Search Results (242)

Detecting pharmaceuticals in environmental matrices, particularly in wastewater, is crucial due to their potential environmental occurrence and unpredictable ecological and health-related consequences. These substances, often present in trace amounts, require highly sensitive and selective analytical methods for effective monitoring. A modified version of the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was evaluated to evaluate 18 pharmaceuticals and 2 metabolites in wastewater samples using liquid chromatography with tandem mass spectrometry (LC-MS/MS). The method’s performance was assessed using linearity, recovery, precision, limits of quantification (LOQ) and detection (LOD), and the matrix effect (ME). The final method was based on acetonitrile, Na₂EDTA, citrate buffer, and graphene oxide (GO). Finally, the calibration curves prepared in acetonitrile and the matrix extract showed a correlation coefficient of 0.99. Most of the compounds had LOQ values lower than 0.5 μg⋅mL⁻¹. Recoveries were achieved in the 70–98% range, with RSD lower than 13%. GO allowed the elimination of the ME, which occurred in the range of −11% to 15%. The results indicate that a low-cost and straightforward method is suitable for routinely monitoring pharmaceuticals in wastewater, which is crucial for minimizing the impact of pollutants on aquatic ecosystems. Full article

Rapid, safe, and field-deployable molecular diagnostics are crucial for the effective management of infectious disease outbreaks, particularly those involving highly infectious pathogens, which can produce clinical symptoms similar to less infectious pathogens, thus raising potential biosafety concerns. In this study, we evaluated DNA/RNA Defend Pro (DRDP) buffer, a novel viral-inactivating transport medium designed to stabilize nucleic acids and allow direct PCR without nucleic acid extraction. To ensure critical qPCR parameters were not compromised by using DRDP, we conducted serial dilution tests using herpes simplex viruses 1 and 2 (HSV-1, HSV-2) and varicella-zoster virus (VZV), comparing DRDP to standard universal transport medium (UTM). Detection sensitivity, determined by cycle quantification (Cq) values, favored DRDP, as UTM samples required a 2–3-fold dilution to mitigate PCR inhibition. DRDP maintained reliable PCR compatibility at reaction volumes containing up to 25% buffer. At higher DRDP concentrations (30–35%), PCR inhibition occurred due to EDTA content but was fully reversible by adding supplemental magnesium. Furthermore, DRDP samples did not require an initial 95 °C thermal lysis step, thus simplifying the procedure without reducing PCR sensitivity or efficiency. Full article

The present study compared the adsorption properties of two plant materials and the waste products after their essential oil extraction for removing Cu(II) ions from contaminated water. Methods like SEM, XRD, nitrogen adsorption, DTA, TGA, FTIR, and XPS were used for characterization of the materials. All materials showed similar porosity and structure, favoring Cu(II) biosorption. The effects of contact time, pH, temperature, sample amount, and initial metal concentration on Cu(II) removal were examined. Optimal pH was 4, with equilibrium reached in less than 10 min. Temperature and sample amount do not significantly influence the biosorption. The experimental data were fitted to the Langmuir, Freundlich, and Dubinin–Radushkevich isotherm models, and maximum adsorption capacities were calculated. The four plant materials proved to be effective biosorbents for removing copper ions from contaminated water. Desorption experiments using 1 M HNO₃ and 0.1 M EDTA showed 100% recovery. The reusability of the most effective biosorbent was confirmed through four adsorption/desorption cycles with EDTA. This material was also used to study the possibilities of purifying a real sample of contaminated water. Full article

Background: This study is the first to investigate the association between colorectal cancer (CRC) risk and the hMLH1 −93G>A and hMSH2 1032G>A polymorphisms of mismatch repair (MMR) genes in the Azerbaijani population. Methods: Peripheral blood samples containing EDTA were collected from the study subjects (134 patients and 137 controls), and genomic DNA was extracted using the non-enzymatic salting-out method. Genotypes were determined by polymerase chain reaction–restriction fragment length polymorphism (PCR-RFLP), and the results were visualized through agarose gel electrophoresis. Results: Overall, no statistically significant correlation was observed between CRC risk and the hMLH1 −93G>A polymorphism in the heterozygous GA (OR = 0.760; 95% CI = 0.374–1.542; p = 0.446), the mutant AA (OR = 1.474; 95% CI = 0.738–2.945; p = 0.270), or the A allele (OR = 1.400; 95% CI = 0.984–1.995; p = 0.062). However, in contrast to the dominant model, a statistically significant association was found between the recessive model and an increased CRC risk, with an odds ratio of 1.788 (95% CI = 1.102–2.900; p = 0.018). The hMLH1 −93G>A polymorphism was identified at a significantly higher frequency across the TNM stages, with the distribution showing statistical significance (p < 0.05). Additionally, no statistically significant association was observed between the hMSH2 1032G>A polymorphism and CRC risk. Conclusions: Although no overall association was observed for hMLH1 −93G>A, our findings suggest a potential link with increased colorectal cancer risk under the recessive model in the Azerbaijani population. Further studies are warranted to confirm this model-specific association and investigate the underlying biological mechanisms. Full article

Background/Objectives: We developed and validated a robust and simple LC–MS/MS method for the simultaneous quantification of amoxicillin and clavulanate in human plasma relative to previously reported methods. Methods: Amoxicillin; clavulanate; and an internal standard, 4-hydroxytolbutamide, in human K₂-EDTA plasma, were deproteinized with acetonitrile and then subjected to back-extraction using distilled water–dichloromethane. Separation was performed on a Poroshell 120 EC-C₁₈ column with a mobile-phase gradient comprising 0.1% aqueous formic acid and acetonitrile at a flow rate of 0.5 mL/min within 6.5 min. The negative electrospray ionization modes were utilized to monitor the transitions of m/z 363.9→223.1 (amoxicillin), m/z 198.0→135.8 (clavulanate), and m/z 285.0→185.8 (4-hydroxytolbutamide). Results/Conclusions: Calibration curves exhibited linear ranges of 10–15,000 ng/mL for amoxicillin (r ≥ 0.9945) and 20–10,000 ng/mL for clavulanate (r ≥ 0.9959). Intra- and inter-day’s coefficients of variation, indicating the precision of the assay, were ≤7.08% for amoxicillin and ≤10.7% for clavulanate, and relative errors in accuracy ranged from −1.26% to 10.9% for amoxicillin and from −4.41% to 8.73% for clavulanate. All other validation results met regulatory criteria. Partial validation in lithium–heparin, sodium–heparin, and K₃-EDTA plasma confirmed applicability in multicenter or large-scale studies. This assay demonstrated itself to be environmentally friendly, as assessed by the Analytical GREEnness (AGREE) tool, and was successfully applied to a clinical pharmacokinetic study of an Augmentin^® IR tablet (250/125 mg). The inter-individual variabilities in clavulanate exposures (AUC_t and C_max) were significantly greater than in amoxicillin, and they may inform the clinical design of future drug–drug interaction. Full article

The probable solid phases controlling phosphorus (P) salts solubility in goat, swine, chicken, and dairy manures were investigated using chemical modeling software, Visual Minteq, coupled with serial dilution and EDTA extraction. In the serial dilution scheme, the manure (wet weight) to water ratios (MWR) used were 1:1, 1:2, 1:5, 1:10, 1:50, and 1:100. The EDTA concentrations used were 1, 5, and 10 mmol L⁻¹ at the 1:50 MWR. The total elemental concentrations in serially diluted samples were measured by ICP-OES, while in the EDTA extracts concentrations were measured by ICP-OES and P was also measured by the molybdate blue-P method. The percentage of total P dissolved from goat, swine, chicken, and dairy manure using serial dilution at 1:10 MWR was 4, 6, 7, and 34% of the total P; while at 1:100 MWR it was 44, 35, 36, and 65%, respectively. Chemical modeling suggested that between 1:1 to 1:10 MWR, Mg-phosphates, primarily struvite, was the probable solid phase controlling P salts solubility in all manures, except dairy. At the 1:50 and 1:100 MWR, the solid phases controlling P solubility shifted from Mg-phosphate to Ca-phosphate minerals in goat, swine, and chicken manures. The use of ICP or molybdate blue for chemical modeling showed the same solid phases in the EDTA extracts. From the EDTA extractions, it was determined that 5 mmol L⁻¹ EDTA lowered Ca and Mg activities that no mineral phases likely remained in goat, swine, and chicken manures. In conclusion, under the conditions of this study, P dissolution from salts present in manure is controlled by the cation concentration in solution. Full article

The effect of root canal irrigants on the mechanical properties of dentin is crucial in endodontic treatment planning. While antiseptics such as sodium hypochlorite and EDTA are widely used, their potential to weaken dentin structure remains a concern. Polyhexanide-based formulations may offer a safer alternative. To assess the impact of a polyhexanide-based antiseptic composition, compared to standard irrigants, on the microhardness, Young’s modulus, and elastic deformation energy of dentin. Sixty extracted human teeth were sectioned and polished to prepare dentin samples. Baseline measurements of Vickers microhardness, Young’s modulus, and elastic deformation work were performed using a Microhardness Tester (CSM Instruments, Switzerland) with a Berkovich indenter. Samples were then divided into six groups (n = 10 per group) and exposed to different irrigants (NaCl 0.9%, NaOCl 3%, chlorhexidine 2%, EDTA 17%, and polyhexanide-based solutions—0.1% and 0.2% Lavasept). Post-treatment measurements were performed. Statistical analysis was conducted using non-parametric tests with Bonferroni correction. Sodium hypochlorite (3%) caused the most pronounced reduction in dentin microhardness and mechanical strength, though not always statistically significant. Polyhexanide-based solutions (0.1% and 0.2% Lavasept) showed a milder effect, with statistically significant changes observed only in elastic deformation energy for 0.2% polyhexanide. EDTA treatment led to severe surface destruction, precluding reliable post-treatment measurements. Polyhexanide-based irrigants demonstrated a more favorable impact on dentin mechanical properties compared to traditional irrigants, supporting their potential use in endodontic protocols aimed at preserving dentin integrity. Full article

Background: The purpose of this study was to analyze the accuracy of two apex locators using seven different canal irrigants. Methods: Forty multi-rooted extracted teeth were included in this study. The actual canal length (ACL) was determined using a #10 file until the tip was visualized (12× magnification) just within the apical foramen (AF). The teeth were placed in a conductive medium of alginate to test the ACL and electronic canal length (ECL) using both apex locators in various conditions. Seven irrigant solutions were used in the root canal: 0.9% saline, FileEZE EDTA 19%, Glyde EDTA 17%, Consepsis V Chlorhexidine 2% CHX, Chlorcid 3%, citric acid 20%, and EDTA 18%. Results: Within a range of ±0.5 mm from the ACL, Raypex showed an accuracy of 87.5% with 0.9% saline solution, 82.5% with Chlorcid 3%, and 75% with Consepsis V CHX 2% solution. The Ipex showed an accuracy of 82.5% with 0.9% saline solution, 80% with Chlorcid 3%, and 70% with Consepsis V CHX 2% solution. The differences among the canal irrigants were significant for both the Raypex (p = 0.021) and Ipex (p < 0.0001) devices. The mean values showed the greatest variations in ECL accuracy with the combination of Raypex and EDTA 18% (p = 0.042) and with the Ipex and Glyde EDTA 17% (p = 0.026). Conclusions: Canal irrigants have an impact on the accuracy of apex locators. The apex locators showed an accuracy of 80% and greater when 0.9% saline and Chlorcid 3% solutions were used. Full article

This research aimed to evaluate how different chemical forms of key nutrients, delivered through an advanced foliar product (PRO) and a standard formulation (TRA), influence maize performance when grown on contrasting soil types. Each fertilizer provided a set of macro- and micronutrients, including nitrogen, phosphorus, potassium, boron, copper, iron, manganese, molybdenum, and zinc, along with trace elements such as chromium, iodine, lithium, and selenium. In TRA, Fe and Zn were complexed with EDTA, and trace elements were present in mineral form. In PRO, Fe and Zn were chelated with amino acids, and trace elements were bound to plant extracts. The study examined increasing doses of PRO and their potential toxicity. Both fertilizers improved maize biomass: fresh weight increased by 5–8% and dry weight by 8–14%, depending on the dose. At the lowest dose, yields were similar. However, PRO was more effective in biofortifying maize with iron and zinc on sandy soil, increasing levels by 16% and 7% compared to TRA at the lowest dose and up to 29% at the highest dose. PRO was well tolerated at higher doses. No significant differences were observed between the second and third doses of PRO, suggesting reduced efficacy at the highest dose. Full article

In the search for new alternatives for controlling parasitic agents, proteases from Beauveria bassiana stand out. The aim of this study was to evaluate in silico and in vitro the ovicidal potential of B. bassiana proteases on Eurytrema pancreaticum Janson, 1889 (Dicrocoeliidae) eggs. Beauveria bassiana Bals. -Criv., 1835 (Cordycipitaceae) (IP 361) was cultivated for enzymatic production. Proteins were precipitated with acetone (1:4 ratio), and specific activity was determined. Protease profiles were assessed via zymography, and inhibition by phenylmethylsulfonyl fluoride (PMSF) and ethylenediaminetetraacetic acid (EDTA) was tested. Three-dimensional models of the proteases were generated. Eurytrema pancreaticum eggs were used for the in vitro anthelmintic evaluation of the proteases. The results showed that precipitation significantly concentrated proteolytic activity (p < 0.01) compared to the crude extract. However, no chitinase activity was detected. The proteolytic profile of the precipitate revealed five bands with molecular weights from 25.6 to 66.9 kDa. In the in vitro tests, the proteases significantly (p < 0.01) reduced the number of intact E. pancreaticum eggs by 53% compared to the control with denatured enzymes. These findings highlight the ovicidal potential of B. bassiana proteases, though further studies are needed to confirm their application in parasite control. Full article

The increasing demand for lithium-ion batteries (LIBs) and their limited lifespan emphasize the urgent need for sustainable recycling strategies. This study investigates the application of tetrabutylphosphonium-based ionic liquids (ILs) as alternative leaching agents for recovering critical metals, Li(I), Co(II), Ni(II), and Mn(II), from spent NMC cathode materials. Initial screening experiments evaluated the leaching efficiencies of nine tetrabutylphosphonium-based ILs for Co(II), Ni(II), Mn(II), and Li(I), revealing distinct metal dissolution behaviors. Three ILs containing HSO₄⁻, EDTA²⁻, and DTPA³⁻ anions exhibited the highest leaching performance and were selected for further optimization. Key leaching parameters, including IL and acid concentrations, temperature, time, and solid-to-liquid ratio, were systematically adjusted, achieving leaching efficiencies exceeding 90%. Among the tested systems, [TBP][HSO₄] enabled near-complete metal dissolution (~100%) even at room temperature. Furthermore, an aqueous biphasic system (ABS) was investigated utilizing [TBP][HSO₄] in combination with ammonium sulfate, enabling the complete extraction of all metals into the salt-rich phase while leaving the IL phase metal-free and potentially suitable for reuse, indicating the feasibility of integrating leaching and extraction into a continuous, interconnected process. This approach represents a promising step forward in LIB recycling, highlighting the potential for sustainable and efficient integration of leaching and extraction within established hydrometallurgical frameworks. Full article

Squid is rich in polyunsaturated fatty acids (PUFAs), especially docosahexaenoic acid (DHA) and eicosapentaenoic acid (EPA), which exert various human health benefits. Pan-fried squid is a popular processed product beloved by consumers. However, the PUFAs of squid can be severely oxidized during thermal processing, which will result in the reduction in nutritional value and generation of harmful compounds like aldehydes. In this study, flavonoids extracted from coconut exocarp (CEF) and the metal ion chelating agent disodium ethylenediaminetetraacetate (EDTA-2Na) were used to inhibit lipid oxidation during the frying of squid, with the lipid oxidation level, the changes in fatty acid composition, and aldehyde concentrations being examined by gas chromatography mass spectrometry and high-performance liquid chromatography mass spectrometry. Results indicated that during pan-frying, the peroxide value, thiobarbituric acid value, and total oxidation value increased significantly, while the contents of EPA and DHA decreased significantly, and the concentrations of most aldehydes increased in a time- and temperature-dependent pattern. Both CEF and EDTA-2Na treatments inhibited these changes; comparatively, the CEF treatment was significantly better than that of EDTA-2Na. For instance, the CEF treatment inhibited the generation of HHE by 31.90%, 33.24%, and 19.73%, respectively, after pan-frying of squid at 180 °C for 6, 8, and 10 min, while the corresponding values for HNE were 22.65%, 18.96%, and 17.28% respectively. These results suggested that CEF can improve the oxidative stability of squid lipids during pan-frying and reduce the generation and accumulation of aldehydes and improve the security of processed squid products. Full article

The antioxidant capacity and modulation of oxidative stress by industrially processed açaí pulp extract from the Amazon (APEA) and its major anthocyanins, cyanidin 3-glucoside (C3G) and cyanidin-3-O-rutinoside (C3R), were evaluated as potential strategies for preventing cardiovascular diseases. The APEA was chemically characterized using ultrafast liquid chromatography-mass spectrometry (UFLC-MS), which revealed six main phenolic compounds. Notably, 9-(2,3-dihydroxypropoxy)-9-oxononanoic acid, acanthoside B, roseoside, cinchonine, and nonanedioate were identified for the first time in açaí extracts. In vitro antioxidant assays demonstrated that APEA exhibited strong DPPH- and ABTS-radical-scavenging activities (up to 80% inhibition and 65 mmol TE/100g DW, respectively) and showed ferrous- and copper-ion-chelating activities comparable to those of EDTA-Na₂ at higher concentrations (up to 95% inhibition). Hydroxyl and superoxide radical scavenging activities reached 80% inhibition, similar to that of ascorbic acid. In H₂O₂-treated H9c2 cardiomyocytes, APEA significantly reduced the intracellular ROS levels by 46.9%, comparable to the effect of N-acetylcysteine. APEA also attenuated menadione-induced oxidative stress in H9c2 cells, as shown by a significant reduction in CellROX fluorescence (p < 0.05). In vivo, APEA (100 mg/kg) significantly reduced CCl-induced hepatic lipid peroxidation (MDA levels), restored glutathione (GSH), and increased the antioxidant enzymes CAT, GPx, and SOD, demonstrating superior effects to C3G and C3R, especially after 21 days of treatment (p < 0.001). These findings suggest that Amazonian açaí pulp (APEA) retains potent antioxidant activity after industrial processing, with protective effects against oxidative damage in cardiomyocytes and hepatic tissue, highlighting its potential as a functional food ingredient with cardioprotective and hepatoprotective properties. Full article

Background and Objectives: Successful endodontic treatment requires thorough disinfection and removal of the smear layer to prevent reinfection. However, conventional irrigants like sodium hypochlorite (NaOCl) and ethylenediaminetetraacetic acid (EDTA) can compromise dentin integrity. This study assessed the efficacy of the Synergistic Microbicidal and Ablative Root canal Technique (SMART), which integrates AromaRoot, a biocompatible irrigation solution based on quaternary ammonium compounds, with 980 nm diode laser activation, to enhance bacterial reduction and smear layer removal. Materials and Methods: Sixty extracted single-rooted human teeth were inoculated with Enterococcus faecalis and divided into four treatment groups using NaOCl, AromaRoot, and 980 nm laser, either alone or in combination. Bacterial counts were measured as colony-forming units per milliliter (CFU/mL). For smear layer analysis, 56 extracted teeth were prepared and irrigated using EDTA, AromaRoot, and laser activation, followed by scanning electron microscopy to evaluate dentinal tubule exposure. Data were analyzed using Kruskal–Wallis and ANOVA. Results: The combination of AromaRoot, NaOCl, and laser activation achieved a 99.00% bacterial reduction (from 8082 to 60 CFU/mL, p < 0.001), outperforming NaOCl alone (98.34%, 131 CFU/mL). For smear layer removal, AromaRoot with laser achieved 78.5% open dentinal tubules in the apical third, significantly higher than EDTA alone (64.5%, p < 0.05), though EDTA remained superior in the coronal third (89.0% vs. 81.0%, p > 0.05). Conclusions: The SMART technique significantly improves both disinfection and smear layer removal in root canal therapy, particularly in the apical region. These findings suggest that AromaRoot, especially when laser-activated, may serve as a safe and effective alternative to conventional irrigants, warranting further clinical evaluation. Full article

A high-throughput method for the determination of a variety of chemical hazards in poultry muscle and egg samples was established via ultra-performance liquid chromatography–tandem triple quadrupole mass spectrometry (UPLC–QqQ-MS). The sample preparation procedure was developed based on this quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and validated for 280 chemical hazards potentially present in poultry products. The target compounds in poultry samples were extracted with a 1% formic acid–acetonitrile solution (15:85, v/v), and the metal ions in the matrix were chelated by adding ethylenediaminetetraacetic acid disodium salt (Na₂EDTA). The supernatant was purified using Enhanced Matrix Removal (EMR) lipid sorbent. Chromatographic gradient separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with multiple reaction monitoring (MRM) under both negative- and positive-ion mode. Internal standard calibration or matrix-matched calibration was used for the quantitation. The results showed that good linearity was achieved for each target compound with correlation coefficients (R²) ≥ 0.99. The limits of detection (LODs) ranged from 0.05 to 10 µg/kg, and the acceptable limits of quantification (LOQs) were determined to be 0.1–20 µg/kg for all 280 compounds. Approximately 90% of the target compounds exhibited mean recoveries ranging from 60% to 120%, with relative standard deviations (RSDs) within 16.2%. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs due to its easy operation and high accuracy. It was applied in real sample detection, and 43 chemicals including metronidazole were found in 211 poultry samples, with a concentration range of 0.11–638 μg/kg. Full article