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Multichannel graphite electrodes (MGrEs) have been designed and fabricated in this study. A template was cut from an adhesive plastic sheet using a desktop cutting device. The template was placed on a polypropylene substrate, and carbon graphite ink was applied with a squeegee to the template. The size of the auxiliary electrode (AE) as well as the location of the reference electrode (RE) of MGrEs design were investigated. Scanning electron microscopy was used to determine the thickness of the ink on the four working electrodes (WEs), which was 21.9 ± 1.8 µm. Cyclic voltammetry with a redox probe solution was used to assess the precision of the four WEs. The intra-electrode repeatability and inter-electrode reproducibility of the MGrEs production were satisfied by low RSD (<6%). Therefore, the MGrEs is reliable and capable of detecting four replicates of the target analyte in a single analysis. The electrochemical performance of four WEs was investigated and compared to one WE. The sensitivity of the MGrEs was comparable to the sensitivity of a single WE. The MGrEs' potential applications were investigated by analyzing the nitrite in milk and tap water samples (recoveries values of 97.6 ± 0.4 to 110 ± 2%).
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Grafite , Técnicas Eletroquímicas/métodos , Eletrodos , Limite de Detecção , Impressão Tridimensional , Reprodutibilidade dos TestesRESUMO
Drugs-facilitated crimes (DFCs) involve the incapacitation of victims under the influence of drugs. Conventionally, a drug administration act is often determined through the examination of biological samples; however, dry residues from any surface, such as drinking glass if related to a DFC could be a potential source of evidence. This study was aimed to establish an attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy coupled with chemometrics for the determination of spiked sedative-hypnotics from dry residues of a drug-spiked beverage. In this study, four sedative-hypnotics, namely diazepam, ketamine, nimetazepam, and xylazine were examined using ATR-FTIR spectroscopy. Subsequently, the ATR-FTIR profiles were compared and decomposed by principal component analysis (PCA) followed by linear discriminant analysis (LDA) for their detection and discrimination. Visual comparison of ATR-FTIR profiles revealed distinct spectra among the tested drugs. An initial unsupervised exploratory PCA model indicated the separation of four main sedative-hypnotics clusters, and the proposed PCA score-LDA model had allowed for a 100% accurate classification. Discrimination of sedative-hypnotics from a dry beverage previously spiked with these drugs was also possible upon an additional extraction procedure. In conclusion, ATR-FTIR coupled with PCA score-LDA model was useful in detecting and discriminating sedative-hypnotics, including those that had been previously spiked into a beverage.
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Bebidas , Quimiometria , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Análise de Fourier , Análise de Componente Principal , Hipnóticos e SedativosRESUMO
Ethnicity, native and/or foreign language knowledge, as well as the learned writing systems potentially influence the development of an individual's handwriting. The unique education system consisting of National schools, Chinese-medium vernacular schools, Tamil-medium vernacular schools, and Islamic religious schools in Malaysia may have established specific characteristic handwritten allographic features that deserve investigation within the intelligence context. This study was aimed to explore handwritten allographic features of handwriting samples from 120 subjects (30 writers from four different educational backgrounds mentioned above). Characteristic features which could be attributed to the study groups were statistically analyzed and identified. In this study, thirteen allographic features, including letters "A", "B", "D", "H", "p", "T", "t", "w", "X" and "x", were found to be discriminative. Such information could serve to indicate the primary education system undergone by a writer; enabling the comparison of different handwriting profiles and allowing characterization of writers to a specific group of people.
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Etnicidade , Escrita Manual , Biometria , Humanos , Índia , IdiomaRESUMO
Formalin is illegally used as an antibacterial and a preservative in seafood products. It is extremely important for public health reasons to be able to simply, rapidly, and accurately detect formalin in fresh seafood. In this work, we developed a flow injection amperometric (FI-Amp) formalin sensor based on a glassy carbon electrode modified with a composite of palladium particles and carbon microspheres (PdPs-CMs/GCE). The CMs were decorated with PdPs via an electroless deposition method. The surface morphology of the CMs and the PdPs-CMs composite was characterized by scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX). The electrochemical behavior and measurement of formalin at the PdPs-CMs/GCE was evaluated by cyclic voltammetry and amperometry. The modified electrode demonstrated good electrocatalytic performance for the oxidation of formalin. The synthesis method and FI-Amp operating conditions were optimized. Under the optimal conditions, the developed sensor showed a linear range of 0.025 to 15.00 mmol L-1 and a detection limit of 8 µmol L-1. Repeatability (RSD < 4.1%, n = 30), reproducibility (RSD = 0.25%, n = 5), stability (RSD = 3.2%, n = 80), and selectivity were good. The fabricated sensor achieved recoveries of formalin in seafood between 96 ± 1 to 105 ± 3 (n = 3).
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Presently, investigations of drug-facilitated crimes (DFCs) rely on the detection of substances extracted from biological samples following intake by the victim. However, such detection requires rapid sampling and analysis prior to metabolism and elimination of the drugs from the body. In cases of suspected DFCs, drug-spiked beverage samples, whether in liquid, droplet, or even dried form, can be tested for the presence of spike drugs and used as evidence for the occurrence of DFCs. This study aimed to quantitatively determine three sedative-hypnotics (ketamine, nimetazepam, and xylazine) from drug-spiked beverages using a vortex-assisted dispersive liquid-liquid microextraction-gas chromatography (VADLLME-GC) approach. In this study, a GC method was first developed and validated, followed by the optimization of the VADLLME protocol, which was then applied to quantify the target substances in simulated forensic case scenarios. The developed GC method was selective, sensitive (limit of detection: 0.08 µg/ml [ketamine]; 0.16 µg/ml [nimetazepam]; 0.08 µg/ml [xylazine]), linear (R2 > 0.99), precise (%RSD <7.2%), and accurate (% recovery: 92.8%-103.5%). Higher recoveries were achieved for the three drugs from beverage samples in liquid form (51%-97%) as compared to droplet (48%-96%) and dried (44%-93%) residues. The recovery was not hindered by very low volumes of spiked beverage and dried residues. In conclusion, the developed VADLLME-GC method successfully recovered ketamine, nimetazepam, and xylazine from spiked beverages that are likely to be encountered during forensic investigation of DFCs.
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Ketamina , Microextração em Fase Líquida , Bebidas/análise , Cromatografia Gasosa , Ketamina/análise , Limite de Detecção , Microextração em Fase Líquida/métodos , Nitrazepam/análogos & derivados , Xilazina/análiseRESUMO
A portable electrochemical device for xylazine detection is presented for the first time. An electrochemical paper-based analytical device (ePAD) was integrated with a smartphone. The fabrication of the ePAD involved wax printing, low-tack transfer tape, and cutting and screen-printing techniques. Graphene ink was coated on the substrate and modified with nanocoral-like polyaniline, providing an electron transfer medium with a larger effective surface area that promoted charge transfer. The conductive ink on the ePAD presented a thickness of 25.0 ± 0.9 µm for an effective surface area of 0.374 cm2. This sensor was then tested directly on xylazine using differential pulse voltammetry. Two linear responses were obtained: from 0.2 to 5 µg mL-1 and from 5 to 100 µg mL-1. The detection limit was 0.06 µg mL-1. Reproducibility was tested on 10 preparations. The relative standard deviation was less than 5%. The applicability of the sensor was evaluated with beverage samples spiked with trace xylazine. Recoveries ranged from 84 ± 4 to 105 ± 2%. The developed sensor demonstrated excellent accuracy in the detection of trace xylazine. It would be possible to develop the portable system to detect various illicit drugs to aid forensic investigations.
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We developed a simple, inexpensive, environmentally friendly one-step fabrication of a flexible laser induced graphene-chitosan-gold nanoparticles (LIG-CS-AuNPs) electrode. The fabrication was based on a laser treatment of polyimide (PI) film coated with CS solution containing gold ions (Au (III)). The AuNPs decorating the induced 3D graphene composite were uniformly distributed. The electrode exhibited good electrical conductivity and excellent electrocatalytic activity toward the oxidation of UA. To enable on-site monitoring of uric acid (UA) in blood serum by differential pulse adsorptive stripping voltammetry (DPAdSV), the electrode was coupled to a portable potentiostat connected to a cellphone to control and monitor analysis. The affecting parameters of DPAdSV were optimized. Under the optimal conditions for UA determination, the limit of detection of the developed sensor was 0.33 µmol L-1 and the limit of quantification 1.10 µmol L-1. Two linear ranges were produced: 1.0-30 µmol L-1 and 30-100 µmol L-1. The sensor was highly sensitive and demonstrated excellent reproducibility and selectivity, determining UA in blood serum with recoveries between 86.6 ± 0.6 and 94.7 ± 0.4%. The analysis results were in agreement with those of the hospital standard enzymatic method.
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Técnicas Biossensoriais , Quitosana , Grafite , Nanopartículas Metálicas , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Eletrodos , Ouro , Lasers , Porosidade , Reprodutibilidade dos Testes , Ácido Úrico/análiseRESUMO
Abuse of solvent-based adhesives jeopardizes world population, especially the young generation. Adhesive-related exhibits encountered in forensic cases might need to be determined if they could have come from a particular source or to establish link between cases or persons. This study was aimed to discriminate solvent-based adhesives, especially to aid forensic investigation of glue sniffing activities. In this study, thirteen brands with three samples each, totaling at 39 adhesive samples, were analyzed using attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy followed by chemometric methods. Experimental output showed that adhesive samples utilized in this study were less likely to change in their ATR-FTIR profiles over time, at least up to 2 months. No interference from plastic materials was noticed based on ATR-FTIR profile comparison. Physical examination could differentiate the samples into two groups, namely contact adhesives and cement adhesives. A principal component analysis-score linear discriminative analysis (PC-score LDA) model resulted in 100% and 98.6% correct classification in discriminating the two groups of adhesive samples, forming seven discriminative clusters. Test set with adhesive samples applied glass slide and plastic substrates also demonstrated a 100% correct classification into their respective groups. As a conclusion, the method allowed for discrimination of adhesive samples based on the spectral features, displaying relationship among samples. It is hoped that this comparative information is beneficial to trace the possible source of solvent-based adhesives, whenever they are recovered from a crime scene, for forensic investigation.
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Due to the outbreak of the COVID-19 pandemic, practicing personal hygiene such as frequent hand sanitising has become a norm. The making of effective hand sanitiser products should follow the recommended formulations, but the high demand worldwide for such affordable products could have made them a candidate for counterfeiting, thus deserving forensic determination and profiling for source determination or supply chain tracing. In this study, determination and discrimination of hand sanitisers was carried out by employing attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy combined with chemometrics. Fifty commercially available hand sanitisers were obtained from the market and analysed. ATR-FTIR profiles of each sanitiser were compared and decomposed by principal component analysis (PCA) followed by linear discriminant analysis (LDA). Physical observation enabled the discrimination of seven samples based on their respective colours, the presence of beads and their colours, and the physical forms of formulations. Subsequently, eight distinct patterns were observed through visual comparison of ATR-FTIR profiles of the remaining 43 samples. An initial unsupervised exploratory PCA model indicated the separation of two main groups with ATR-FTIR profiles similar to those of ethanol and isopropanol, respectively. The PCA score-LDA model provided good predictions, with a 100% correct classification into eight different groups. In conclusion, this study demonstrated a quick determination and discrimination of hand sanitiser samples, allowing screening for any restricted components and sample-to-sample comparison.
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Higienizadores de Mão/normas , COVID-19 , Análise de Fourier , Higiene das Mãos , Humanos , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
BACKGROUND: Low birth weight and preterm or early-term babies may have a higher risk of poor health. One of the main factors is the weight gain of a pregnant woman during gestational weeks in the second and third trimesters. Changes in weight over a month in a pregnant woman might also have an impact on infant outcomes. This study aimed to investigate the association between maternal weight at different time points and low birth weight and preterm or early-term babies (premature babies). METHODS: A total of 156 pregnant women were recruited. Maternal weight was collected at different gestational weeks. Maternal age, body mass index, delivery mode, delivery week, and infant weight were also recorded. Maternal data were restructured into a person-period format before mixed-effects multiple logistic regression was used. Various weight variables with either a fixed effect or time-varying effects were tested in the model. RESULTS: Thirty (19.23%) women had delivered low birth weight or premature babies. Multiple logistic regression model demonstrated that mothers with higher increases in weight at 32 weeks of gestation than that in the predelivery stage had a lower probability of having a low birth weight or premature baby (odds ratio [OR] = 0.64; 95% CI, 0.49-0.85; p < 0.001). Women with a weight increase of more than 2 kg in a 4-week gestation period had a higher probability of having a low birth weight or premature baby than those with an increment of <1 kg (OR = 8.43; 95% CI, 2.90-24.54; p < 0.001). CONCLUSION: An increase in weight gain after 32 weeks was shown to reduce the risk of low birth weight and premature babies. Maternal weight monitoring was suggested to be conducted every 4 weeks to minimize the chance of having a low birth weight and premature baby.
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Ganho de Peso na Gestação , Recém-Nascido de Baixo Peso , Nascimento Prematuro , Adulto , Índice de Massa Corporal , Feminino , Humanos , Malásia , GravidezRESUMO
A portable electrochemical sensor was developed to determine xylazine in spiked beverages by adsorptive stripping voltammetry (AdSV). The sensor was based on a graphene nanoplatelets-modified screen-printed carbon electrode (GNPs/SPCE). The electrochemical behavior of xylazine at the GNPs/SPCE was an adsorption-controlled irreversible oxidation reaction. The loading of graphene nanoplatelets (GNPs) on the modified SPCE, electrolyte pH, and AdSV accumulation potential and time were optimized. Under optimal conditions, the GNPs/SPCE provided high sensitivity, linear ranges of 0.4-6.0 mg L-1 (r = 0.997) and 6.0-80.0 mg L-1 (r = 0.998) with a detection limit of 0.1 mg L-1 and a quantitation limit of 0.4 mg L-1. Repeatability was good. The accuracy of the proposed sensor was investigated by spiking six beverage samples at 1.0, 5.0, and 10.0 mg L-1. The recoveries from this method ranged from 80.8 ± 0.2-108.1 ± 0.3 %, indicating the good accuracy of the developed sensor. This portable electrochemical sensor can be used to screen for xylazine in beverage samples as evidence in cases of sexual assault or robbery.
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Técnicas Eletroquímicas , Drogas Veterinárias , Bebidas , Eletrodos , XilazinaRESUMO
A 3D porous graphene structure was directly induced by CO2 laser from the surface of Kapton tape (carbon source) supported by polyethylene terephthalate (PET) laminating film. A highly flexible laser-induced porous graphene (LI-PGr) electrode was then fabricated via a facile one-step method without reagent and solvent in a procedure that required no stencil mask. The method makes pattern design easy, and production cost-effective and scalable. We investigated the performance of the LI-PGr electrode for the detection of methamphetamine (MA) on household surfaces and in biological fluids. The material properties and morphology of LI-PGr were analysed by scanning electron microscopy (SEM), energy dispersive x-ray (EDX) and Raman spectroscopy. The LI-PGr electrode was used as the detector in a portable electrochemical sensor, which exhibited a linear range from 1.00 to 30.0 µg mL-1 and a detection limit of 0.31 µg mL-1. Reproducibility was good (relative standard deviation of 2.50% at 10.0 µg mL-1; n = 10) and anti-interference was excellent. The sensor showed good precision and successfully determined MA on household surfaces and in saliva samples.
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Wherever an impact mark is found, either on the surface or on the recovered projectile, it is important for forensic investigators to extract useful information in solving shooting-related cases. This article reviews a collection of works on examination of impact marks upon striking of projectiles on inanimate objects, emphasizing on the retrievable information from a shooting scene and their forensic significance in shooting event reconstruction. Literature suggested that impact marks on target surfaces and the degree of deformation on striking projectiles vary according to different combinations of ammunition and surface materials. It was noted that conditions in real-case scenarios further differed unpredictably in comparison with controlled studies, where forensic investigation should be treated as case-specific basis. Furthermore, the way forensic science is researched and applied operationally has to be reconsidered to reduce the gap via translational approach for more effective use of forensic evidence.
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The topcoat color of motor vehicles offers vital information while investigating vehicular accidents, especially in instance of hit-and-run, since witnesses seldom perceive and retain the plate details. Differences in color perceptions among individuals with normal vision may lead to confusion in determining the color of the car involved. In this way, witnesses of crash accidents could potentially initiate flawed leads in forensic investigation, and thus affect the administration of justice. In this study, the inter-rater reliability of vehicle color determination by different volunteers was explored. Six individuals observed the topcoat colors of 500 stationary and 500 moving vehicles from five locations, employing a common system of color gradation. The outcome was binary: the vehicle color was either a "match" or "non-match". This was followed by statistical analysis in terms of the colors' frequencies and inter-rater reliability, based on which more suitable color descriptions were determined for subsequent comparisons of stationary and moving vehicles. Higher match frequencies and greater inter-rater reliability were observed when color gradations were disregarded. The frequency of correct matches could have been closely related to their relative on-the-road distribution, regardless of the statuses of observed vehicles. It was also found that black and white were associated with a greater number of matches than were intermediate colors, which should be carefully interpreted during forensic investigation to avoid wrong leads. In conclusion, the present study demonstrated the forensic significance of vehicle topcoat color determination, particularly in cases where witness statements are crucial.
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Acidentes de Trânsito , Percepção de Cores , Cor , Ciências Forenses , Adulto , Humanos , Veículos AutomotoresRESUMO
Gunshot residues, produced after shooting activity, have acquired their importance in analysis due to the notoriety of firearms-related crimes. In this study, solid-phase microextraction was performed to extract the headspace composition of spent cartridges using 85-µm polyacrylate fiber at 66°C for 21 min. Organic compounds, that is, naphthalene, 2,6-dinitrotoluene, 2,4-dinitrotoluene, diphenylamine, and dibutyl phthalate were detected and analyzed by gas chromatography-flame ionization detection technique. Evaluation of chromatograms for diphenylamine, dibutyl phthalate, and naphthalene indicates the period after a gunshot was discharged, whether it was 1 days, 2-4 days, <5 days, 10 days, 20 days, or more than 30 days ago. This study revealed the potential effects of environmental factors such as occasional wind blow and direct sunlight on the estimation of time after spent cartridges were discharged. In conclusion, we proposed reliable alternative in analyzing the headspace composition of spent cartridges in a simulated crime scene.
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Smokeless powders are low explosives and are potentially found in cases involving firearms and improvised explosive devices. Apart from inorganic compound analysis, forensic determination of organic components of these materials appears as a promising alternative, especially the chromatographic techniques. This work describes the optimization of a solid-phase microextraction technique using an 85 µm polyacrylate fiber followed by gas chromatography-flame ionization detection for smokeless powder. A multivariate experimental design was performed to optimize extraction-influencing parameters. A 2(4) factorial first-order design revealed that sample temperature and extraction time were the major influencing parameters. Doehlert matrix design has subsequently selected 66°C and 21 min as the compromised conditions for the two predetermined parameters. This extraction technique has successfully detected the headspace compounds of smokeless powders from different ammunition types and allowed for their differentiation. The novel technique allows more rapid sample preparation for chromatographic detection of smokeless powders.