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Emerging pollutants pose an increasing threat to the environment and human well-being, requiring substantial progress in analytical methodologies. Dispersive micro-solid phase extraction (µ-dSPE) has proven successful in detecting and measuring these contaminants, particularly in trace quantities. However, challenges persist in achieving a uniform sorbent distribution and efficient separation from the sample matrix. To address these issues, effervescent-assisted dispersive micro-solid phase extraction (EA-µ-dSPE) was developed. This method uses on-site produced carbon dioxide as a dispersing agent, eliminating the need for vortexing or ultrasonication. Due to the sorbent dispersion in the sample solution, the contact surface between the analyte and the sorbent increases, resulting in increased extraction efficiency, reduced extraction time, and promotes of sustainability. Several parameters are critical to the successful execution of this procedure to extract the analytes, including the type and structure of sorbent, composition of dispersing agents, sorbent separation procedure, and type and properties of desorption solvents. The sorbent plays a critical role in successful extraction of emerging pollutants. It is clear that for the extraction of the analyte on the sorbent, proper interaction must be established between the analyte and the sorbent via physical and chemical interactions. This review thoroughly evaluates the underlying principles of the approach, its potential, and the significant advancements that have been documented. It explores the method's capacity to analyse and identify emerging pollutants, emphasising its potential across various sample matrices for enhanced pollutant identification and quantification.
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Poly(methyl methacrylate-vinyl imidazole bromide) (poly-MMA-IL)-grafted magnetic nanoparticles were successfully developed and applied in the micro-magnetic solid phase extraction (µ-MSPE) for 16 types of polycyclic aromatic hydrocarbons (PAHs) from tea, fried food, and grilled food samples via gas chromatography flame ionization detector (GC-FID). One variable at a time (OVAT) and response surface methodology (RSM) were used for efficient optimization. The validation method showed a good coefficient of determination (R2) ranging from 0.9901 to 0.9982 (n = 3) with linearity of 0.2 µg L-1-500 µg L-1. Detection and quantification limits were 0.06 µg L-1-0.32 µg L-1 and 0.18 µg L-1-0.97 µg L-1. Additionally, satisfactory reproducibility was attained with intra-day and inter-day precisions having RSD ranges of 3.6%-11.1%. The spiked recovery value of 16 PAHs in fried food, grilled food and tea samples obtained from the night market in Malaysia ranged from 80%-12%, respectively.
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Análise de Alimentos , Contaminação de Alimentos , Líquidos Iônicos , Nanopartículas de Magnetita , Hidrocarbonetos Policíclicos Aromáticos , Hidrocarbonetos Policíclicos Aromáticos/análise , Hidrocarbonetos Policíclicos Aromáticos/química , Contaminação de Alimentos/análise , Nanopartículas de Magnetita/química , Líquidos Iônicos/química , Microextração em Fase Sólida , Extração em Fase Sólida , Chá/química , Polímeros/químicaRESUMO
A paper-based polymeric ionic liquid (p-Poly-(MMA-IL)) was successfully developed by grafting the polymeric ionic liquid on the surface of commercial filter paper (FP) by using the dipping method, presenting a new cost-effective film. The newly developed p-Poly-(MMA-IL) FP was then applied as a paper-based thin-film microextraction (p-TFME) analytical device to extract 14 compounds as representative of five groups of antibiotic drugs, which were sulfonamides, tetracyclines, fluoroquinolones, penicillin and macrolides in environmental water samples. Besides, p-Poly-(MMA-IL) FP, p-Poly-(MMA) FP, and unmodified filter paper were successfully characterised by FTIR, NMR, FESEM, TGA, and XRD techniques. They underwent significant parameters optimisation, which affected the extraction efficiency. Under optimal conditions, the proposed (p-Poly-(MMA-IL) FP-TFME) device method was evaluated and applied to analyse multi-class antibiotic drugs in environmental water samples by using a liquid chromatography-mass spectrometry (LC-MS). The validation method showed that a good linearity (0.1 µg L-1 - 500 µg L-1) was noted (R2 > 0.993, n = 3). Detection and quantification limits were within 0.05 µg L-1 - 4.52 µg L-1 and 0.15 µg L-1 - 13.6 µg L-1, respectively. The relative standard deviation (RSD) values ranged at 1.4%-12.2% (intra-day, n = 15) and 4.4%-11.0% (inter-day, n = 10). The extraction recoveries of environmental water samples ranged from 79.1% to 126.8%, with an RSD of less than 15.4% (n = 3). The newly developed paper-based polymeric ionic liquid (p-Poly-(MMA-IL) FP) for analysis of multi-class antibiotic drugs under the p-TFME analytical device procedure was successfully achieved with limited sample volume and organic solvent, fast extraction, and feasible in daily analysis. The detection concentration and relative RSD of multi-class antibiotics determined in various environmental water samples by the proposed method (n = 5) were within 0.44 µg L-1 - 54.41 µg L-1 and 0.69%-15.56%, respectively. These results signified the potential of the p-Poly-(MMA-IL) FP-TFME device as an efficient, sensitive and environmentally friendly approach for analysing antibiotics.
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Líquidos Iônicos , Microextração em Fase Líquida , Cromatografia Líquida/métodos , Antibacterianos , Cromatografia Líquida de Alta Pressão , Líquidos Iônicos/química , Espectrometria de Massas em Tandem/métodos , Água/química , Microextração em Fase Líquida/métodos , Limite de DetecçãoRESUMO
Clinacanthus nutans is a medicinal plant recognised for its anticancer properties. We previously discovered that the C. nutans extract had the most potent inhibitory effect on MCF7 breast cancer cell and significantly induced apoptosis. However, there is a scarcity of studies demonstrating the molecular interactions of C. nutans-derived chemical compounds associated with apoptosis-related proteins. Therefore, the objective of this study was to determine the potential chemical compounds found in the C. nutans extract and examine their interactions with the targeted apoptotic proteins using molecular docking and molecular dynamic simulations. To address this objective, the compounds found in the SF2 extract of C. nutans were analysed using Gas Chromatography-Mass Spectrometry (GC-MS). The molecular interaction of the compounds with the targeted apoptotic proteins were determined using molecular docking and molecular dynamic simulations. GC-MS analysis revealed a total of 32 compounds in the SF2 extract. Molecular docking analysis showed that compound ß-amyrenol had the highest binding affinity for MDM2-P53 (-7.26 kcal/mol), BCL2 (-11.14 kcal/mol), MCL1-BAX (-6.42 kcal/mol), MCL1-BID (-6.91 kcal/mol), and caspase-9 (-12.54 kcal/mol), whereas campesterol had the highest binding affinity for caspase-8 (-10.11 kcal/mol) and caspase-3 (-10.14 kcal/mol). These selected compounds were subjected to molecular dynamic simulation at 310 K for 100 ns. The results showed that the selected protein-ligand conformation complexes were stable, compact, and did not alter much when compared to the protein references. The findings indicate that ß-amyrenol and campesterol are potentially significant compounds that might provide insight into the molecular interactions of the compounds with the apoptosis-related proteins.Communicated by Ramaswamy H. Sarma.
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Simulação de Dinâmica Molecular , Extratos Vegetais , Cromatografia Gasosa-Espectrometria de Massas , Extratos Vegetais/farmacologia , Extratos Vegetais/química , Simulação de Acoplamento Molecular , Proteína de Sequência 1 de Leucemia de Células Mieloides , Proteínas Reguladoras de Apoptose , ApoptoseRESUMO
Clinacanthus nutans dichloromethane fraction (CN-Dcm) extract has previously been proven to suppress breast cancer (MCF7) cell proliferation. Despite this, the extrinsic and intrinsic apoptosis mechanisms involved in C. nutans extract-treated MCF7 cells are still unknown. This study was intended to subfractionate CN-Dcm extract using column chromatography and analyse the treated MCF7 cells using the CellTiter 96® AQueous One Solution Cell Proliferation (MTS) assay, Annexin V/propidium iodide (PI) assay, western blot, and reverse transcription-qualitative polymerase chain reaction (RT-qPCR). Out of nine subfraction extracts (SF1 to SF9), SF2 extract strongly inhibited MCF7 cells with the lowest IC50 value (23.51 ± 1.00 µg/mL) and substantially induced apoptosis in the MCF7 cells. In treated MCF7 cells, SF2 extract significantly upregulated the expression of P53, BAX, BID, caspase-8, caspase-9, and caspase-3, while downregulating the expression of BCL2. The presence of potential bioactive chemical compounds in the SF2 extract was identified using liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (LC-QTOF-MS). Thus, the SF2 extract has the potential to induce apoptosis in MCF7 cells through intrinsic and extrinsic pathways.
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Acanthaceae , Neoplasias da Mama , Humanos , Feminino , Caspase 3 , Caspase 9 , Caspase 8 , Cloreto de Metileno , Anexina A5 , Propídio , Proteína Supressora de Tumor p53 , Proteína X Associada a bcl-2 , Extratos Vegetais/farmacologia , Extratos Vegetais/química , Acanthaceae/química , ApoptoseRESUMO
Clinacanthus nutans has been reported to have many medicinal properties and it is traditionally used in treating viral lesions. This study aims to determine the molecular docking of C. nutans compounds detected by Gas Chromatography-Mass Spectrometry (GC-MS) with the novel severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2 main protease) protein and its host receptor angiotensin-converting enzyme 2 (ACE2) protein using the AutoDock 4.2 tool. The drug-likeness and molecular docking analyses showed that fourteen compounds of C. nutans satisfied the Lipinski's rule of five and they exhibited good inhibitory effects against the SARS-Cov-2 main protease and ACE2 proteins. In addition, the glyceryl 2-linolenate compound was found to have the most potent binding affinities with both proteins. The results provide useful insights into the molecular inhibitory interactions of C. nutans compounds detected by GC-MS analysis with the targeted SARS-CoV-2 main protease and ACE2 protein.
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Acanthaceae , Tratamento Farmacológico da COVID-19 , Acanthaceae/química , Enzima de Conversão de Angiotensina 2 , Antivirais/farmacologia , Proteases 3C de Coronavírus , Cromatografia Gasosa-Espectrometria de Massas , Simulação de Acoplamento Molecular , Extratos Vegetais/farmacologia , SARS-CoV-2RESUMO
A dynamic pH junction was used in capillary electrophoresis (CE-DAD) to on-line preconcentrate, separate, and determine trace amounts of sulfonamide antibiotics (SAs) in milk and yoghurt samples in this study. A sample matrix with 0.15% acetic acid and 10% methanol (MeOH) at a pH of 4.0, and a background electrolyte (BGE) that contained 35 mM sodium citrate with 10% MeOH at a pH of 8.5, and an acidic barrage of 0.4% acetic acid with 10% MeOH at a pH of 2.5 were utilised to achieve a stacking effect for SAs through a dynamic pH junction. Under optimised conditions, the proposed preconcentration method showed good linearity (30-500 ng/mL, r2 ≥ 0.9940), low limits of detection (LODs) of 4.1-6.3 ng/mL, and acceptable analytes recovery (81.2-106.9%) with relative standard deviations (RSDs) within 5.3-13.7 (n = 9). The limits of quantification (LOQs) were below the maximum residue limit approved by the European Union (EU) in this type of matrices. Sensitivity enhancement factors of up to 129 were reached with the optimised dynamic pH junction using CE with a diode array detector (DAD). The method was used to determine SAs in fresh milk, low-fat milk, full-cream milk, and yoghurt samples.
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Antibacterianos , Iogurte , Animais , Eletroforese Capilar , Concentração de Íons de Hidrogênio , Leite , SulfonamidasRESUMO
BACKGROUND: C. vespertiliomis extracts were evaluated for antiproliferative and apoptosis effect on breast cancer (MCF7) cells. METHODS AND RESULTS: The leaves extracts were analysed for its antiproliferative effect on breast cancer (MCF7) cells and normal epithelial breast (MCF 10A) cells using Sulforhodamine B (SRB) assay. The selective extract was evaluated for its ability to induce apoptosis using Annexin V-FITC apoptosis staining and the expression of molecular genes using qualitative reverse transcription-polymerase chain reaction (RT-PCR) against MCF7 cells. Gas chromatography-mass spectrometry (GC-MS) was used to identify the compounds from the selective extract. The findings showed that dichloromethane fraction (CV-Dcm) extract had high antiproliferative effect against MCF7 cells (IC50 = 24 µg/mL, selective index (SI) = 8.17). The percentages of apoptosis cells in CV-Dcm-treated MCF7 cells was 58.8%. The CV-Dcm extract induced downregulation of PCNA level. The apoptotic genes were also triggered in both extrinsic and intrinsic signaling pathways, affecting a 1.5-fold increase in BAX, 1.4-fold increase in cytochrome c, 1.3-fold increase in caspase-8, 1.7-fold increase in caspase-3 and 0.5-fold-decrease in BCL-2. Treated MCF7 cells also activated P53-dependent apoptotic death pathway. CONCLUSIONS: The present work strongly suggests that high efficacy of CV-Dcm extract was attributed to its antiproliferative and apoptosis-inducing activation in MCF7 cells, most likely due to its favourable compounds.
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Apoptose , Neoplasias da Mama/tratamento farmacológico , Proliferação de Células , Fabaceae/química , Extratos Vegetais/farmacologia , Antineoplásicos Fitogênicos/farmacologia , Antineoplásicos Fitogênicos/uso terapêutico , Neoplasias da Mama/fisiopatologia , Caspase 3 , Feminino , Humanos , Células MCF-7 , Extratos Vegetais/uso terapêuticoRESUMO
Silver nanoparticles (AgNPs) previously synthesised using leaf (AgNP-L) and stem (AgNP-S) extracts of Clinacanthus nutans (C. nutans) were tested to evaluate antimicrobial, antioxidant, and cytotoxicity activities. The AgNPs showed good inhibition against bacteria, but not fungi. The inhibition results showed the highest activity against Staphylococcus aureus (S. aureus) with 11.35 mm (AgNP-L) and 11.52 mm (AgNP-S), while the lowest inhibition was against Escherichia coli (E. coli) with 9.22 mm (AgNP-L) and 9.25 mm (AgNP-S) in the disc diffusion method. The same trend of results was noted in the well diffusion method. The IC50 of AgNP-L and AgNP-S in 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2'-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) assays was 417.05 µg/mL and 434.60 µg/mL, as well as 304.31 µg/mL and 326.83 µg/mL, respectively. Ferric reducing power (FRAP) assay showed that AgNP-L [872.389 µmol/L Fe(II)] and AgNP-S [612.770 µmol/L Fe(II)] exhibited significantly (p < 0.05) greater antioxidant activities than leaf extract (CNL) [152.260 µmol/L Fe(II)] and stem extract (CNS) [110.445 µmol/L Fe(II)] of C. nutans. The AgNPs were also proven to possess cytotoxic effects on the breast (MCF-7), cervical (HeLa), and colon (HT-29) cancer cells in a dose-dependent manner. AgNP-S and AgNP-L showed significantly (p < 0.05) higher cytotoxicity against MCF-7 (117.43 µg/mL) and HT-29 (78.47 µg/mL), respectively. In conclusion, the biosynthesised AgNPs from aqueous extract leaves and stem of C. nutans have demonstrated promising potential towards antioxidant, antimicrobial, and cytotoxicity activities.
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A simple and sensitive preconcentration strategy using sequential electrokinetic and hydrodynamic injection modes in micellar electrokinetic chromatography with diode array detection was developed and applied for the separation and determination of anticancer agent, 5-fluorouracil and its metabolite, 5-fluoro-2'-deoxyuridine, in human plasma. Sequential injection modes with increased analyte loading capacity using the anionic pseudo-stationary phase facilitated collection of the dispersed neutral and charged analytes into narrow zones and improved sensitivity. Several important parameters affecting sample enrichment performance were evaluated and optimized in this study. Under the optimized experimental conditions, 614- and 643-fold and 782- and 803-fold sensitivity improvement were obtained for 5-fluorouracil and its metabolite when compared with normal hydrodynamic and electrokinetic injection, respectively. The method has good linearity (1-1,000 ng/ml) with acceptable coefficient of determination (r2 > 0.993), low limits of detection (0.11-0.14 ng/ml) and satisfactory analyte relative recovery (97.4-99.7%) with relative standard deviations of 4.6-9.3% (n = 6). Validation results as well as the application to analysis of human plasma samples from cancer patients demonstrate the applicability of the proposed method to clinical studies.
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Antineoplásicos/sangue , Cromatografia Capilar Eletrocinética Micelar/métodos , Desoxiuridina/análogos & derivados , Fluoruracila/sangue , Desoxiuridina/sangue , HumanosRESUMO
A chiral separation method coupled with capillary electrophoresis (CE) analysis for ketoconazole and miconazole enantiomers using chiral selectors such as ß-cyclodextrin (ß-CD) and hydroxypropyl-ß-CD (HP-ß-CD) was developed in this study, which included the optimisation, validation and application of the method on the antifungal cream samples. The formation of inclusion complex between the hosts (ß-CD and HP-ß-CD) and guests (ketoconazole and miconazole) were compared and analysed using ultraviolet-visible spectrophotometry, nuclear magnetic resonance (NMR) spectroscopy and molecular docking methods. Results from the study showed that in a concentration that ranged between 0.25 and 50 mg L-1 , the linear calibration curves of each enantiomer had a high coefficient of regression (R2 > 0.999), low limit of detection (0.075 mg L-1 ) and low limit of quantification (0.25 mg L-1 ). The relative standard deviation (RSD) of the intraday and interday analyses ranged from 0.79% to 8.01% and 3.30% to 11.43%, respectively, while the recoveries ranged from 82.0% to 105.7% (RSD < 7%, n = 3). The most probable structure of the inclusion complexes was proposed based on the findings from the molecular docking studies conducted using the PatchDock server.
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A bottom-up approach for synthesizing silver nanoparticles (AgNPs-GA) phytomediated by Garcinia atroviridis leaf extract is described. Under optimized conditions, the AgNPs-GA were synthesized at a concentration of 0.1 M silver salt and 10% (w/v) leaf extract, 1:4 mixing ratio of reactants, pH 3, temperature 32 °C and 72 h reaction time. The AgNPs-GA were characterized by various analytical techniques and their size was determined to be 5-30 nm. FTIR spectroscopy indicates the role of phenolic functional groups in the reduction of silver ions into AgNPs-GA and in supporting their subsequent stability. The UV-Visible spectrum showed an absorption peak at 450 nm which reflects the surface plasmon resonance (SPR) of AgNPs-GA and further supports the stability of these biosynthesized nanoparticles. SEM, TEM and XRD diffractogram analyses indicate that AgNPs-GA were spherical and face-centered-cubic in shape. This study also describes the efficacy of biosynthesized AgNPs-GA as anti-proliferative agent against human breast cancer cell lines, MCF-7 and MCF-7/TAMR-1. Our findings indicate that AgNPs-GA possess significant anti-proliferative effects against both the MCF-7 and MCF-7/TAMR-1 cell lines, with inhibitory concentration at 50% (IC50 values) of 2.0 and 34.0 µg/mL, respectively, after 72 h of treatment. An induction of apoptosis was evidenced by flow cytometry using Annexin V-FITC and propidium iodide staining. Therefore, AgNPs-GA exhibited its anti-proliferative activity via apoptosis on MCF-7 and MCF-7/TAMR-1 breast cancer cells in vitro. Taken together, the leaf extract from Garcinia atroviridis was found to be highly capable of producing AgNPs-GA with favourable physicochemical and biological properties.
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Antineoplásicos/síntese química , Antineoplásicos/farmacologia , Apoptose/efeitos dos fármacos , Neoplasias da Mama/patologia , Nanopartículas Metálicas/química , Prata/química , Prata/farmacologia , Antineoplásicos/química , Proliferação de Células/efeitos dos fármacos , Sobrevivência Celular/efeitos dos fármacos , Técnicas de Química Sintética , Garcinia/química , Química Verde , Humanos , Células MCF-7 , Extratos Vegetais/químicaRESUMO
This work describes the development of a new methodology based on magnetic nanoparticles assisted dispersive liquid-liquid microextraction (DLLME-MNPs) for preconcentration and extraction of chloramphenicol (CAP) antibiotic residues in water. The approach is based on the use of decanoic acid as the extraction solvent followed by the application of MNPs to magnetically retrieve the extraction solvent containing the extracted CAP. The coated MNPs were then desorbed with methanol, and the clean extract was analysed using ultraviolet-visible spectrophotometry. Several important parameters, such as the amount of decanoic acid, extraction time, stirring rate, amount of MNPs, type of desorption solvent, salt addition and sample pH, were evaluated and optimized. Optimum parameters were as follows: amount of decanoic acid: 200 mg; extraction time: 10 min; stirring rate: 800 rpm; amount of MNPs: 60 mg; desorption solvent: methanol; salt: 10%; and sample pH, 8. Under the optimum conditions, the method demonstrated acceptable linearity (R 2 = 0.9933) over a concentration range of 50-1000 µg l-1. Limit of detection and limit of quantification were 16.5 and 50.0 µg l-1, respectively. Good analyte recovery (91-92.7%) and acceptable precision with good relative standard deviations (0.45-6.29%, n = 3) were obtained. The method was successfully applied to tap water and lake water samples. The proposed method is rapid, simple, reliable and environmentally friendly for the detection of CAP.
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Clinacanthus nutans is a well-known herb that has been used as an alternative and therapeutic medicine, however more selective C. nutans extracts are needed. In this study, leaves were extracted with 80% methanol and further fractionated with n-hexane, dichloromethane, chloroform, n-butanol, and aqueous residue. Subsequently, the total phenolic content (TPC), total flavonoid content (TFC), antioxidant scavenging activity, and antiproliferative effects on breast cancer (Michigan Cancer Foundation-7 [MCF7]) and normal breast (Michigan Cancer Foundation-10A [MCF 10A]) cells of the extracts were measured. Additionally, molecular docking simulation of the major compounds from C. nutans extracts was conducted. The aqueous residue had the highest TPC and TFC, whereas the crude extract had the highest scavenging activity. Among the extracts, dichloromethane extract (CN-Dcm) was selected as it had the highest selectivity index (SI) (1.48). Then, the chosen extract (CN-Dcm) was proceed for further analysis. The compounds from CN-Dcm were identified using gas chromatography-mass spectrometry (GC-MS). The major compounds from CN-Dcm were further investigated through molecular docking studies. Palmitic acid and linolenyl alcohol were the compounds found in the CN-Dcm extract that exhibited the highest binding affinities with p53-binding protein Mdm-2. These results highlight the potential of C. nutans as a source of anticancer activities.
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Acanthaceae/química , Antineoplásicos Fitogênicos/farmacologia , Antioxidantes/farmacologia , Simulação de Acoplamento Molecular , Simulação de Dinâmica Molecular , Extratos Vegetais/farmacologia , Antineoplásicos Fitogênicos/química , Antineoplásicos Fitogênicos/isolamento & purificação , Antioxidantes/química , Antioxidantes/isolamento & purificação , Linhagem Celular Tumoral , Fracionamento Químico , Relação Dose-Resposta a Droga , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Conformação Molecular , Estrutura Molecular , Extratos Vegetais/química , Extratos Vegetais/isolamento & purificação , Folhas de Planta/químicaRESUMO
Plant essential oils are widely used in perfumes and insect repellent products. However, due to the high volatility of the constituents in essential oils, their efficacy as a repellent product is less effective than that of synthetic compounds. Using a nanoemulsion as a carrier is one way to overcome this disadvantage of essential oils. Nutmeg oil-loaded nanoemulsion (NT) was prepared using a high speed homogenizer and sonicator with varying amounts of surfactant, glycerol, and distilled water. Using a phase diagram, different formulations were tested for their droplet size and insect repellent activity. The nanoemulsion containing 6.25% surfactant and 91.25% glycerol (NT 6) had the highest percentage of protection (87.81%) in terms of repellent activity among the formulations tested for the 8 h duration of the experiment. The droplet size of NT 6 was 217.4 nm, and its polydispersity index (PDI) was 0.248. The zeta potential value was -44.2 mV, and the viscosity was 2.49 Pa.s at pH 5.6. The in vitro release profile was 71.5%. When the cytotoxicity of NT 6 at 400 µg/mL was tested using the MTS assay, cell viability was 97.38%. Physical appearance and stability of the nanoemulsion improved with the addition of glycerol as a co-solvent. In summary, a nutmeg oil-loaded nanoemulsion was successfully formulated and its controlled release of the essential oil showed mosquito repellent activity, thus eliminating the disadvantages of essential oils.
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Poly(ß-cyclodextrin-ionic liquid) grafted magnetic nanoparticles combined with 1-octanol as supramolecular solvents (SUPRASs) presenting new ferrofluid was developed and successfully applied in the dispersive liquid-phase microextraction of seven representative polycyclic aromatic hydrocarbons. One variable at-a-time (OVAT) analysis and response surface methodology (RSM) were used for efficient optimization of the main variables. The calibration curves were found to be linear in the range of 0.1-150 ng mL-1 with correlation of determinations (R2) ranging from 0.9944 to 0.9986. Detection limits ranged at 0.02-0.07 ng mL-1 for all studied PAHs. The intra and inter-day precision values (RSD %) were in the range of 1.80%-7.56% and 2.97%-8.23%, respectively. The ferrofluid showed a satisfactory reproducibility between 1.72% and 5.90%, and acceptable recovery values at 84%-110% were obtained for the real samples analysis. The optimized method was successfully applied to access the content safety of the PAHs studied in a variety of commercial food and beverages available in Malaysia.
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Hidrocarbonetos Policíclicos Aromáticos/análise , beta-Ciclodextrinas/química , Cromatografia Gasosa , Coloides , Líquidos Iônicos , Limite de Detecção , Microextração em Fase Líquida , Fenômenos Magnéticos , Reprodutibilidade dos TestesRESUMO
Poly(ß-cyclodextrin functionalized ionic liquid) immobilized magnetic nanoparticles (Fe3O4@ßCD-Vinyl-TDI) as sorbent in magnetic µ-SPE was developed for the determination of selected polycyclic aromatic hydrocarbons (PAHs) in rice samples coupled with gas chromatographic-flame ionization detector (GC-FID). The nanocomposite was characterized by various tools and significant parameters that affected the extraction efficiency of PAHs were investigated. The calibration curves were linear for the concentration ranging between 0.1 and 500⯵gâ¯kg-1 with correlation determinations (R2) from 0.9970 to 0.9982 for all analytes. Detection limits ranged at 0.01-0.18⯵gâ¯kg-1 in real matrix. The RSD values ranged at 2.95%-5.34% (intra-day) and 4.37%-7.05% (inter-day) precision for six varied days. The sorbents showed satisfactory reproducibility in 2.9% to 9.9% range and acceptable recovery values at 80.4%-112.4% were obtained for the real sample analysis. The optimized method was successfully applied to access content safety of selected PAHs for 24 kinds of commercial rice available in Malaysia.
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Contaminação de Alimentos/análise , Nanocompostos/química , Oryza/química , Hidrocarbonetos Policíclicos Aromáticos/análise , Microextração em Fase Sólida/métodos , Cromatografia Gasosa , Líquidos Iônicos/química , Limite de Detecção , Magnetismo , Malásia , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Microextração em Fase Sólida/instrumentação , beta-Ciclodextrinas/químicaRESUMO
In the field of medicine, nanomaterials, especially those derived using the green method, offer promise as anti-cancer agents and drug carriers. However, the biosafety of metallic nanoparticles used as anti-cancer agents remains a concern. The goal of this systematic review was to compare the cytotoxicity of different plant-mediated syntheses of metallic nanoparticles based on their potency, therapeutic index, and cancer cell type susceptibility in the hopes of identifying the most promising anti-cancer agents. A literature search of electronic databases including Science Direct, PubMed, Springer Link, Google Scholar, and ResearchGate, was conducted to obtain research articles. Keywords such as biosynthesis, plant synthesis, plant-mediated, metallic nanoparticle, cytotoxicity, and anticancer were used in the literature search. All types of research materials that met the inclusion criteria were included in the study regardless of whether the results were positive, negative, or null. The therapeutic index was used as a safety measure for the studied compound of interest. Data from 76 selected articles were extracted and synthesised. Seventy-two studies reported that the cytotoxicity of plant-mediated synthesis of metallic nanoparticles was time and/or dose-dependent. Biosynthesised silver nanoparticles demonstrated higher cytotoxicity potency compared to gold nanoparticles synthesised by the same plants (Plumbago zeylanica, Commelina nudiflora, and Cassia auriculata) irrespective of the cancer cell type tested. This review also identified a correlation between the nanoparticle size and morphology with the potency of cytotoxicity. Cytotoxicity was found to be inversely proportional to nanoparticle size. The plant-mediated syntheses of metallic nanoparticles were predominantly spherical or quasi-spherical, with the median lethal dose of 1â»20 µg/mL. Nanoparticles with other shapes (triangular, hexagonal, and rods) were less potent. Metallic nanoparticles synthesised by Abutilon inducum, Butea monosperma, Gossypium hirsutum, Indoneesiella echioides, and Melia azedarach were acceptably safe as anti-cancer agents, as they had a therapeutic index of >2.0 when tested on both cancer cells and normal human cells. Most plant-mediated syntheses of metallic nanoparticles were found to be cytotoxic, although some were non-cytotoxic. The results from this study suggest a focus on a selected list of potential anti-cancer agents for further investigations of their pharmacodynamic/toxicodynamic and pharmacokinetic/toxicokinetic actions with the goal of reducing the Global Burden of Diseases and the second leading cause of mortality.
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Ouro/toxicidade , Nanopartículas Metálicas/toxicidade , Plantas/metabolismo , Animais , Humanos , Tamanho da PartículaRESUMO
Polyaniline (PANI) modified magnetic nanoparticle (MNP) nanocomposites coated with newly synthesized dicationic ionic liquid (DICAT) forming MNP-PANI-DICAT were successfully synthesized as a potential material for the removal of Rhodamine B (RB) from water samples. The synthesized material was successfully characterized using a few techniques such as Fourier transform infrared spectroscopy (FT-IR), X-ray powder diffraction (XRD), thermo gravimetric analysis (TGA), Brunauer-Emmett-Teller (BET), and transmission electron microscopy (TEM) analysis. Several parameters have been optimized to enhance the efficiency of the removal process. The adsorption kinetics were investigated and the results showed that MNP-PANI-DICAT was best fitted to a pseudo-second order model for the adsorption of RB. As for the isotherm studies, Temkin's model was found to fit well with the adsorption isotherm of RB on MNP-PANI-DICAT. Other than that, thermodynamics results showed negative values of ΔG° for the adsorption of RB, which indicated that the process is thermodynamically feasible, spontaneous and chemically controlled at lower temperature. The negative value of enthalpy ΔH° (-40.41) indicated that the adsorption was an exothermic process. The percentage removal of RB was found to be 94.7% by MNP-PANI-DICAT under optimized conditions.