glucose oxidation behaviour of NiCo2 S4 @2D-Carbyne modified GCE has also been performed. The diffusion of glucose from the electrolyte to the electrode obeys the kinetic control process. Furthermore, the fabricated NiCo2 S4 @2D-Carbyne non-enzymatic glucose sensor exhibits a limit of detection of about 34.5 μM with a sensitivity of about 135 μA mM-1 cm-2 . These findings highlight the need to design and synthesis electrode materials with adequate electrolyte-electrode contact, strong structural integrity, and rapid ion/electron transport.

A novel NiO/C@rGO nanocomposite derived from Ni(gallate): A non-enzymatic electrochemical glucose sensor

The development of suitable substrate materials in electrochemical sensors is essential for rapid and reliable quantification in the diagnostic and clinical fields. In this paper, NiO/C@rGO nanocomposite was synthesized through nickel (gallate) pyrolysis with graphene oxide and employed as a substrate to construct a glucose sensor with high selectivity and sensitivity. The structural characterizations of NiO/C@rGO were assessed by Fourier transform infrared spectroscopy, X-ray diffraction, field emission scanning electron microscopy, energy disperse spectroscopy, and elemental mapping. The newly fabricated biosensor (NiO/C@rGO/GCE) exhibited a high sensing performance with an extensive dynamic linear range (from 1 μM to 1115 μM) and a low limit of detection (LOD) 0.658 μM (S/N = 3) toward glucose. In addition, the NiO/C@rGO-based sensor displayed good stability, favorable repeatability, and anti-interference ability for determining glucose. It was also used to measure glucose in serum samples, and satisfactory results were attained. These results illustrated that the NiO/C@rGO nanocomposite could be applied as an excellent electrochemical sensing material with high sensitivity to diagnose glucose-related illnesses.