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  1. Ng KL, Lee SM, Khor SM, Tan GH
    Anal Sci, 2015;31(10):1075-81.
    PMID: 26460374 DOI: 10.2116/analsci.31.1075
    Graphite material is abundantly available from recyclable sources. It possesses a good electrical conductance property, which makes it an attractive material as a working electrode. However, due to a high activation overpotential it has limited applications as compared to other solid metal electrodes. In this present work, we obtained a graphite rod from a used battery, and carried out electrochemical improvements by electro-deposition with gold nanoparticles (AuNPs). The heterogeneous electron transfer rate and electron transfer resistance of the fabricated electrode were improved. The electrode overpotential has shown improvement by 50 mV, and the effective surface area has increased by 2 fold. To determine the practicability of the AuNPs/graphite electrode, we used the electrode in the analysis of myricetin. A square-wave voltammetry was used in the analysis, and the detection response increased by 2.5 fold, which suggested an improvement in the electrode sensitivity.
  2. Saad B, Wai WT, Ali AS, Saleh MI
    Anal Sci, 2006 Jan;22(1):45-50.
    PMID: 16429771
    A flow injection analysis (FIA) method for the determination of four residual chlorine species, namely combined available chlorine (CAC), free available chlorine (FAC), total available chlorine (TAC) and chlorite (ClO2-) was developed using a flow-through triiodide-selective electrode as a detector. An important strategy of speciation studies utilized the kinetic discrimination of reactions between the CAC and FAC with Fe2+, which was applied to the speciation of FAC, CAC and TAC. The speciation of available chlorine species and chlorite (an oxychlorine species) was achieved by using the same set-up, but using flow streams of different pH. The effects of the pH of the carrier stream, the flow rate and the sample volume were studied. The method exhibited linearity from 2.8 x 10(-6) to 2.8 x 10(-4) M active chlorine (expressed as OCl-) with a detection limit of 1.4 x 10(-6) M. The selectivity of the method was studied by examining the minimum pH for the oxidation of iodide by other oxidants, and also by assessing the potentiometric selectivity coefficients. The proposed method was successfully applied to the determination of chlorine species in tap water, and disinfecting formulations where good agreement occurred between the proposed and standard methods were found.
  3. Badawy MEI, El-Nouby MAM, Kimani PK, Lim LW, Rabea EI
    Anal Sci, 2022 Dec;38(12):1457-1487.
    PMID: 36198988 DOI: 10.1007/s44211-022-00190-8
    Analytical processes involving sample preparation, separation, and quantifying analytes in complex mixtures are indispensable in modern-day analysis. Each step is crucial to enriching correct and informative results. Therefore, sample preparation is the critical factor that determines both the accuracy and the time consumption of a sample analysis process. Recently, several promising sample preparation approaches have been made available with environmentally friendly technologies with high performance. As a result of its many advantages, solid-phase extraction (SPE) is practiced in many different fields in addition to the traditional methods. The SPE is an alternative method to liquid-liquid extraction (LLE), which eliminates several disadvantages, including many organic solvents, a lengthy operation time and numerous steps, potential sources of error, and high costs. SPE advanced sorbent technology reorients with various functions depending on the structure of extraction sorbents, including reversed-phase, normal-phase, cation exchange, anion exchange, and mixed-mode. In addition, the commercial SPE systems are disposable. Still, with the continual developments, the restricted access materials (RAM) and molecular imprinted polymers (MIP) are fabricated to be active reusable extraction cartridges. This review will discuss all the theoretical and practical principles of the SPE techniques, focusing on packing materials, different forms, and performing factors in recent and future advances. The information about novel methodological and instrumental solutions in relation to different variants of SPE techniques, solid-phase microextraction (SPME), in-tube solid-phase microextraction (IT-SPME), and magnetic solid-phase extraction (MSPE) is presented. The integration of SPE with analytical chromatographic techniques such as LC and GC is also indicated. Furthermore, the applications of these techniques are discussed in detail along with their advantages in analyzing pharmaceuticals, biological samples, natural compounds, pesticides, and environmental pollutants, as well as foods and beverages.
  4. See WP, Heng LY, Nathan S
    Anal Sci, 2015;31(10):997-1003.
    PMID: 26460363 DOI: 10.2116/analsci.31.997
    A new approach for the development of a highly sensitive aluminium(III) ion sensor via the preconcentration of aluminium(III) ion with a self-assembled monolayer on a gold nanoparticles modified screen-printed carbon electrode and current mediation by potassium ferricyanide redox behavior during aluminium(III) ion binding has been attempted. A monolayer of mercaptosuccinic acid served as an effective complexation ligand for the preconcentration of trace aluminium; this led to an enhancement of aluminium(III) ion capture and thus improved the sensitivity of the sensor with a detection limit of down to the ppb level. Under the optimum experimental conditions, the sensor exhibited a wide linear dynamic range from 0.041 to 12.4 μM. The lower detection limit of the developed sensor was 0.037 μM (8.90 ppb) using a 10 min preconcentration time. The sensor showed excellent selectivity towards aluminium(III) ion over other interference ions.
  5. Saad B, Zin ZM, Jab MS, Rahman IA, Saleh MI, Mahsufi S
    Anal Sci, 2005 May;21(5):521-4.
    PMID: 15913140
    Poly (vinyl chloride) membrane electrodes that responded selectively towards the antimalarial drug chloroquine are described. The electrodes were based on the use of the lipophilic potassium tetrakis(4-chlorophenyl)borate as ion-exchanger and bis(2-ethylhexyl)adipate (BEHA), or trioctylphosphate (TOP) or dioctylphenylphosphonate (DOPP) as plasticizing solvent mediator. All electrodes produced good quality characteristics such as Nernstian- and rapid responses, and are minimally interfered with by the alkali and alkaline earth metal ions tested. The membranes were next applied to a flow-through device, enabling it to function as flow-injection analysis (FIA) detector. The performance of the sensor after undergoing the FIA optimization was further evaluated for its selectivity characteristics and lifetime. Results for the determination of chloroquine in synthetic samples that contained common tablet excipients such as glucose, starch, and cellulose, and other foreign species such as cations, citric acid or lactic acid were generally satisfactory. The sensor was also successfully used for the determination of the active ingredients in mock tablets, synthetic fluids and biological fluids. The sensor was applied for the determination of active ingredients and the dissolution profile of commercial tablets was also established.
  6. El-Nouby MAM, Lim LW
    Anal Sci, 2023 Dec;39(12):2019-2029.
    PMID: 37672170 DOI: 10.1007/s44211-023-00416-3
    This article describes the fabrication of porous nicotinic acid-functionalized chito-oligosaccharide-bonded titania/silica hybrid monoliths (TiO2/SiO2@ChO-N) through a co-gelation sol-gel process. A capillary monolith with a well-defined and homogeneous structure was obtained by controlling the hydrolysis speed of titanium alkoxides in a sol mixture by using glycerol and acetylacetone. As a result of the functionalization with chito-oligosaccharides (ChO)-modified nicotinic acid, the obtained stationary phase provides superior physiochemical properties, such as a cationic hydrophilic surface, porosity, and mechanical strength. Scanning electron microscope and attenuated total reflectance-infrared spectroscopy were used to characterize the functionalized monolithic columns. The produced capillary columns showed high chromatographic performance with acceptable selectivity for charged analytes as well as organic polar compounds such as nucleic bases, nucleosides, carbamate pesticides, and strobilurin fungicides. The obtained results also indicated that the functionalized ChO's amino, amide, hydroxyl, and pyridinium ring moieties served as hydrophilic electrostatic traps for charged substances, in addition to stroing π-π interaction with the carbamate pesticides and strobilurin fungicides analytes via hydrogen bonding.
  7. Chai M, Tan G, Lal A
    Anal Sci, 2008 Feb;24(2):273-6.
    PMID: 18270422
    A headspace solid-phase microextraction method has been developed for the determination of 8 pesticides in vegetables and fruits by using gas chromatography with an electron capture detector. Two types of fibers (polyacrylate, 85 microm and polydimethylsiloxane, 100 microm) have been assayed and compared. The main factors: extraction and desorption parameters, ionic strength, and the effects of dilution and organic solvents, were studied and optimized. The optimized procedures resulted in more than 80% recovery for all the investigated vegetable and fruit samples with RSD values below 10%.
  8. Windarsih A, Bakar NKA, Rohman A, Erwanto Y
    Anal Sci, 2024 Mar;40(3):385-397.
    PMID: 38095741 DOI: 10.1007/s44211-023-00470-x
    Due to the different price and high quality, halal meat such as beef can be adulterated with non-halal meat with low price to get an economical price. The objective of this research was to develop an analytical method for halal authentication testing of beef meatballs (BM) from dog meat (DM) using a non-targeted metabolomics approach employing liquid chromatography-high-resolution mass spectrometry (LC-HRMS) and chemometrics. The differentiation of authentic BM from that adulterated with DM was successfully performed using partial least square-discriminant analysis (PLS-DA) with high accuracy (R2X = 0.980, and R2Y = 0.980) and good predictivity (Q2 = 0.517). In addition, partial least square (PLS) and orthogonal PLS (OPLS) were successfully used to predict the DM added (% w/w) in BM with high accuracy (R2 > 0.990). A number of metabolites, potential for biomarker candidates, were identified to differentiate BM and that adulterated with DM. It showed that the combination of a non-targeted LC-HRMS Orbitrap metabolomics and chemometrics could detect up to 0.1% w/w of DM adulteration. The developed method was successfully applied for analysis of commercial meatball samples (n = 28). Moreover, pathway analysis revealed that beta-alanine, histidine, and ether lipid metabolism were significantly affected by dog meat adulteration. In summary, this developed method has great potential to be developed and used as an alternative method for analysis of non-halal meats in halal meat products.
  9. Lal A, Tan G, Chai M
    Anal Sci, 2008 Feb;24(2):231-6.
    PMID: 18270414
    A new extraction and cleanup procedure with gas chromatography was developed for the sensitive determination of acephate, dimethoate, malathion, diazinon, quinalphos, chlorpyrifos, profenofos, alpha-endosulfan, beta-endosulfan, chlorothalonil and carbaryl using 1-chloro-4-fluorobenzene as an internal standard in fruits and vegetables. Several extracting and eluting solvents for solid-phase extraction were investigated. The overall extracting solvent with a mixture of acetone:ethyl acetate:hexane (10:80:10, v/v/v) and a eluting solvent of 5% acetone in hexane used with the RPC18 cartridge gave the best recovery for all of the investigated pesticides, and minimized the interference from co-extractants. Under the optimal extraction and clean-up conditions, recoveries of 85 - 99% with RSD < 5.0% (n = 3) for most of the pesticides at the 0.02 - 0.5 mg/kg level were obtained. The limit of detection was between 0.005 - 0.01 mg/kg and the limit of quantification was 0.01 mg/kg. This analytical procedure was characterized with high accuracy and acceptable sensitivity to meet requirements for monitoring pesticides in crops.
  10. Hanifah SA, Heng LY, Ahmad M
    Anal Sci, 2009 Jun;25(6):779-84.
    PMID: 19531887
    Electrochemical biosensors for phenolic compound determination were developed by immobilization of tyrosinase enzyme in a series of methacrylic-acrylic based biosensor membranes deposited directly using a photocuring method. By modifying the hydrophilicity of the membranes using different proportions of 2-hydroxyethyl methacrylate (HEMA) and butyl acrylate (nBA), we developed biosensor membranes of different hydrophilic characters. The differences in hydrophilicity of these membranes led to changes in the sensitivity of the biosensors towards different phenolic compounds. In general biosensors constructed from the methacrylic-acrylic based membranes showed the poorest response to catechol relative to other phenolic compounds, which is in contrast to many other biosensors based on tyrosinase. The decrease in hydrophilicity of the membrane also allowed better selectivity towards chlorophenols. However, phenol biosensors constructed from the more hydrophilic membrane materials demonstrated better analytical performance towards phenol compared with those made from less hydrophilic ones. For the detection of phenols, these biosensors with different membranes gave detection limits of 0.13-0.25 microM and linear response range from 6.2-54.2 microM phenol. The phenol biosensors also showed good phenol recovery from landfill leachate samples (82-117%).
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