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Liquid chromatography-high-resolution mass spectrometry analysis of erectile dysfunction drugs and their analogues in food products

Mohd Yusop AY, Xiao L, Fu S

Forensic Sci Int, 2021 May;322:110748.
PMID: 33711768 DOI: 10.1016/j.forsciint.2021.110748

The presence of erectile dysfunction (ED) drugs in adulterated dietary supplements, mainly in pharmaceutical dosage forms, is frequently addressed in the literature. Little attention is given to food products despite their increasing adulteration trend. To address this knowledge gap targeted, suspected-target, and non-targeted strategies were utilised to analyse ED drugs and their analogues in powdered drink mix (PDM), honey, jelly, hard candy, and sugar-coated chewing gum using liquid chromatography-high-resolution mass spectrometry (LC-HRMS). The method was optimised and validated using 23 target analytes, representing different ED drugs with structural similarities. The modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction exhibited insignificant matrix effect (ME) within - 9.2-8.8% and provided complete coverage of target analytes with acceptable extraction recovery (RE) within 75.5-123.9%, except for carbodenafil in the PDM matrix. Based on the ME and RE performance, the analytical method was validated to analyse 25 food samples that claimed to enhance male sexual performance. The method exhibited good specificity and linearity with a limit of detection within 10-70 ng/mL and limit of quantification of 80 ng/mL. Similarly, the accuracy and precision were satisfactory within 77.4-122.0% and

Matched MeSH terms: Limit of Detection
RP-HPLC analytical method development and optimization for quantification of donepezil hydrochloride in orally disintegrating tablet

Liew KB, Peh KK, Fung Tan YT

Pak J Pharm Sci, 2013 Sep;26(5):961-6.
PMID: 24035953

An easy, fast and validated RV-HPLC method was invented to quantify donepezil hydrochloride in drug solution and orally disintegrating tablet. The separation was carried out using reversed phase C-18 column (Agilent Eclipse Plus C-18) with UV detection at 268 nm. Method optimization was tested using various composition of organic solvent. The mobile phase comprised of phosphate buffer (0.01M), methanol and acetonitrile (50:30:20, v/v) adjusted to pH 2.7 with phosphoric acid (80%) was found as the optimum mobile phase. The method showed intraday precision and accuracy in the range of 0.24% to -1.83% and -1.83% to 1.99% respectively, while interday precision and accuracy ranged between 1.41% to 1.81% and 0.11% to 1.90% respectively. The standard calibration curve was linear from 0.125 μg/mL to 16 μg/mL, with correlation coefficient of 0.9997±0.00016. The drug solution was stable under room temperature at least for 6 hours. System suitability studies were done. The average plate count was > 2000, tailing factor <1, and capacity factor of 3.30. The retention time was 5.6 min. The HPLC method was used to assay donepezil hydrochloride in tablet and dissolution study of in-house manufactured donepezil orally disintegrating tablet and original Aricept.

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
Solid-phase extraction of non-steroidal anti-inflammatory drugs in human plasma and water samples using sol-gel-based metal-organic framework coating

Amiri A, Ghaemi F

J Chromatogr A, 2021 Jul 05;1648:462168.
PMID: 33984648 DOI: 10.1016/j.chroma.2021.462168

In this research, the Cu-based metal-organic framework (MOF-199) was fabricated and coated on the stainless steel mesh as substrates through sol-gel procedure. Then the coated substrates were placed in a small column known as solid-phase extraction cartridge. The SPE based coated stainless steel mesh coupled with high-performance liquid chromatography-UV detector (HPLC-UV) was used for the fast extraction, and quantification of non-steroidal anti-inflammatory drugs (NSAIDs) from human plasma and water samples. To find optimum extraction conditions, the impacts of effective parameters on analytical performance like sample pH, sample volume, type, and volume of desorption solvent were optimized. At the optimized conditions, calibration graphs of analytes were linear in the concentration range of 0.03-300 ng mL-1 for water samples, and 0.1-200 ng mL-1 for plasma samples. The correlation coefficients were in the range of 0.9938 to 0.9989. Also, the limits of detection (LODs) were from 0.01 to 0.02 ng mL-1 for water samples and 0.03 to 0.1 ng mL-1 for plasma samples. The cartridge repeatability was studied at different values, and the relative standard deviations (RSDs%) were achieved between 3.5 and 5.1%. Consequently, this procedure was successfully used in the extraction and detection of NSAIDs in real water and plasma samples with relative recoveries ranged from 93.6 to 99.6%.

Matched MeSH terms: Limit of Detection
Magnetized graphene layers synthesized on the carbon nanofibers as novel adsorbent for the extraction of polycyclic aromatic hydrocarbons from environmental water samples

Rezvani-Eivari M, Amiri A, Baghayeri M, Ghaemi F

J Chromatogr A, 2016 Aug 16.
PMID: 27578405 DOI: 10.1016/j.chroma.2016.08.034

The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis.

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
Fulltext Hummingbird-Leaves-Reared Black Soldier Fly Prepupae: Assessment of Nutritional and Heavy Metal Compositions

Kuppusamy G, Kong CK, Segaran GC, Tarmalingam E, Herriman M, Ismail MF, et al.

Biology (Basel), 2020 Sep 05;9(9).
PMID: 32899563 DOI: 10.3390/biology9090274

Black soldier fly (BSF) larva is an attractive animal feed replacer due to its noticeable nutritional content. However, the conventional rearing method often resulted in BSF with undesirably high heavy metal residues that are harmful to animals. In this work, putrefied Sesbania grandiflora (S. Grandiflora) leaves were employed as feed to rear BSF larvae. The resultant BSF prepupae were found to contain 43.5% protein and 16.7% fat, reflecting a comparable protein content and a 2-fold reduction in crude fat than those reared using conventional kitchen waste. Moreover, high quantities of arginine (25.4 g/kg dry matter basis (DM)), carnitine (32.9 g/kg DM), and short-chain fatty acids, including lauric (40.00%), palmitic (19.20%), and oleic (12.10%) acids, have also been noticed in the BSF prepupae. Furthermore, the BSF larvae have been recorded with 0.185 mg/kg chromium, 0.380 mg/kg selenium, and mercury below the detection limit, which is far lower than those reared using conventional kitchen and agricultural wastes (≈1.7 mg/kg chromium, 1.2 mg/kg selenium, and 0.2 mg/kg mercury). Overall, the study shows that the nutritional quality of BSF prepupae is extensively improved when using S. Grandiflora as their feed. The resultant BSF prepupae may serve as an alternative feed for animal rearing.

Matched MeSH terms: Limit of Detection
Fulltext Quantification of cortisol for the medical diagnosis of multiple pregnancy-related diseases

Zhang J, Gopinath SCB

3 Biotech, 2020 Feb;10(2):35.
PMID: 31988829 DOI: 10.1007/s13205-019-2030-z

Cortisol is a stress hormone released from the adrenal glands and is responsible for both hyperglycemia and hypertension during pregnancy. These factors make it mandatory to detect the levels of cortisol during pregnancy to identify and treat hypoglycemia and hypertension. In this study, cortisol levels were quantified with an aptamer-conjugated gold nanorod using an electrochemical interdigitated electrode sensor. The surface uniformity was analyzed by high-power microscopy and 3D-nanoprofiler imaging. The detection limit was determined to be 0.01 ng/mL, and a linear regression indicated that the sensitivity range was in the range of 0.01-0.1 ng/mL, based on a 3σ calculation. Moreover, the specificity of the aptamer was determined by a binding analysis against norepinephrine and progesterone, and it was clearly found that the aptamer specifically recognizes only cortisol. Further, the presence of cortisol was detected in the serum in a dose-dependent manner. This method is useful to detect and correlate multiple pregnancy-related diseases by quantifying the levels of cortisol.

Matched MeSH terms: Limit of Detection
Gold-nanorod enhances dielectric voltammetry detection of c-reactive protein: A predictive strategy for cardiac failure

Letchumanan I, Md Arshad MK, Balakrishnan SR, Gopinath SCB

Biosens Bioelectron, 2019 Apr 01;130:40-47.
PMID: 30716591 DOI: 10.1016/j.bios.2019.01.042

This paper primarily demonstrates the approach to enhance the sensing performance on antigen C-reactive protein (CRP) and anti-CRP antibody binding event. A nanogapped electrode structure with the gap of ~100 nm was modified by the anti-CRP antibody (Probe) to capture the available CRP. In order to increase the amount of antigen to be captured, a gold nanorod with 119 nm in length and 25 nm in width was integrated, to increase the surface area. A comparative study between the existence and non-existence of gold nanorod utilization was evaluated. Analysis of the sensing surface was well-supported by atomic force microscopy, scanning electron microscopy, 3D nano-profilometry, high-power microscopy and UV-Vis spectroscopy. The dielectric voltammetric analysis was carried out from 0 V to 2 V. The sensitivity was calculated based on 3σ and attained as low as 1 pM, which is tremendously low compared to real CRP concentration (119 nM) in human blood serum. The gold nanorod conjugation with antibody has enhanced the sensitivity to 100 folds (10 fM). The specificity of the CRP detection by the proposed strategy was anchored by ELISA and failure in the detection of human blood clotting factor IX by voltammetry. Despite, CRP antigen was further detected in human serum by spiking CRP to run-through the detection with the physiologically relevant samples.

Matched MeSH terms: Limit of Detection
Fulltext Diagnostic accuracy and limit of detection of ten malaria parasite lactate dehydrogenase-based rapid tests for Plasmodium knowlesi and P. falciparum

Tan AF, Sakam SSB, Rajahram GS, William T, Abd Rachman Isnadi MF, Daim S, et al.

Front Cell Infect Microbiol, 2022;12:1023219.
PMID: 36325471 DOI: 10.3389/fcimb.2022.1023219

BACKGROUND: Plasmodium knowlesi causes zoonotic malaria across Southeast Asia. First-line diagnostic microscopy cannot reliably differentiate P. knowlesi from other human malaria species. Rapid diagnostic tests (RDTs) designed for P. falciparum and P. vivax are used routinely in P. knowlesi co-endemic areas despite potential cross-reactivity for species-specific antibody targets.
METHODS: Ten RDTs were evaluated: nine to detect clinical P. knowlesi infections from Malaysia, and nine assessing limit of detection (LoD) for P. knowlesi (PkA1-H.1) and P. falciparum (Pf3D7) cultures. Targets included Plasmodium-genus parasite lactate dehydrogenase (pan-pLDH) and P. vivax (Pv)-pLDH.
RESULTS: Samples were collected prior to antimalarial treatment from 127 patients with microscopy-positive PCR-confirmed P. knowlesi mono-infections. Median parasitaemia was 788/µL (IQR 247-5,565/µL). Pan-pLDH sensitivities ranged from 50.6% (95% CI 39.6-61.5) (SD BIOLINE) to 87.0% (95% CI 75.1-94.6) (First Response® and CareStart™ PAN) compared to reference PCR. Pv-pLDH RDTs detected P. knowlesi with up to 92.0% (95% CI 84.3-96.7%) sensitivity (Biocredit™). For parasite counts ≥200/µL, pan-pLDH (Standard Q) and Pv-pLDH RDTs exceeded 95% sensitivity. Specificity of RDTs against 26 PCR-confirmed negative controls was 100%. Sensitivity of six highest performing RDTs were not significantly different when comparing samples taken before and after (median 3 hours) antimalarial treatment. Parasite ring stages were present in 30% of pre-treatment samples, with ring stage proportions (mean 1.9%) demonstrating inverse correlation with test positivity of Biocredit™ and two CareStart™ RDTs.For cultured P. knowlesi, CareStart™ PAN demonstrated the lowest LoD at 25 parasites/µL; LoDs of other pan-pLDH ranged from 98 to >2000 parasites/µL. Pv-pLDH LoD for P. knowlesi was 49 parasites/µL. No false-positive results were observed in either P. falciparum-pLDH or histidine-rich-protein-2 channels.
CONCLUSION: Selected RDTs demonstrate sufficient performance for detection of major human malaria species including P. knowlesi in co-endemic areas where microscopy is not available, particularly for higher parasite counts, although cannot reliably differentiate among non-falciparum malaria.

Matched MeSH terms: Limit of Detection
A lead(II) ion selective electrode via a metal complex of poly(hydroxamic acid)

Anuar K, Hamdan S

Talanta, 1992 Dec;39(12):1653-6.
PMID: 18965586

A new lead(II) electrode has been constructed with poly(hydroxamic acid) (PHXA) as the active material and silicone rubber as the supporting material. The electrode gave near Nerstian response over the concentration range 4 x 10(-5)-1 x 10(-2)M lead(II). The detection limit of the electrode is approximately 4 x 10(-6)M and the electrode works well in the pH range 4.5-6.0. The response time was 50-120 sec over the whole concentration range and the electrode has a working life of at least 4 weeks. Iron(III) severely poisoned the electrode membrane. Nickel(II) and mercury(II) gave very strong interference compared to copper(II), silver(I), cobalt(II), sodium(I), potassium(I), zinc(II) and cadmium(II) which gave some or little interference. Values determined with atomic absorption (AAS) and a commercial lead(II) electrode were in good agreement with those measured with the lead(II) electrode reported here.

Matched MeSH terms: Limit of Detection
Rapid ultrasound assisted emulsification micro-solid phase extraction based on molecularly imprinted polymer for HPLC-DAD determination of bisphenol A in aqueous matrices

Rozaini MNH, Yahaya N, Saad B, Kamaruzaman S, Hanapi NSM

Talanta, 2017 Aug 15;171:242-249.
PMID: 28551135 DOI: 10.1016/j.talanta.2017.05.006

Molecularly imprinted polymer (MIP) was employed as sorbent in ultrasound assisted emulsification molecularly imprinted polymer micro-solid phase extraction (USAE-MIP-µ-SPE) of bisphenol A (BPA) in water, beverages and the aqueous liquid in canned foods prior to high performance liquid chromatography-diode array detector (HPLC-DAD) analysis. Several effective variables, such as types of emulsification solvent and its volume, types of desorption solvent and its volume, salting out effect, pH of sample solution, mass of sorbent, extraction and desorption time, and sample volume, were optimized comprehensively. Under the optimized USAE-MIP-µ-SPE and HPLC-DAD conditions, the method demonstrated good linearity over the range of 0.5-700μgL-1with a coefficient determination of R2=0.9973, low limit of detection (0.07μgL-1), good analyte recoveries (82.2-118.9%) and acceptable RSDs (0.7-14.2%, n=3) with enrichment factor of 49. The method was applied to thirty samples of drinking water, mineral water, river water, lake water, as well as beverages and canned foods, the presence of BPA was identified in four samples. The proposed method showed good selectivity and reusability for extraction of BPA, and hence the USAE-MIP-µ-SPE is rapid, simple, cost effective and environmentally friendly.

Matched MeSH terms: Limit of Detection
Fulltext Determination of acrylamide in banana based snacks by gas chromatography-mass spectrometry

Daniali, G., Jinap, S., Zaidul, S.I.M., Hanifah, N.L.

International Food Research Journal, 2010;17(2):433-439.
MyJurnal

Fried and baked banana-based snacks are popular in South East Asia and banana chip is popular in
other countries, such as India, Indonesia, China, African countries, etc; these snacks may contain acrylamide in concentration which may be of concern due to its toxicity. This study was carried out to determine acrylamide concentration in popular banana based snacks in Malaysia using a modified method of gas chromatographymass spectrometry. The limit of detection and limit of quantitation of the modified method are 5 and 15 μg/kg, respectively. Acrylamide concentration of five types of Malaysian popular fried and baked banana based snacks from different local markets ranged from 74.0 to 7468.8 μg/ kg for banana fritter (pisang goreng), 28.9 to 243.7μg/kg for banana chips (kerepek pisang), 160.7 to 500.4 μg/kg for sweet banana chips (kerepek pisang manis), not detected to 154.4 μg/kg for banana cake (kek pisang) and 31.7 to 609.1 μg/kg for banana balls (cekodok pisang). Analysis of variance showed a significant difference (P

Matched MeSH terms: Limit of Detection
Agarose film liquid phase microextraction combined with gas chromatography-mass spectrometry for the determination of polycyclic aromatic hydrocarbons in water

Sanagi MM, Loh SH, Wan Ibrahim WA, Hasan MN

J Chromatogr A, 2012 Nov 2;1262:43-8.
PMID: 23021646 DOI: 10.1016/j.chroma.2012.09.007

Agarose film liquid phase microextraction (AF-LPME) procedure for the extraction and preconcentration of polycyclic aromatic hydrocarbons (PAHs) in water has been investigated. Agarose film was used for the first time as an interface between donor and acceptor phases in liquid phase microextraction which allowed for selective extraction of the analytes prior to gas chromatography-mass spectrometry. Using 1-octanol as acceptor phase, high enrichment factors in the range of 57-106 for the targeted analytes (fluorene, phenanthrene, fluoranthene and pyrene) were achieved. Under the optimum extraction conditions, the method showed good linearity in the range of 0.1-200 μgL(-1), good correlation coefficients in the range of 0.9963-0.9999, acceptable reproducibility (RSD 6.1-9.2%, n=3), low limits of detection (0.01-0.04 μgL(-1)) and satisfactory relative recoveries (92.9-104.7%). As the AF-LPME device was non-expensive, reuse or recycle of the film was not required, thus eliminating the possibility of analytes carry-over between runs. The AF-LPME technique is environment-friendly and compatible with the green chemistry concept as agarose is biodegradable polysaccharide extracted from seaweed and the procedure requires small volume of organic solvent and generates little waste. The validated method was successfully applied to the analysis of the four analytes in river water samples.

Matched MeSH terms: Limit of Detection
Fulltext Visual and Optical Absorbance Detection of Melamine in Milk by Melamine-Induced Aggregation of Gold Nanoparticles

Siddiquee S, Saallah S, Bohari NA, Ringgit G, Roslan J, Naher L, et al.

Nanomaterials (Basel), 2021 Apr 28;11(5).
PMID: 33924923 DOI: 10.3390/nano11051142

The present study reported a facile method for the determination of melamine in milk powder products based on the aggregation of reactant-free 5 nm gold nanoparticles (AuNPs). The strong electrostatic attraction between the positively charged exocyclic amine groups present in the melamine molecule and the negatively charged ions bound to the AuNPs induced aggregation of the AuNPs, resulting in visible color changes that could be seen with the naked eye and monitored by ultraviolet-visible (UV-Vis) absorbance spectra. The method shows high sensitivity with detection limits of 1 × 10-9 M for visual detection and 1 × 10-11 M for UV-Vis analysis, which is far below the safety limit of melamine ingestion in infant formula (1 ppm = 7.9 × 10-6 M) and the detection limit acquired by most AuNP-based melamine detection methods. Good recoveries were obtained over the range of 94.7-95.5% with a relative standard deviation of mean recovery (RSD) ranging from 1.40 to 5.81. The method provides a simple, feasible, fast and real-time detection of melamine adulterants in infant formula by the naked eye, without the aid of advanced instruments.

Matched MeSH terms: Limit of Detection
Fulltext A New and All-Solid-State Potentiometric Aluminium Ion Sensor for Water Analysis

Ying KS, Heng LY, Hassan NI, Hasbullah SA

Sensors (Basel), 2020 Dec 03;20(23).
PMID: 33287113 DOI: 10.3390/s20236898

An all-solid-state potentiometric electrode system for aluminium ion determination was developed with a new aluminium ion sensor as the working electrode based on a new ionophore for aluminium ion, 1,1'-[(methylazanediyl)bis(ethane-2,1-diyl)]bis[3-(naphthalen-1-yl)thiourea] (ACH). The reference electrode was a potassium ion sensor, which acts as a pseudo-reference. Both electrodes were made from Ag/AgCl screen-print electrodes fabricated from a non-plasticized and photocurable poly(n-butyl acrylate) membrane that contained various other membrane components. The pseudo-reference potential based on the potassium ion sensor was fixed in 0.050 M KNO3, and such concentration of K+ ion did not interfere with the measurement of the Al3+ ion using the aluminium sensor. With such a pseudo-reference and in the presence of 0.050 M KNO3 as a background medium, the aluminium sensor measured changes of aluminium ion concentrations linearly from 10-6 to 10-2 M Al3+ ion with a Nernstian response of 17.70 ± 0.13 mV/decade. A low detection limit of 2.45 × 10-7 M was achieved with this all-solid-state potentiometric system. The aluminium sensor was insensitive to pH effects from 2.0 to 8.0 with a response time of less than 50 s. Under optimum conditions, a lifetime of 49 days was achieved with good sensor selectivity, reversibility, repeatability, and reproducibility. The all-solid-state electrode system was applied to analyze the Al3+ ion content of water samples from a water treatment plant. Compared with the conventional potentiometric detection system for aluminium ions, the new all-solid-state aluminium ion sensor incorporating a pseudo-reference from the potassium sensor demonstrated similar analytical performance. It thus provided a convenient means of aluminium content analysis in water treatment plants.

Matched MeSH terms: Limit of Detection
Fulltext A Highly Sensitive Impedimetric DNA Biosensor Based on Hollow Silica Microspheres for Label-Free Determination of E. coli

Yuhana Ariffin E, Heng LY, Tan LL, Abd Karim NH, Hasbullah SA

Sensors (Basel), 2020 Feb 26;20(5).
PMID: 32111092 DOI: 10.3390/s20051279

A novel label-free electrochemical DNA biosensor was constructed for the determination of Escherichia coli bacteria in environmental water samples. The aminated DNA probe was immobilized onto hollow silica microspheres (HSMs) functionalized with 3-aminopropyltriethoxysilane and deposited onto a screen-printed electrode (SPE) carbon paste with supported gold nanoparticles (AuNPs). The biosensor was optimized for higher specificity and sensitivity. The label-free E. coli DNA biosensor exhibited a dynamic linear response range of 1 × 10-10 µM to 1 × 10-5 µM (R2 = 0.982), with a limit of detection at 1.95 × 10-15 µM, without a redox mediator. The sensitivity of the developed DNA biosensor was comparable to the non-complementary and single-base mismatched DNA. The DNA biosensor demonstrated a stable response up to 21 days of storage at 4 ℃ and pH 7. The DNA biosensor response was regenerable over three successive regeneration and rehybridization cycles.

Matched MeSH terms: Limit of Detection
Distinguishing normal and aggregated alpha-synuclein interaction on gold nanorod incorporated zinc oxide nanocomposite by electrochemical technique

Adam H, Gopinath SCB, Arshad MKM, Parmin NA, Hashim U

Int J Biol Macromol, 2021 Feb 28;171:217-224.
PMID: 33418041 DOI: 10.1016/j.ijbiomac.2021.01.014

Misfolding and accumulation of the protein alpha synuclein in the brain cells characterize Parkinson's disease (PD). Electrochemical based aluminum interdigitated electrodes (ALIDEs) was fabricated by using conventional photolithography method and modified the surfaces with zinc oxide and gold nanorod by using spin coating method for the analysis of PD protein biomarker. The device surface modified with gold nanorod of 25 nm diameter was used. The bare devices and the surface modified devices were characterized by Scanning Electron Microscope, 3D-Profilometer, Atomic Force Microscope and high-power microscope. The above measurement was also performed to measure the interaction of antibody with aggregated alpha-synuclein for normal, aggregated and aggregated alpha synuclein in human serum and distinguished against 3 control proteins (PARK1, DJ-1 and Factor IX). The detection limit for normal alpha synuclein was 1 f. with the sensitivity of 1 f. on a linear regression (R2 = 0.9759). The detection limit for aggregated alpha synuclein was 10 aM with the sensitivity of 1 aM on a linear regression (R2 = 0.9797). Also, the detection limit of aggregated alpha synuclein in serum was 10 aM with the sensitivity of 1 aM on a linear regression (R2 = 0.9739). These results however indicate that, serum has only minimal amount of alpha synuclein.

Matched MeSH terms: Limit of Detection
Health Risk Assessment of Heavy Metal in Urban Surface Soil (Klang District, Malaysia)

Yuswir NS, Praveena SM, Aris AZ, Ismail SN, Hashim Z

Bull Environ Contam Toxicol, 2015 Jul;95(1):80-9.
PMID: 25904089 DOI: 10.1007/s00128-015-1544-2

Urban environmental quality is vital to be investigated as the majority of people live in cities. However, given the continuous urbanization and industrialization in urban areas, heavy metals are continuously emitted into the terrestrial environment and pose a great threat to human. In this study, a total of 76 urban surface soil samples were collected in the Klang district (Malaysia), and analyzed for total and bioavailable heavy metal concentrations by inductively coupled plasma-optical emission spectrometry. Results showed that the concentrations of bioavailable heavy metals declined in the order of Al, Fe, Zn, Cu, Co, Cd, Pb, and Cr, and the concentrations of total heavy metals declined in the order of Fe, Al, Cu, Zn, Pb, Cr, Co, and Cd. Principal component analysis (PCA) showed that heavy metals could be grouped into three principal components, with PC1 containing Al and Fe, PC2 comprising Cd, Co, Cr, and Cu, and PC3 with only Zn. PCA results showed that PC1 may originate from natural sources, whereas PC2 and PC3 most likely originated from anthropogenic sources. Health risk assessment indicated that heavy metal contamination in the Klang district was below the acceptable threshold for carcinogenic and non-carcinogenic risks in adults, but above the acceptable threshold for carcinogenic and non-carcinogenic risks in children.

Matched MeSH terms: Limit of Detection
An electrochemical DNA biosensor fabricated from graphene decorated with graphitic nanospheres

Raja Jamaluddin RZA, Tan LL, Chong KF, Heng LY

Nanotechnology, 2020 Nov 27;31(48):485501.
PMID: 32748805 DOI: 10.1088/1361-6528/abab2e

Graphene decorated with graphitic nanospheres functionalized with pyrene butyric acid (PBA) is used for the first time to fabricate a DNA biosensor. The electrode was formed by attaching a DNA probe onto PBA, which had been stacked onto a graphene material decorated with graphene nanospheres (GNSs). The nanomaterial was drop-coated onto a carbon screen-printed electrode (SPE) to create the GNS-PBA modified electrode (GNS-PBA/SPE). A simple method was used to produce GNS by annealing graphene oxide (GO) solution at high temperature. Field emission scanning electron micrographs confirmed the presence of a spherical shape of GNS with a diameter range of 40-80 nm. A stable and uniform PBA-modified GNS (GNS-PBA) was obtained with a facile ultrasonication step. Thus allowing aminated DNA probes of genetically modified (GM) soybean to be attached to the nanomaterials to form the DNA biosensor. The GNS-PBA/SPE exhibited excellent electrical conductivity via cyclic voltammetry (CV) and differential pulse voltammetry (DPV) tests using potassium ferricyanide (K3[Fe(CN)6]) as the electroactive probe. By employing an anthraquinone monosulfonic acid (AQMS) redox intercalator as the DNA hybridization indicator, the biosensor response was evaluated using the DPV electrochemical method. A good linear relationship between AQMS oxidation peak current and target DNA concentrations from 1.0 × 10-16 to 1.0 × 10-8 M with a limit of detection (LOD) of less than 1.0 × 10-16 M was obtained. Selectivity experiments revealed that the voltammetric GM DNA biosensor could discriminate complementary sequences of GM soybean from non-complementary sequences and hence good recoveries were obtained for real GM soybean sample analysis. The main advantage of using GNS is an improvement of the DNA biosensor analytical performance.

Matched MeSH terms: Limit of Detection

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