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A green solvent holder in electro-mediated microextraction for the extraction of phenols in water

Chong YT, Mohd Ariffin M, Mohd Tahir N, Loh SH

Talanta, 2018 Jan 01;176:558-564.
PMID: 28917790 DOI: 10.1016/j.talanta.2017.08.068

Electro-mediated microextraction (EMM) combined with micro-high performance liquid chromatography-ultraviolet detection was successfully developed for the determination of selected phenols, namely 4-chlorophenol (4CP), 2-nitrophenol (2NP) and 2,4-dichlorophenols (2,4 DCP) in water. A solvent-impregnated agarose gel disc was utilized as a solvent holder in this study. Under optimum extraction conditions, the method showed good linearity in the range of 0.1-250µgL-1, 0.3-250µgL-1and 0.2-500µgL-1for 4CP, 2NP and 2,4 DCP, respectively with correlation coefficients of ≥ 0.9975, ultra-trace LODs (0.03-0.1µgL-1) and satisfactory relative recovery average (85.0-114.1%) for the analysis of selected phenols. The proposed method was rapid and eco-friendly as the solvent holder was constructed using minute amounts of extraction solvent immobilized within the biodegradable agarose gel disc. A comparative microextraction technique termed solvent-impregnated agarose gel liquid phase microextraction (AG-LPME) was re-optimized and validated for the extraction of phenols in water. The method offered good linearity, ultra-trace LODs ranging 0.1-0.5µgL-1and satisfactory average of relative recovery (86.1-114.1%). The EMM was superior in terms of sensitivity and time-effectiveness compared to AG-LPME. Both techniques combine extraction and pre-concentration in mini-scaled approaches using an eco-friendly solvent holder that fulfil the green chemistry concept.

Matched MeSH terms: Limit of Detection
An Optical Biosensor based on Immobilization of Laccase and MBTH in Stacked Films for the Detection of Catechol

Abdullah J, Ahmad M, Heng LY, Karuppiah N, Sidek H

Sensors (Basel), 2007 Oct 11;7(10):2238-2250.
PMID: 28903224 DOI: 10.3390/s7102238

The fabrication of an optical biosensor by using stacked films where 3-methyl-2-benzothiazolinone hydrazone (MBTH) was immobilized in a hybrid nafion/sol-gelsilicate film and laccase in a chitosan film for the detection of phenolic compounds wasdescribed. Quinone and/or phenoxy radical product from the enzymatic oxidation ofphenolic compounds was allowed to couple with MBTH to form a colored azo-dye productfor spectrophometric detection. The biosensor demonstrated a linear response to catecholconcentration range of 0.5-8.0 mM with detection limit of 0.33 mM and response time of10 min. The reproducibility of the fabricated biosensor was good with RSD value of 5.3 %(n = 8) and stable for at least 2 months. The use of the hybrid materials of nafion/sol-gelsilicate to immobilize laccase has altered the selectivity of the enzyme to various phenoliccompounds such as catechol, guaicol, o-cresol and m-cresol when compared to the non-immobilized enzyme. When immobilized in this hybrid film, the biosensor response onlyto catechol and not other phenolic compounds investigated. Immobilization in this hybridmaterial has enable the biosensor to be more selective to catechol compared with the non-immobilized enzyme. This shows that by a careful selection of different immobilizationmatrices, the selectivity of an enzyme can be modified to yield a biosensor with goodselectivity towards certain targeted analytes.

Matched MeSH terms: Limit of Detection
Fulltext Colorimetric Approach for Nucleic Acid Salmonella spp. Detection: A Systematic Review

Ahmad Faris AN, Ahmad Najib M, Mohd Nazri MN, Hamzah ASA, Aziah I, Yusof NY, et al.

Int J Environ Res Public Health, 2022 Aug 25;19(17).
PMID: 36078284 DOI: 10.3390/ijerph191710570

Water- and food-related health issues have received a lot of attention recently because food-poisoning bacteria, in particular, are becoming serious threats to human health. Currently, techniques used to detect these bacteria are time-consuming and laborious. To overcome these challenges, the colorimetric strategy is attractive because it provides simple, rapid and accurate sensing for the detection of Salmonella spp. bacteria. The aim of this study is to review the progress regarding the colorimetric method of nucleic acid for Salmonella detection. A literature search was conducted using three databases (PubMed, Scopus and ScienceDirect). Of the 88 studies identified in our search, 15 were included for further analysis. Salmonella bacteria from different species, such as S. Typhimurium, S. Enteritidis, S. Typhi and S. Paratyphi A, were identified using the colorimetric method. The limit of detection (LoD) was evaluated in two types of concentrations, which were colony-forming unit (CFU) and CFU per mL. The majority of the studies used spiked samples (53%) rather than real samples (33%) to determine the LoDs. More research is needed to assess the sensitivity and specificity of colorimetric nucleic acid in bacterial detection, as well as its potential use in routine diagnosis.

Matched MeSH terms: Limit of Detection
Uricase biofunctionalized plasmonic sensor for uric acid detection with APTES-modified gold nanotopping

Onifade OA, Yusairie FA, Abu Bakar MH, Alresheedi MT, Khoon Ng E, Mahdi MA, et al.

Biosens Bioelectron, 2024 Oct 01;261:116486.
PMID: 38861811 DOI: 10.1016/j.bios.2024.116486

Current uric acid detection methodologies lack the requisite sensitivity and selectivity for point-of-care applications. Plasmonic sensors, while promising, demand refinement for improved performance. This work introduces a biofunctionalized sensor predicated on surface plasmon resonance to quantify uric acid within physiologically relevant concentration ranges. The sensor employs the covalent immobilization of uricase enzyme using 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-Hydroxysuccinimide (NHS) crosslinking agents, ensuring the durable adherence of the enzyme onto the sensor probe. Characterization through atomic force microscopy and Fourier transform infrared spectroscopy validate surface alterations. The Langmuir adsorption isotherm model elucidates binding kinetics, revealing a sensor binding affinity of 298.83 (mg/dL)-1, and a maximum adsorption capacity of approximately 1.0751°. The biofunctionalized sensor exhibits a sensitivity of 0.0755°/(mg/dL), a linear correlation coefficient of 0.8313, and a limit of detection of 0.095 mg/dL. Selectivity tests against potentially competing interferents like glucose, ascorbic acid, urea, D-cystine, and creatinine showcase a significant resonance angle shift of 1.1135° for uric acid compared to 0.1853° for interferents at the same concentration. Significantly, at a low uric acid concentration of 0.5 mg/dL, a distinct shift of 0.3706° was observed, setting it apart from the lower values noticed at higher concentrations for all typical interferent samples. The uricase enzyme significantly enhances plasmonic sensors for uric acid detection, showcasing a seamless integration of optical principles and biological recognition elements. These sensors hold promise as vital tools in clinical and point-of-care settings, offering transformative potential in biosensing technologies and the potential to revolutionize healthcare outcomes in biomedicine.

Matched MeSH terms: Limit of Detection
Fulltext Detection of Plasmodium knowlesi in whole blood samples with sandwich enzyme-linked immunosorbent assay (ELISA) using rhoptry-associated protein 1 specific polyclonal antibodies

Wan Nazri WSM, Ling LY, Wen CF

J Vector Borne Dis, 2024 Apr 01;61(2):203-210.
PMID: 38922654 DOI: 10.4103/jvbd.jvbd_55_23

BACKGROUND OBJECTIVES: Plasmodium knowlesi, a simian malaria species, is now known to infect humans. Due to disadvantages in the current diagnosis methods, many efforts have been placed into developing new methods to diagnose the disease. This study assessed the ability of the PkRAP-1 sandwich enzyme-linked immunosorbent (ELISA) to detect P knowlesi antigens in whole blood specimens.
METHODS: Western blot assay was conducted to evaluate the ability of raised mouse and rabbit anti-PkRAP-1 polyclonal antibodies to bind to the native proteins in P. knowlesi lysate. The polyclonal antibodies were then used in sandwich ELISA to detect P. knowlesi. In the sandwich ELISA, mouse and rabbit polyclonal antibodies were used as the capture and detection antibodies, respectively. The limit of detection (LOD) of the assay was determined using P. knowlesi A1H1 culture and purified recombinant PkRAP-1.
RESULTS: Western blot results showed positive reactions towards the proteins in P. knowlesi lysate. The LOD of the assay from three technical replicates was 0.068% parasitaemia. The assay performance in detecting P. knowlesi was 83% sensitivity and 70% specificity with positive and negative predictive values of 74% and 80%, respectively. The anti-PkRAP-1 polyclonal antibodies did not cross-react with P. falciparum and healthy samples, but P. vivax by detecting all 12 samples.
INTERPRETATION CONCLUSION: PkRAP-1 has the potential as a biomarker for the development of a new diagnostic tool for P. knowlesi detection. Further studies need to be conducted to establish the full potential of the usage of anti-PkRAP-1 antibodies for P. knowlesi detection.

Matched MeSH terms: Limit of Detection
Fulltext Flexible and highly selective NO2 gas sensor based on direct-ink-writing of eco-friendly graphene oxide for smart wearable application

Khan J, Rezo V, Vincze T, Weis M, Momin SA, El-Atab N, et al.

Chemosphere, 2024 Nov;367:143618.
PMID: 39490758 DOI: 10.1016/j.chemosphere.2024.143618

Nitrogen dioxide (NO2) is a major cause of respiratory disorders in outdoor and indoor environments. Real-time NO2 monitoring using nonintrusive wearable devices can save lives and provide valuable health data. This study reports a room-temperature, wearable, and flexible smart NO2 gas sensor fabricated via cost-effective printing technology on a polyimide substrate. The sensor uses alkali lignin with edge-oxidised graphene oxide (EGO-AL) ink, demonstrating a sensitivity of 1.70% ppm⁻1 and a detection limit of 12.70 ppb, with excellent selectivity towards NO2. The high sensing properties are attributed to labile oxygen functional groups from GO and alkali lignin, offering abundant interacting sites for NO2 adsorption and electron transfer. The sensor fully recovers to the baseline after heat treatment at 150 °C, indicating its reusability. Integration into lab coats showcased its wearable application, utilising a flexible printed circuit board to wirelessly alert the wearer via cell phone to harmful NO2 levels (>3 ppm) in the environment. This smart sensing application underscores the potential for practical, real-time air quality monitoring, personal safety enhancement, and health management.

Matched MeSH terms: Limit of Detection
Ultrasonic synthesis of CuO nanoflakes: A robust electrochemical scaffold for the sensitive detection of phenolic hazard in water and pharmaceutical samples

Hwa KY, Karuppaiah P, Gowthaman NSK, Balakumar V, Shankar S, Lim HN

Ultrason Sonochem, 2019 Nov;58:104649.
PMID: 31450344 DOI: 10.1016/j.ultsonch.2019.104649

Hydroquinone (HQ), a phenolic compound is expansively used in many industrial applications and due to the utilization of HQ, water pollution tragedies frequently found by the improper handling and accidental outflows. When HQ is adsorbed directly through the skin that create toxic effects to human by affecting kidney, liver, lungs, and urinary tract and hence, a highly selective and sensitive technique is required for its quantification. Herein, we have developed the ultrasonic synthesis of copper oxide nanoflakes (CuO-NFs) using ultrasonic bath (20 kHz, 100 W) and successfully employed for the sensitive detection of the environmental hazardous pollutant HQ. The formed CuO-NFs were confirmed by X-ray diffraction, field emission scanning electron microscopy (FE-SEM), FT-IR spectroscopy and UV-visible spectroscopy and fabricated with the screen-printed carbon electrode (SPCE). The SEM images exhibited the uniform CuO-NFs with an average width of 85 nm. The linker-free CuO-NFs fabricated electrode showed the appropriate wide range of concentrations from 0.1 to 1400 µM and the limit of detection was found to be 10.4 nM towards HQ. The fabricated sensor having long term stability and sensitivity was successfully applied for the environmental and commercial real sample analysis and exhibited good recovery percentage, implying that the SPCE/CuO-NFs is an economically viable and benign robust scaffold for the determination of HQ.

Matched MeSH terms: Limit of Detection*
Synthesis and characterization of cellulose and hydroxyapatite-carbon electrode composite for trace plumbum ions detection and its validation in blood serum

Ajab H, Dennis JO, Abdullah MA

Int J Biol Macromol, 2018 Jul 01;113:376-385.
PMID: 29486259 DOI: 10.1016/j.ijbiomac.2018.02.133

A novel synthesis and characterization of cellulose, hydroxyapatite and chemically-modified carbon electrode (Cellulose-HAp-CME) composite was reported for the analysis of trace Pb(II) ions detection and its validation in blood serum. The Field Emission Scanning Electron Microscopy (FESEM) analyses showed that the composite retained the orderly porous structure but with scattered particle size agglomeration. The Fourier Transform Infrared Spectroscopy (FTIR) spectra suggested the presence of functional groups associated with the bending and stretching of carbon bonds and intermolecular H-bonding. X-ray Diffraction (XRD) analyses further elucidated that the crystallite size could have influenced the properties of the electrode. Based on Thermo-gravimetric Analysis (TGA/DTG), the composites showed thermal stability with more than 60% residual content at 700°C. The sensor was successfully developed for trace Pb(II) ions detection in complex medium such as blood serum, in the physiologically relevant range of 10-60ppb, with resulting Limit of Detection (LOD) of 0.11±0.36ppb and Limit of Quantification (LOQ) of 0.36±0.36ppb. The newly fabricated electrode could be advantageous as a sensing platform with favourable electrochemical characteristics for robust, in situ and rapid environmental and clinical analyses of heavy metal ions.

Matched MeSH terms: Limit of Detection*
Sensitive Leptospira DNA detection using tapered optical fiber sensor

Zainuddin NH, Chee HY, Ahmad MZ, Mahdi MA, Abu Bakar MH, Yaacob MH

J Biophotonics, 2018 08;11(8):e201700363.
PMID: 29570957 DOI: 10.1002/jbio.201700363

This paper presents the development of tapered optical fiber sensor to detect a specific Leptospira bacteria DNA. The bacteria causes Leptospirosis, a deadly disease but with common early flu-like symptoms. Optical single mode fiber (SMF) of 125 μm diameter is tapered to produce 12 μm waist diameter and 15 cm length. The novel DNA-based optical fiber sensor is functionalized by incubating the tapered region with sodium hydroxide (NaOH), (3-Aminopropyl) triethoxysilane and glutaraldehyde. Probe DNA is immobilized onto the tapered region and subsequently hybridized by its complementary DNA (cDNA). The transmission spectra of the DNA-based optical fiber sensor are measured in the 1500 to 1600 nm wavelength range. It is discovered that the shift of the wavelength in the SMF sensor is linearly proportional with the increase in the cDNA concentrations from 0.1 to 1.0 nM. The sensitivity of the sensor toward DNA is measured to be 1.2862 nm/nM and able to detect as low as 0.1 fM. The sensor indicates high specificity when only minimal shift is detected for non-cDNA testing. The developed sensor is able to distinguish between actual DNA of Leptospira serovars (Canicola and Copenhageni) against Clostridium difficile (control sample) at very low (femtomolar) target concentrations.

Matched MeSH terms: Limit of Detection*
Simultaneous electrochemical determination of DNA nucleobases using AgNPs embedded covalent organic framework

Arul P, Huang ST, Gowthaman NSK, Shankar S

Mikrochim Acta, 2021 Oct 01;188(10):358.
PMID: 34596766 DOI: 10.1007/s00604-021-05021-7

An efficient electrochemical biosensor has been developed for the simultaneous evaluation of DNA bases using AgNPs-embedded covalent organic framework (COF). The COF (p-Phenylenediamine and terephthalaldehyde) was synthesized by reflux (DMF; 150 °C; 12 h) and the nanoparticles were embedded from the aqueous solutions of AgNO3 and NaBH4. The nanocomposite-modified COF was confirmed by spectral, microscopic, and electrochemical techniques. The nanocomposite material was deposited on a glassy carbon electrode (GCE) and the redox behavior of AgNPs was confirmed by cyclic voltammetry. The electrocatalytic activities of DNA bases were analyzed by differential pulse voltammetry (DPV) in a physiological environment (PBS; pH = 7.0) based on simple and easy-to-use electrocatalyst. The AgNPs-COF/GCE showed well-defined anodic peak currents for the bases guanine (+ 0.63 V vs. Ag/AgCl), adenine (+ 0.89 V vs. Ag/AgCl), thymine (+ 1.10 V vs. Ag/AgCl), and cytosine (+ 1.26 V vs. Ag/AgCl) in a mixture as well as individuals with respect to the conventional, COF, and AgNPs/GCEs. The AgNPs-COF/GCE showed linear concentration range of DNA bases from 0.2-1000 µM (guanine; (G)), 0.1-500 µM (adenine (A)), 0.25-250 µM (thymine (T)) and 0.15-500 µM (cytosine (C)) and LOD of 0.043, 0.056, 0.062, and 0.051 µM (S/N = 3), respectively. The developed sensor showed reasonable selectivity, reproducibility (RSD = 1.53 ± 0.04%-2.58 ± 0.02% (n = 3)), and stability (RSD = 1.22 ± 0.06%-2.15 ± 0.04%; n = 3) over 5 days of storage) for DNA bases. Finally, AgNPs-COF/GCE was used for the determination of DNA bases in human blood serum, urine and saliva samples with good recoveries (98.60-99.11%, 97.80-99.21%, and 98.69-99.74%, respectively).

Matched MeSH terms: Limit of Detection*
Carbonaceous nanomaterials immobilised mixed matrix membrane microextraction for the determination of polycyclic aromatic hydrocarbons in sewage pond water samples

Mukhtar NH, See HH

Anal Chim Acta, 2016 08 10;931:57-63.
PMID: 27282751 DOI: 10.1016/j.aca.2016.04.032

In this study, the potential for carbonaceous nanomaterials to be used as adsorbents for the mixed matrix membrane (MMM) microextraction and preconcentration of organic pollutants was demonstrated. For this method, multiwall carbon nanotubes (MWCNT) and single layer graphene (SLG) nanoparticles were individually incorporated through dispersion in a cellulose triacetate (CTA) polymer matrix to form a MWCNT-MMM and SLG-MMM, respectively. The prepared membranes were evaluated for the extraction of selected polycyclic aromatic hydrocarbons (PAHs) present in sewage pond water samples. The extraction was performed by dipping a small piece of membrane (7 mm × 7 mm) in a stirred 7.5 mL sample solution to initiate the analyte adsorption. This step was followed by an analyte desorption into 60 μL of methanol prior to high performance liquid chromatography (HPLC) analysis. When the optimum SLG-MMM microextraction technique was applied to spiked sewage pond water samples, the detection limit of the method for the PAHs were in the range of 0.02-0.09 ng/mL, with relative standard deviations of between 1.4% and 7.8%. Enrichment factors of 54-100 were achieved with relative recoveries of 99%-101%. A comparison was also made between the proposed approach and standard solid phase extraction using polymeric bonded octadecyl (C18) cartridges.

Matched MeSH terms: Limit of Detection
Facile hydrothermal growth graphene/ZnO nanocomposite for development of enhanced biosensor

Low SS, Tan MT, Loh HS, Khiew PS, Chiu WS

Anal Chim Acta, 2016 Jan 15;903:131-41.
PMID: 26709306 DOI: 10.1016/j.aca.2015.11.006

Graphene/zinc oxide nanocomposite was synthesised via a facile, green and efficient approach consisted of novel liquid phase exfoliation and solvothermal growth for sensing application. Highly pristine graphene was synthesised through mild sonication treatment of graphite in a mixture of ethanol and water at an optimum ratio. The X-ray diffractometry (XRD) affirmed the hydrothermal growth of pure zinc oxide nanoparticles from zinc nitrate hexahydrate precursor. The as-prepared graphene/zinc oxide (G/ZnO) nanocomposite was characterised comprehensively to evaluate its morphology, crystallinity, composition and purity. All results clearly indicate that zinc oxide particles were homogenously distributed on graphene sheets, without any severe aggregation. The electrochemical performance of graphene/zinc oxide nanocomposite-modified screen-printed carbon electrode (SPCE) was evaluated using cyclic voltammetry (CV) and amperometry analysis. The resulting electrode exhibited excellent electrocatalytic activity towards the reduction of hydrogen peroxide (H2O2) in a linear range of 1-15 mM with a correlation coefficient of 0.9977. The sensitivity of the graphene/zinc oxide nanocomposite-modified hydrogen peroxide sensor was 3.2580 μAmM(-1) with a limit of detection of 7.4357 μM. An electrochemical DNA sensor platform was then fabricated for the detection of Avian Influenza H5 gene based on graphene/zinc oxide nanocomposite. The results obtained from amperometry study indicate that the graphene/zinc oxide nanocomposite-enhanced electrochemical DNA biosensor is significantly more sensitive (P

Matched MeSH terms: Limit of Detection
New chrysin-functionalized silica-core shell magnetic nanoparticles for the magnetic solid phase extraction of copper ions from water samples

Abd Ali LI, Ibrahim WA, Sulaiman A, Kamboh MA, Sanagi MM

Talanta, 2016 Feb 1;148:191-9.
PMID: 26653440 DOI: 10.1016/j.talanta.2015.10.062

This study describes the synthesis, characterization and application of a new chrysin-based silica core-shell magnetic nanoparticles (Fe3O4@SiO2-N-chrysin) as an adsorbent for the preconcentration of Cu(II) from aqueous environment. The morphology, thermal stability and magnetic property of Fe3O4@SiO2-N-chrysin were analyzed using FTIR, FESEM, TEM, XRD, thermal analysis and VSM. The extraction efficiency of Fe3O4@SiO2-N-chrysin was analyzed using the batch wise method with flame atomic absorption spectrometry. Parameters such as the pH, the sample volume, the adsorption-desorption time, the concentration of the desorption solvent, the desorption volume, the interference effects and the regeneration of the adsorbent were optimized. It was determined that Cu(II) adsorption is highly pH-dependent, and a high recovery (98%) was achieved at a pH 6. The limit of detection (S/N=3), the limit of quantification (S/N=10), the preconcentration factor and the relative standard deviation for Cu(II) extraction were 0.3 ng mL(-1), 1 ng mL(-1), 100 and 1.9% (concentration=30 ng mL(-1), n=7), respectively. Excellent relative recoveries of 97-104% (%RSD<3.12) were achieved from samples from a spiked river, a lake and tap water. The MSPE method was also validated using certified reference materials SLRS-5 with good recovery (92.53%).

Matched MeSH terms: Limit of Detection
Utilization of reduced graphene oxide/cadmium sulfide-modified carbon cloth for visible-light-prompt photoelectrochemical sensor for copper (II) ions

Foo CY, Lim HN, Pandikumar A, Huang NM, Ng YH

J Hazard Mater, 2016 Mar 5;304:400-8.
PMID: 26595899 DOI: 10.1016/j.jhazmat.2015.11.004

A newly developed CdS/rGO/CC electrode was prepared based on a flexible carbon cloth (CC) substrate with cadmium sulfide (CdS) nanoparticles and reduced graphene oxide (rGO). The CdS was synthesized using an aerosol-assisted chemical vapor deposition (AACVD) method, and the graphene oxide was thermally reduced on the modified electrode surface. The existence of rGO in the CdS-modified electrode increased the photocurrent intensity of the CdS/rGO/CC-modified electrode by three orders of magnitude, compared to that of the CdS/ITO electrode and two orders of magnitude higher than the CdS/CC electrode. A new visible-light-prompt photoelectrochemical sensor was developed based on the competitive binding reaction of Cu(2+) and CdS on the electrode surface. The results showed that the effect of the Cu(2+) on the photocurrent response was concentration-dependent over the linear ranges of 0.1-1.0 μM and 1.0-40.0 μM with a detection limit of 0.05 μM. The results of a selectivity test showed that this modified electrode has a high response toward Cu(2+) compared to other heavy metal ions. The proposed CdS/rGO/CC electrode provided a significantly high potential current compared to other reported values, and could be a practical tool for the fast, sensitive, and selective determination of Cu(2+).

Matched MeSH terms: Limit of Detection
Novel solid-phase membrane tip extraction and gas chromatography with mass spectrometry methods for the rapid analysis of triazine herbicides in real waters

Sanagi MM, Muhammad SS, Hussain I, Ibrahim WA, Ali I

J Sep Sci, 2015 Feb;38(3):433-8.
PMID: 25421899 DOI: 10.1002/jssc.201400912

Novel, fast, selective, eco-friendly and reproducible solid-phase membrane tip extraction and gas chromatography with mass spectrometry methods were developed and validated for the analysis of triazine herbicides (atrazine and secbumeton) in stream and lake waters. The retention times of atrazine and secbumeton were 7.48 and 8.51 min. The solid-phase membrane tip extraction was carried out in semiautomated dynamic mode on multiwall carbon nanotubes enclosed in a cone-shaped polypropylene membrane cartridge. Acetone and methanol were found as the best preconditioning and desorption solvents, respectively. The extraction and desorption times for these herbicides were 15.0 and 10.0 min, respectively. The percentage recoveries of atrazine and secbumeton were 88.0 and 99.0%. The linearity range was 0.50-80.0 μg/L (r(2) > 0.994), with detection limits (<0.47 μg/L, S/N = 3) and good reproducibility (<8.0%). The ease of operation, eco-friendly nature, and low cost of solid-phase membrane tip extraction made these methods novel. The Solid-phase membrane tip extraction method was optimized by considering the effect of extraction time, desorbing solvents and time.

Matched MeSH terms: Limit of Detection
Fulltext Screen Printed Carbon Electrode Based Electrochemical Immunosensor for the Detection of Dengue NS1 Antigen

Parkash O, Yean CY, Shueb RH

Diagnostics (Basel), 2014;4(4):165-80.
PMID: 26852684 DOI: 10.3390/diagnostics4040165

An electrochemical immunosensor modified with the streptavidin/biotin system on screen printed carbon electrodes (SPCEs) for the detection of the dengue NS1 antigen was developed in this study. Monoclonal anti-NS1 capture antibody was immobilized on streptavidin-modified SPCEs to increase the sensitivity of the assay. Subsequently, a direct sandwich enzyme linked immunosorbent assay (ELISA) format was developed and optimized. An anti-NS1 detection antibody conjugated with horseradish peroxidase enzyme (HRP) and 3,3,5,5'-tetramethybezidine dihydrochloride (TMB/H₂O₂) was used as an enzyme mediator. Electrochemical detection was conducted using the chronoamperometric technique, and electrochemical responses were generated at -200 mV reduction potential. The calibration curve of the immunosensor showed a linear response between 0.5 µg/mL and 2 µg/mL and a detection limit of 0.03 µg/mL. Incorporation of a streptavidin/biotin system resulted in a well-oriented antibody immobilization of the capture antibody and consequently enhanced the sensitivity of the assay. In conclusion, this immunosensor is a promising technology for the rapid and convenient detection of acute dengue infection in real serum samples.

Matched MeSH terms: Limit of Detection
Validation of a HPLC method for determination of hydroxymethylfurfural in crude palm oil

Ariffin AA, Ghazali HM, Kavousi P

Food Chem, 2014 Jul 1;154:102-7.
PMID: 24518321 DOI: 10.1016/j.foodchem.2013.12.082

For the first time 5-hydroxymethyl-2-furaldehyde (HMF) was separated from crude palm oil (CPO), and its authenticity was determined using an RP-HPLC method. Separation was accomplished with isocratic elution of a mobile phase comprising water and methanol (92:8 v/v) on a Purospher Star RP-18e column (250mm×4.6mm, 5.0μm). The flow rate was adjusted to 1ml/min and detection was performed at 284nm. The method was validated, and results obtained exhibit a good recovery (95.58% to 98.39%). Assessment of precision showed that the relative standard deviations (RSD%) of retention times and peak areas of spiked samples were less than 0.59% and 2.66%, respectively. Further, the limit of detection (LOD) and LOQ were 0.02, 0.05mg/kg, respectively, and the response was linear across the applied ranges. The crude palm oil samples analysed exhibited HMF content less than 2.27mg/kg.

Matched MeSH terms: Limit of Detection
Development and validation of an ion-pair chromatographic method for simultaneous determination of trans- and cis-urocanic acid in fish samples

Zare D, Muhammad K, Bejo MH, Ghazali HM

J Chromatogr A, 2012 Sep 21;1256:144-9.
PMID: 22885043 DOI: 10.1016/j.chroma.2012.07.083

Urocanic acid (UCA) has been reported to be a mast cell degranulator and has also been suggested as a complementary agent in implicated scombroid fish poisoning. In this research, a new method is described to extract, clean up and perform simultaneous ion-pair chromatographic analysis of trans- and cis-urocanic acid (UCA) in fish samples. UCA was extracted using 0.05 M HCl and protein was removed from the extract by precipitation with 10% trisodium citrate and 10% citric acid. The HPLC method that is developed showed a rapid, precise and sensitive method with short retention time for simultaneous separation of UCA isomers in fish samples. Estimation of trans- and cis-UCA in the muscle of Indian mackerel, tuna and sardine showed that, as expected, no cis-UCA existed in fish muscles and the highest concentration of trans-UCA was found in Indian mackerel with 118.8 mg kg(-1) while the highest concentrations of trans-UCA in tuna and sardine were 12.1 and 17.5 mg kg(-1), respectively.

Matched MeSH terms: Limit of Detection
Solid phase microextraction using new sol-gel hybrid polydimethylsiloxane-2-hydroxymethyl-18-crown-6-coated fiber for determination of organophosphorous pesticides

Wan Ibrahim WA, Farhani H, Sanagi MM, Aboul-Enein HY

J Chromatogr A, 2010 Jul 23;1217(30):4890-7.
PMID: 20561627 DOI: 10.1016/j.chroma.2010.05.050

A new sol-gel hybrid coating, polydimethylsiloxane-2-hydroxymethyl-18-crown-6 (PDMS-2OHMe18C6) was prepared in-house for use in solid phase microextraction (SPME). The three compositions produced were assessed for its extraction efficiency towards three selected organophosphorus pesticides (OPPs) based on peak area extracted obtained from gas chromatography with electron capture detection. All three compositions showed superior extraction efficiencies compared to commercial 100 microm PDMS fiber. The composition showing best extraction performance was used to obtain optimized SPME conditions: 75 degrees C extraction temperature, 10 min extraction time, 120 rpm stirring rate, desorption time 5 min, desorption temperature 250 degrees C and 1.5% (w/v) of NaCl salt addition. The method detection limits (S/N=3) of the OPPs with the new sol-gel hybrid material ranged from 4.5 to 4.8 ng g(-1), which is well below the maximum residue limit set by Codex Alimentarius Commission and European Commission. Percentage recovery of OPPs from strawberry, green apple and grape samples with the new hybrid sol-gel SPME material ranged from 65 to 125% with good precision of the method (%RSD) ranging from 0.3 to 7.4%.

Matched MeSH terms: Limit of Detection
HPLC method development and validation for simultaneous detection of Arabinoside-C and doxorubicin

Mistiran AF, Dzarr AA, Gan SH

Toxicol. Mech. Methods, 2010 Oct;20(8):472-81.
PMID: 20626302 DOI: 10.3109/15376516.2010.503246

This paper describes a new validated high performance liquid chromatography (HPLC) method for the simultaneous determination of two anti-cancer drugs, Arabinoside-C (Ara-C) and doxorubicin hydrochloride (DOX). A simultaneous determination method saves cost and time as both drugs can be injected into a single HPLC system without the need to change or re-equilibrate with a new mobile phase. The objective of the study is to develop a simultaneous determination method of two anti-cancer drugs, Ara-C and DOX. The mobile phase consisted of a mixture (45:55) of acetonitrile:ammonium hydrogen phosphate aqueous solution (0.01 M) at pH 6.2 at a flow rate of 0.3 ml/min, with UV detection at 252 nm. Separation was achieved on a C-18 column (5 µm: 250 mm × 4.6 mm) maintained at 30°C in a column oven. The method was linear between 325 ng/ml and 10 µg/ml for Ara-C and 625 ng/ml and 20 µg/ml for DOX. The limit of detection (LOD) was 20 ng/ml for Ara-C and 60 ng/ml for DOX. The developed HPLC method achieved good precision and accuracy as well as limit of quantitations. The developed and validated method is suitable to be used for routine analysis of Ara-C and DOX.

Matched MeSH terms: Limit of Detection

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