Displaying publications 1 - 20 of 35 in total

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  1. Mahmoudian MR, Basirun WJ, Woi PM, Hazarkhani H, Alias YB
    Mikrochim Acta, 2019 05 22;186(6):369.
    PMID: 31119482 DOI: 10.1007/s00604-019-3481-y
    The study presents the synthesis of polypyrrole-coated palladium platinum/nitrogen-doped reduced graphene oxide nanocomposites (PdPt-PPy/N-rGO NC) via direct the reduction of Pd(II) and Pt(II) in the presence of pyrrole monomer, N-rGO and L-cysteine as the reducing agent. X-ray diffraction confirmed the presence of metallic Pd and Pt from the reduction of Pd and Pt cations. Transmission electron microscopy images revealed the presence of Pd, Pt and PPy deposition on N-rGO. Impedance spectroscopy results gave a decreased charge transfer resistance due to the presence of N-rGO. The nanocomposites were synthesized with different Pd/Pt ratios (2:1, 1:1 and 1:2). A glassy carbon electrode (GCE) modified with the nanocomposite showed enhanced electrochemical sensing capability for formaldehyde in 0.1 M sulfuric acid solution. Cyclic voltammetry showed an increase in the formaldehyde oxidation peak current at the GCE modified with Pd2Pt1 PPy N-rGO. At a typical potential of 0.45 V (vs. SCE), the sensitivity in the linear segment was 345.8 μA.mM -1. cm-2. The voltammetric response was linear between 0.01 and 0.9 mM formaldehyde concentration range, with a 27 µM detection limit (at S/N = 3). Graphical abstract Schematic presentation of formaldehyde detection by Pd2Pt1-PPy/nitrogen-doped reduced Graphene Oxide Nanocomposite (Pd2Pt1-PPy /N-Gr NC). The decrease of charge transfer resistance and the agglomeration of deposited metals in the presence of N-rGO enhance the current response of the electrochemical sensor.
  2. Ramanathan S, Gopinath SCB, Arshad MKM, Poopalan P, Anbu P
    Mikrochim Acta, 2019 07 18;186(8):546.
    PMID: 31321546 DOI: 10.1007/s00604-019-3696-y
    A genomic DNA-based colorimetric assay is described for the detection of the early growth factor receptor (EGFR) mutation, which is the protruding reason for non-small cell lung cancer. A DNA sequence was designed and immobilized on unmodified gold nanoparticles (GNPs). The formation of the respective duplex indicates the presence of an EGFR mutation. It is accompanied by the aggregation of the GNPs in the presence of monovalent ions, and it indicates the presence of an EGFR mutation. This is accompanied by a color change from red (520 nm) to purple (620 nm). Aggregation was evidenced by transmission electron microscopy, scanning electron microscopy and atomic force microscopy. The limit of detection is 313 nM of the mutant target strand. A similar peak shift was observed for 2.5 μM concentrations of wild type target. No significant peak shift was observed with probe and non-complementary DNA. Graphical abstract Schematic representation of high-specific genomic DNA sequence on gold nanoparticle (GNP) aggregation with sodium chloride (NaCl). It illustrates the detection method for EGFR mutation on lung cancer detection. Red and purple colors of tubes represent dispersed and aggregated GNP, respectively.
  3. Taniselass S, Arshad MKM, Gopinath SCB, Fathil MFM, Ibau C, Anbu P
    Mikrochim Acta, 2021 07 15;188(8):257.
    PMID: 34268634 DOI: 10.1007/s00604-021-04922-x
    A label-free chemical bonding strategy mediated by reduced graphene oxide (rGO) basal plane functional groups has been developed for cardiac Troponin I (cTnI) detection. Four different chemical strategies on respective electrode sensing surface were precedingly examined using electrochemical impedance spectroscopy. The impedimetric assessment was carried out by sweeping frequency at the range 0.1-500 kHz perturbated at a small amplitude of AC voltage (25 mV). The chemical strategy-4 denoted as S-4 shows a significant analytical performance on cTnI detection in spiked buffer and human serum, whereby the pre-mixture of rGO and (3-Aminopropyl)triethoxysilane (APTES) creates a large number of amine sites (-NH2), which significantly enhanced the antibody immobilization without excessive functionalization. The as-fabricated immunosensor exhibited an ultra-low limit of detection of 6.3 ag mL-1 and the lowest antigen concentration measured was at 10 ag mL-1. The immunosensor showed a linear and wide range of cTnI detection (10 ag mL-1-100 ng mL-1) in human serum with a regression coefficient of 0.9716, rapid detection (5 min of binding time), and stable and highly reproducible bioelectrode response with RSD 
  4. Taha BA, Addie AJ, Kadhim AC, Azzahran AS, Haider AJ, Chaudhary V, et al.
    Mikrochim Acta, 2024 Apr 08;191(5):250.
    PMID: 38587660 DOI: 10.1007/s00604-024-06314-3
    Rapid technological advancements have created opportunities for new solutions in various industries, including healthcare. One exciting new direction in this field of innovation is the combination of skin-based technologies and augmented reality (AR). These dermatological devices allow for the continuous and non-invasive measurement of vital signs and biomarkers, enabling the real-time diagnosis of anomalies, which have applications in telemedicine, oncology, dermatology, and early diagnostics. Despite its many potential benefits, there is a substantial information vacuum regarding using flexible photonics in conjunction with augmented reality for medical purposes. This review explores the current state of dermal augmented reality and flexible optics in skin-conforming sensing platforms by examining the obstacles faced thus far, including technical hurdles, demanding clinical validation standards, and problems with user acceptance. Our main areas of interest are skills, chiroptical properties, and health platform applications, such as optogenetic pixels, spectroscopic imagers, and optical biosensors. My skin-enhanced spherical dichroism and powerful spherically polarized light enable thorough physical inspection with these augmented reality devices: diabetic tracking, skin cancer diagnosis, and cardiovascular illness: preventative medicine, namely blood pressure screening. We demonstrate how to accomplish early prevention using case studies and emergency detection. Finally, it addresses real-world obstacles that hinder fully realizing these materials' extraordinary potential in advancing proactive and preventative personalized medicine, including technical constraints, clinical validation gaps, and barriers to widespread adoption.
  5. Letchumanan I, Gopinath SCB, Arshad MKM
    Mikrochim Acta, 2020 01 14;187(2):128.
    PMID: 31938893 DOI: 10.1007/s00604-020-4115-0
    A method is described for the electrochemical determination of squamous cell carcinoma (SCC) antigen, and by testing the effect of 30 nm gold nanoparticles (GNPs). Three comparative studies were performed in the presence and absence of GNPs, and with agglomerated GNPs. The divalent ion Ca(II) was used to induce a strong agglomeration of GNPs, as confirmed by colorimetry and voltammetry. Herein, colorimetry was used to test the best amount of salt needed to aggregate the GNPs. Despite, voltammetry was used to determine the status of biomolecules on the sensor. The topography of the surface of ZnO-coated interdigitated electrodes was analyzed by using 3D-nano profilometry, scanning electron microscopy, atomic force microscopy and high-power microscopy. The interaction between SCC antigen and antibody trigger vibrations on the sensor and cause dipole moment, which was measured using a picoammeter with a linear sweep from 0 to 2 V at 0.01 V step voltage. The sensitivity level was 10 fM by 3σ calculation for the dispersed GNP-conjugated antigen. This indicates a 100-fold enhancement compared to the condition without GNP conjugation. However, the sensitivity level for agglomerated GNPs conjugated antibody was not significant with 100 fM sensitivity. Specificity was tested for other proteins in serum, namely blood clotting factor IX, C-reactive protein, and serum albumin. The SCC antigen was quantified in spiked serum and gave recoveries that ranged between 80 and 90%. Graphical abstractSchematic representation of SCC (squamous cell carcinoma) antigen determination using divalent ion induced agglomerated GNPs. Sensitivity increment depends on the occurrence of more SCC antigen and antibody binding event via GNPs integration. Notably, lower detection limit was achieved at femto molar with proper orientation of biological molecules.
  6. Numan A, Singh S, Zhan Y, Li L, Khalid M, Rilla K, et al.
    Mikrochim Acta, 2021 12 14;189(1):27.
    PMID: 34905090 DOI: 10.1007/s00604-021-05127-y
    Change in the level of human prostate-specific antigen (PSA) is a major element in the development and progression of prostate cancer (PCa). Most of the methodologies are currently restricted to their application in routine clinical screening due to the scarcity of adequate screening tools, false reading, long assay time, and cost. Innovative techniques and the integration of knowledge from a variety of domains, such as materials science and engineering, are needed to provide sustainable solutions. The convergence of precision point-of-care (POC) diagnostic techniques, which allow patients to respond in real time to changes in PSA levels, provides promising possibilities for quantitative and quantitative detection of PSA. This solution could be interesting and relevant for use in PCa diagnosis at the POC. The approaches enable low-cost real-time detection and are simple to integrate into user-friendly sensor devices. This review focuses on the investigations, prospects, and challenges associated with integrating engineering sciences with cancer biology to develop nanotechnology-based tools for PCa diagnosis. This article intends to encourage the development of new nanomaterials to construct high-performance POC devices for PCa detection. Finally, the review concludes with closing remarks and a perspective forecast.
  7. Nadzirah S, Hashim U, Gopinath SCB, Parmin NA, Hamzah AA, Yu HW, et al.
    Mikrochim Acta, 2020 03 17;187(4):235.
    PMID: 32185529 DOI: 10.1007/s00604-020-4214-y
    A titanium dioxide nanoparticle (TiO2 NP)-mediated resistive biosensor is described for the determination of DNA fragments of Escherichia coli O157:H7 (E. coli O157:H7). The sol-gel method was used to synthesize the TiO2 NP, and microlithography was applied to fabricate the interdigitated sensor electrodes. Conventional E. coli DNA detections are facing difficulties in long-preparation-and-detection-time (more than 3 days). Hence, electronic biosensor was introduced by measuring the current-voltage (I-V) DNA probe without amplification of DNA fragments. The detection scheme is based on the interaction between the electron flow on the sensor and the introduction of negative charges from DNA probe and target DNA. The biosensor has a sensitivity of 1.67 × 1013 Ω/M and a wide analytical range. The limit detection is down to 1 × 10-11 M of DNA. The sensor possesses outstanding repeatability and reproducibility and is cabable to detect DNA within 15 min in a minute-volume sample (1 μL). Graphical abstract Fig. (a) Graphical illustration of electronic biosensor set up and (b) relationship between limit of detection (LOD) and the unaffected poultry samples on E. coli O157:H7.
  8. Yan G, Li Q, Hong X, Gopinath SCB, Anbu P, Li C, et al.
    Mikrochim Acta, 2021 05 11;188(6):185.
    PMID: 33977395 DOI: 10.1007/s00604-021-04836-8
    An abdominal aortic aneurysm (AAA) is abnormal swelling in the abdominal aorta and a prevalent life-threatening disease. This research introduces a new interdigitated microelectrode (IDME)-sensing surface modified by iron oxide nanoworms (IONWs) for detecting the AAA biomarker insulin-like growth factor-1 (IGF1). A sandwich pattern was formulated with the IGF1 aptamer and IGFBP1 (IGF binding protein-1) on the IONW-constructed IDME hybrid to identify IGF1. The surface morphology of the IONWs revealed a uniform distribution of worm-like structures (80-100 nm) as confirmed by FESEM and FETEM analyses. Further, the presence of the major elements, Fe and O, was confirmed by EDX and XPS studies. The crystal planes that appeared in the IONW reflect cubic magnetite. IONW-modified IDME attained a limit of detection for IGF1 of 1 fM (3σ) with an aptamer-IGF1-IGFBP1 sandwich. This sandwich with IGFBP1 enhanced the current level at all concentrations of IGF1 and displayed linearity in the range 1 fM to 100 pM with a determination coefficient of R2 = 0.9373 [y = 3.38221x - 4.79]. Control experiments with complementary aptamer sequences, IGF2 and IGFBP3 did not show notable signal changes, indicating the specific detection of IGF1. This IONW constructed electrode helps to achieve the detection of low amounts of IGF1 and diagnose AAA at the stage prior to rupture.
  9. Dalila NR, Arshad MKM, Gopinath SCB, Nuzaihan MNM, Fathil MFM
    Mikrochim Acta, 2020 10 05;187(11):588.
    PMID: 33015730 DOI: 10.1007/s00604-020-04562-7
    Nanofabricated gold nanoparticles (Au-NPs) on MoS2 nanosheets (Au-NPs/MoS2) in back-gated field-effect transistor (BG-FET) are presented, which acts as an efficient semiconductor device for detecting a low concentration of C-reactive protein (C-RP). The decorated nanomaterials lead to an enhanced electron conduction layer on a 100-μm-sized transducing channel. The sensing surface was characterized by Raman spectroscopy, ultraviolet-visible spectroscopy (UV-Vis), atomic force microscopy (AFM), scanning electron microscopy (SEM), and high-power microscopy (HPM). The BG-FET device exhibits an excellent limit of detection of 8.38 fg/mL and a sensitivity of 176 nA/g·mL-1. The current study with Au-NPs/MoS2 BG-FET displays a new potential biosensing technology; especially for integration into complementary metal oxide (CMOS) technology for hand-held future device application.
  10. Pandian K, Mohana Soundari D, Rudra Showdri P, Kalaiyarasi J, Gopinath SCB
    Mikrochim Acta, 2019 01 07;186(2):54.
    PMID: 30618010 DOI: 10.1007/s00604-018-3117-7
    Differential pulse voltammetry (DPV) was employed for the determination of caffeic acid (CA) in acidic solutions by using a glassy carbon electrode (GCE) modified with a chitosan-protected nanohybrid composed of carbon black and reduced graphene oxide. Electrochemical impedance spectroscopy and cyclic voltammetry were utilized to study the interfacial electron transfer on the modified GCE. Cyclic voltammetry shows that CA exhibits a reversible redox reaction with an oxidation peak at + 0.30 V (vs. Ag/AgCl) and a reduction peak at + 0.24 V in pH 3.0 solution at a scan rate of 50 mV·s-1. Under the optimized experimental conditions, the response to CA is linear in 0.3× 10-9 to 57.3 × 10-5 M concentration range. The limit of detection is 0.03 × 10-9 M (at an S/N ratio of 3), and the electrochemical sensitivity is 5.96 μA∙ μM-1∙cm-2. This sensor for CA displays better sensitivity and a response over a wider concentration range. It was applied to the determination of CA at trace levels in various (spiked) wine samples. Graphical abstract Schematic presentation of a sensitive electrochemical method for the quantitative detection of caffeic acid using chitosan protected carbon black and reduced graphene oxide. It can be used for the quantitative detection of caffeic acid in wine samples.
  11. Ranjani B, Kalaiyarasi J, Pavithra L, Devasena T, Pandian K, Gopinath SCB
    Mikrochim Acta, 2018 02 23;185(3):194.
    PMID: 29594516 DOI: 10.1007/s00604-018-2715-8
    A sensing device was constructed for the amperometric determination of nitrite. It is based on the use of titanium dioxide (TiO2) nanotubes template with natural fibers and carrying hemin acting as the electron mediator. A glassy carbon electrode (GCE) was modified with the hemin/TNT nanocomposite. The electrochemical response to nitrite was characterized by impedance spectroscopy and cyclic voltammetry. An amperometric study, performed at a working potential of + 0.75 V (vs. Ag/AgCl), showed the sensor to enable determination of nitrite with a linear response in the 0.6 to 130 μM concentration range and with a 59 nM limit of detection. Corresponding studies by differential study voltammetry (Ep = 0.75 V) exhibited a linear range from 0.6 × 10-6 to 7.3 × 10-5 M with a limit of detection of 84 nM. The sensing device was applied to the determination of nitrite in spiked tap and lake water samples. Graphical abstract Natural fibers templated synthesis of TNT immobilized hemin as electron transfer mediator for quantitative detection of nitrite with detection limit of 59 nM and good electrochemical sensitivity and the method can be used for quantitative determination of nitrite in water samples.
  12. Rahman SFA, Arshad MKM, Gopinath SCB, Fathil MFM, Sarry F, Ibau C, et al.
    Mikrochim Acta, 2024 Jan 31;191(2):118.
    PMID: 38296851 DOI: 10.1007/s00604-024-06189-4
    Highly specific detection of tumor-associated biomarkers remains a challenge in the diagnosis of prostate cancer. In this research, Maackia amurensis (MAA) was used as a recognition element in the functionalization of an electrochemical impedance-spectroscopy biosensor without a label to identify cancer-associated aberrant glycosylation prostate-specific antigen (PSA). The lectin was immobilized on gold-interdigitated microelectrodes. Furthermore, the biosensor's impedance response was used to assess the establishment of a complex binding between MAA and PSA-containing glycans. With a small sample volume, the functionalized interdigitated impedimetric-based (IIB) biosensor exhibited high sensitivity, rapid response, and repeatability. PSA glycoprotein detection was performed by measuring electron transfer resistance values within a concentration range 0.01-100 ng/mL, with a detection limit of 3.574 pg/mL. In this study, the ability of MAA to preferentially recognize α2,3-linked sialic acid in serum PSA was proven, suggesting a potential platform for the development of lectin-based, miniaturized, and cost effective IIB biosensors for future disease detection.
  13. Yusoff N, Rameshkumar P, Mohamed Noor A, Huang NM
    Mikrochim Acta, 2018 04 03;185(4):246.
    PMID: 29616348 DOI: 10.1007/s00604-018-2782-x
    An amperometric sensor for L-Cys is described which consists of a glassy carbon electrode (GCE) that was modified with reduced graphene oxide placed in a Nafion film and decorated with palladium nanoparticles (PdNPs). The film was synthesized by a hydrothermal method. The PdNPs have an average diameter of about 10 nm and a spherical shape. The modified GCE gives a linear electro-oxidative response to L-Cys (typically at +0.6 V vs. SCE) within the 0.5 to 10 μM concentration range. Other figures of merit include a response time of less than 2 s, a 0.15 μM lower detection limit (at signal to noise ratio of 3), and an analytical sensitivity of 1.30 μA·μM-1·cm-2. The sensor displays selectivity over ascorbic acid, uric acid, dopamine, hydrogen peroxide, urea, and glucose. The modified GCE was applied to the determination of L-Cys in human urine samples and gave excellent recoveries. Graphical abstract Spherical palladium nanoparticles (PdNPs) on reduced graphene oxide-Nafion (rGO-Nf) films were synthesized using a hydrothermal method. This nanohybrid was used for modifying a glassy carbon electrode to develop a sensor electrode for detecting L-cysteine that has fast response (less than 2 s), low detection limit (0.15 μM), and good sensitivity (0.092 μA μM-1 cm-2).
  14. Ibrahim I, Lim HN, Huang NM
    Mikrochim Acta, 2019 06 14;186(7):452.
    PMID: 31201543 DOI: 10.1007/s00604-019-3547-x
    A multi-functional hybrid of cellulose acetate with cadmium sulfide and Methylene blue (CA/CdS/MB) in a bead composition was synthesized and investigated as a photosensor-adsorbent for the rapid, selective, and sensitive detection, and adsorption of Cu(II) ions. These hybrid CA-modified beads are composed of multiple adsorption active sites and possess a surface area of 58 cm2 g-1. They are an efficient adsorbent with a maximum adsorption capacity of 0.57 mg g-1. Photoelectrochemical (PEC) detection of Cu(II) was accomplished by modifying the beads on a glassy carbon electrode. The beads containing 20 mmol of sulfur displayed the widest linear analytical range (0.1-290 nM) and the lowest detection limit (16.9 nM) for Cu(II) with high selectivity and reliable reproducibility. The successful application of the beads has provided a new insight for the selection of a responsive photoactive material for a PEC assay, as well as an effective adsorbent material for Cu(II) ions. Graphical abstract A multi-functional hybrid of cellulose acetate with cadmium sulfide and Methylene blue (CA/CdS/MB) in a bead composition was synthesized and investigated as a photosensor-adsorbent for the rapid, selective and sensitive detection and adsorption of Cu(II) ions.
  15. Ahmad H, Haseen U, Umar K, Ansari MS, Ibrahim MNM
    Mikrochim Acta, 2019 08 27;186(9):649.
    PMID: 31456042 DOI: 10.1007/s00604-019-3753-6
    The authors describe a method for solvent-free mechano-chemical synthesis of a bioinspired sorbent. A 2D ultra-thin carbon sheet similar to graphene oxide was prepared using a natural waste (onion sheet). The formation of 2D carbon sheets was confirmed by Raman spectroscopy, X-ray photoelectron spectroscopy and ATR-IR. The surface morphology was characterized by field emission scanning electron microscopy and high-resolution tunneling electron microscopy. The carbon sheets were decorated with crystalline MnFe2O4 nanoparticles by solid-state reaction at room temperature. The presence of magnetic particles in the final product was confirmed by vibrating sample magnetometry and electron microscopy. The synergistic effect of carbon sheets and MnFe2O4 led to an enhanced sorption of arsenic species compared to bare carbon sheets or to MnFe2O4 nanoparticles. A column was prepared for the simultaneous preconcentration and determination of trace levels of As(III) and As(V) from water samples. The preconcentration factors are between 900 and 833 for As(III) and As(V) species, respectively. The linearity of the calibration plot ranges from 0.4-10 ng mL-1. The detection limits (at 3σ) for both As(III) and As(V) are 30 pg mL-1. The Student's t values for the analysis of spiked samples are lower than the critical Student's t values at a 95% confidence level. The recoveries from spiked water samples range between 99 and 102.8%. Graphical abstract Schematic representation of the preparation of carbon sheets similar to graphene oxide from onion sheaths after pyrolysis at 800 °C. The prepared carbon sheet-MnFe2O4 composite shows excellent arsenic sorption and preconcentration down to the pg mL-1 concentration.
  16. Arul P, Huang ST, Gowthaman NSK, Govindasamy M, Jeromiyas N
    Mikrochim Acta, 2020 11 09;187(12):650.
    PMID: 33165679 DOI: 10.1007/s00604-020-04631-x
    A copper-1,4-naphthalenedicarboxylic acid-based organic framework (Cu-NDCA MOF) with different morphologies was synthesized by solvothermal synthetic route via a simple protonation-deprotonation approach. The synthesized Cu-NDCA MOFs were analyzed by diverse microscopic and spectral techniques. The FE-SEM and TEM image results exhibited the flake-like (FL), partial anisotropic (PAT), and anisotropic (AT)-Cu-NDCA MOFs formation obtained at different pH (3.0, 7.0, and 9.0) of the reaction medium. The AT-Cu-NDCA MOF/GC electrode not only increases the electroactive surface area but also boosts the electron transfer rate reaction compared to other modified electrodes (PAT- and FL-Cu-NDCA MOFs/GCEs). Under the optimized conditions, the modified electrode (AT-Cu-NDCA MOF) exhibited a sharp oxidation peak (+ 0.46 V vs. Ag/AgCl) and higher current response for rutin. The electrode provides a wide linear range from 1 × 10-9 to 50 × 10-6 M, a low detection limit of 1.21 × 10-10 M, LOQ of 0.001 μM, and sensitivity of 0.149 μA μM-1 cm-2. The AT-Cu-NDCA MOF/GC electrode exhibited good stability (RSD = 3.52 ± 0.02% over 8 days of storage), and excellent reproducibility (RSD = 2.62 ± 0.02% (n = 3)). The modified electrode was applied to the determination of rutin in apple, orange, and lemon samples with good recoveries (99.79-99.91, 99.24-99.69, and 99.53-99.83, respectively). Graphical abstract Anisotropic structure of Cu-NDCA MOFs and its modification on glassy carbon electrode for ultra-sensitive determination of rutin in fruit samples.
  17. Azri FA, Eissa S, Zourob M, Chinnappan R, Sukor R, Yusof NA, et al.
    Mikrochim Acta, 2020 04 12;187(5):266.
    PMID: 32279134 DOI: 10.1007/s00604-020-4218-7
    An electrochemical aptasensor is described for determination of the phytohormone of zearalenone (ZEA). The gold electrode was modified with ZEA via covalent attachment using cysteamine-hydrochloride and 1,4-phenylene diisocyanate linker. A truncated ZEA aptamer with a dissociation constant of 13.4 ± 2.1 nM was used in an aptasensor. The electrochemical property was investigated using square wave voltammetry for monitoring the change in the electron transfer using the ferro/ferricyanide system as redox probe. Under optimal experimental conditions, the response was best measured at a potential of 0.20 V (vs. Ag/AgCl). The signals depended on the competitive mechanism between the immobilised ZEA and free ZEA for the aptamer binding site. The aptasensor works in the range 0.01 to 1000 ng·mL-1 ZEA concentration, with a detection limit of 0.017 ng·mL-1. High degree of cross-reactivity with the other analogues of ZEA was observed, whereas none towards other mycotoxins. The aptasensor was further applied for the determination of ZEA in the extract of maize grain and showed good recovery percentages between 87 and 110%. Graphical abstract Schematic representation of the electrochemical determination of zearalenone based on indirect competitive assay. Step a Immobilisation of ZEA on the surface of gold electrode via covalent attachment, b competition for the ZEA aptamer binding site between immobilised and free ZEA, and c current signal of the binding event based on SWV technique.
  18. Ahmad H, Umar K, Ali SG, Singh P, Islam SS, Khan HM
    Mikrochim Acta, 2018 05 10;185(6):290.
    PMID: 29748777 DOI: 10.1007/s00604-018-2829-z
    A column sorbent for arsenic was obtained through immobilization of highly branched polyethylenimine (PEI) on graphene oxide (GO). The composite material enables speciation of arsenic by tuning the pH of the sample solution which governs the surface charge of the sorbent, depending on whether amino groups (-NH2) are present (at high pH) or ammonium groups (-NH3+; at low pH). The composite can be applied to improved speciation of arsenic (compared to unmodified GO). There is no need for oxidation or reduction of arsenic. A column procedure was applied for the sequestered extraction and speciation of As(III) and As(V) from environmental water samples before their determination by hydride generation-microwave induced plasma-atomic emission spectrometry. The method has a preconcentration factor of 440 for As(III) and of 400 for As(V). The limits of detection (at 3 S/N) are extremely low, being 1.8 ± 0.2 ngL-1 for As(III) and 1.3 ± 0.08 ngL-1 for As(V). This is much lower than the arsenic guideline value of 10 μgL-1 as given by the WHO. Graphical abstract Graphene oxide interconnected with polyethyleneimine has been employed for the speciation and determination of arsenic. Quantitation by atomic emission spectroscopy reveals a high preconcentration factor (440 and 400) and low LODs of 1.8 ± 0.2 and 1.3 ± 0.08 ngL-1for As(III) and As(V), respectively.
  19. Kannan SK, Esakkiappa S, Anthonysamy E, Sudalaimuthu S, Sulaiman Y, Khan MM, et al.
    Mikrochim Acta, 2023 Feb 10;190(3):87.
    PMID: 36759372 DOI: 10.1007/s00604-023-05664-8
    Spermine (SPM) is considered a biomarker for prostate cancer and detecting it becomes highly challenging due to its electro- and optical-inactive nature. SPM has a tendency to interact with groups such as phosphates and sulfides to form macrocyclic arrangements known as nuclear aggregates of polyamines. Using this tendency, an electrochemical sensor has been developed using a polysulfide (PS) modified Au electrode (PS@Au electrode). PS has been synthesized from elemental sulfur by hydrothermal method and characterized using UV-Vis, fluorescence, FTIR, SEM, and XPS analyses. The PS@Au electrode was employed for electrochemical sensing of SPM. In the presence of SPM, a decrease in gold oxide reduction current was noted which is proportional to the concentration of SPM. The decrease in gold oxide reduction (0.5 V) current was attributed to the complexing nature of SPM-PS at the electrode interface. The reason for the decrease in current has been substantiated using XRF, XPS, and spectroelectrochemical studies. Under the optimized conditions, the PS@Au electrode exhibited a linear range of 1.55-250 µM with LOD of 0.511 ± 0.02 µM (3σ). The electrochemical strategy for SPM sensing exhibited better selectivity even in the presence of possible interferents. The selectivity stems from the selective interaction of SPM with PS on the Au electrode surface; the tested amino acids, and other molecules do not complex with PS and hence they could not interfere. The PS@Au electrode has been subjected to the determination of SPM in artificial urine samples and exhibited outstanding performance in the synthetic sample.
  20. Amiri A, Ghaemi F, Maleki B
    Mikrochim Acta, 2019 02 01;186(3):131.
    PMID: 30707373 DOI: 10.1007/s00604-019-3246-7
    Different types of hybrid nanocomposites were prepared from a copper-based metal-organic framework (MOF-199) and graphene (Gr) or fullerene (Fl). The porosity and quality of the nanocomposites were studied by scanning electron microscopy, transmission electron microscopy and BET surface area analysis. The nanocomposites are shown to be viable sorbents for the dispersive micro solid phase extraction of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. This is due to (a) the presence of MOF-199 which leads to improved adsorption capacity, and (b) the presence of Gr or Fl on the surface of MOF-199 which enhances the interaction with PAHs. Specifically, acenaphthene, anthracene, benz[a]anthracene, fluorene, naphthalene, 2-methylnaphthalene, and pyrene were studied. A comparison of the sorbents shows MOF-199/Gr to possess the highest adsorption affinity and to be most durable, probably a result of the high porosity of graphene. Following desorption with acetonitrile, the PAHs were quantified by GC with FID detection. Under the optimum conditions, limits of detection (at an S/N ratio of 3) range from 3 to 10 pg mL-1, and the analytical ranges are linear at 0.01-100 ng mL-1 of PAHs. The relative standard deviations for five replicates at two spiking levels (0.03 and 50 ng mL-1) range from 5.0 to 7.4%. The applicability of this method was confirmed by analyzing spiked real water samples, and recoveries are between 91.9 and 99.5%. Graphical abstract Different types of the hybrid nanocomposites of the copper-based metal-organic framework MOF-199 with graphene or fullerene were synthesized and used as sorbent for the dispersive micro solid phase extraction of polycyclic aromatic hydrocarbons in environmental water samples.
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