RESUMO
Four simple, specific, easy, precise and accurate spectrophotometric methods were developed for the first time to examine ciprofloxacin and metronidazole in combination, without having been separated beforehand by the developed methods. Ciprofloxacin and metronidazole were determined by utilizing advanced absorbance subtraction (AAS), spectrum subtraction, bivariate and ratio difference methods. Precision, repeatability, robustness, and accuracy were all determined to be within acceptable levels after each of these procedures underwent validation in accordance with ICH recommendations. Each method's benefits and drawbacks are illustrated, and the proposed and reported methodologies were statistically compared.
RESUMO
Catechol is a pollutant that can lead to serious health issues. Identification in aquatic environments is difficult. A highly specific, selective, and sensitive electrochemical biosensor based on a copper-polypyrrole composite and a glassy carbon electrode has been created for catechol detection. The novelty of this newly developed biosensor was tested using electrochemical techniques. The charge and mass transfer functions and partially reversible oxidation kinetics of catechol on the redesigned electrode surface were examined using electrochemical impedance spectroscopy and cyclic voltammetry scan rates. Using cyclic voltammetry, chronoamperometry, and differential pulse voltammetry, the characteristics of sensitivity (8.5699 µA cm-2), LOD (1.52 × 10-7 µM), LOQ (3.52 × 10-5 µM), linear range (0.02-2500 µM), specificity, interference, and real sample detection were investigated. The morphological, structural, and bonding characteristics were investigated using XRD, Raman, FTIR, and SEM. Using an oxidation-reduction technique, a suitable biosensor material was produced. In the presence of interfering compounds, it was shown that it was selective for catechol, like an enzyme.
RESUMO
The clinical significance of benzimidazole-containing drugs has increased in the current study, making them more effective scaffolds. These moieties have attracted strong research interest due to their diverse biological features. To examine their various biological significances, several research synthetic methodologies have recently been established for the synthesis of benzimidazole analogs. The present study aimed to efficiently and quickly synthesize a new series of benzimidazole analogs. Numerous spectroscopic techniques, including 1H-NMR, 13C-NMR, and HREI-MS, were used to confirm the synthesized compounds. To explore the inhibitory activity of the analogs against α-amylase and α-glucosidase, all derivatives (1-17) were assessed for their biological potential. Compared to the reference drug acarbose (IC50 = 8.24 ± 0.08 µM), almost all the derivatives showed promising activity. Among the tested series, analog 2 (IC50 = 1.10 ± 0.10 & 2.10 ± 0.10 µM, respectively) displayed better inhibitory activity. Following a thorough examination of the various substitution effects on the inhibitory capacity of α-amylase and α-glucosidase, the structure-activity relationship (SAR) was determined. We looked at the potential mechanism of how active substances interact with the catalytic cavity of the targeted enzymes in response to the experimental results of the anti-glucosidase and anti-amylase. Molecular docking provided us with information on the interactions that the active substances had with the various amino acid residues of the targeted enzymes for this purpose.
RESUMO
Common methodologies such as liquid-liquid extraction and solid-phase extraction are applied for the extraction of opioids from biological specimens i.e., blood and urine. Techniques including LC-MS/LC-MSMS, GC-MS, etc. are used for qualitative or quantitative determination of opioids. The goal of the present work is to design a green, economic, rugged, and simple extraction technique for famous opioids in human blood and urine and their simultaneous quantification by GC-MS equipped with an inert plus electron impact (EI) ionization source at SIM mode to produce reproducible and efficient results. Morphine, codeine, 6-acetylmorphine, nalbuphine, tramadol and dextromethorphan were selected as target opioids. Anhydrous Epsom salt was applied for dSPE of opioids from blood and urine into acetonitrile extraction solvent with the addition of sodium phosphate buffer (pH 6) and n-hexane was added to remove non-polar interfering species from samples. BSTFA was used as a derivatizing agent for GC-MS. Following method validation, the LOD/LLOQ and ULOQ were determined for morphine, codeine, nal-buphine, tramadol, and dextromethorphan at 10 ng/mL and 1500 ng/mL, respectively, while the LOD/LLOQ and ULOQ were determined for 6-acetylmorphine at 5 ng/mL and 150 ng/mL, respectively. This method was applied to real blood and urine samples of opioid abusers and the results were found to be reproducible with true quantification.
Assuntos
Nalbufina , Tramadol , Acetonitrilas , Analgésicos Opioides , Codeína/análise , Dextrometorfano , Cromatografia Gasosa-Espectrometria de Massas/métodos , Humanos , Morfina/análise , Derivados da Morfina/urina , Extração em Fase Sólida/métodos , Solventes , Detecção do Abuso de Substâncias/métodosRESUMO
Hexavalent chromium is a very poisonous oxyanion and has had a negative impact on human health. This study assessed the viability of removing chromium(vi) using micellar modified adsorbents. In this study, chromium(vi) was removed from locally accessible wheat bran using separate applications of anionic sodium dodecyl sulfate (SDS) and cationic cetyltrimethylammonium bromide (CTAB) surfactants. The initial chromium content (5-12 ppm), pH (2-12), adsorbent dose (1-6 g/100 mL), agitation time (15-240 min), agitation speed (50-300 rpm), and temperature (15-50 °C) were all varied in the adsorption investigation. Pseudo first-order and second-order kinetic models were utilized to analyze the kinetic investigation. To determine thermodynamic parameters, the van't Hoff relationship was used. The maximum result for chromium(vi) uptake was obtained as 87.7%, 83.5% and 98.9% for WB, SDS-mWB, and CTAB-mWB, respectively, at an agitation time of 240 min (i.e., 4 h), temperature (i.e., 25-30 °C), agitation speed (150 rpm). However, both WB and CTAB-mWB derives metal ion removal at lower pH levels (2-4), whereas SDS-mWB requires a pH between 4 and 6 for maximum percentage removal of Cr(vi). The equilibrium data of WB and SDS-mWB were modeled by the Langmuir adsorption isotherm, while the data of CTAB-mWB fitted well in the Freundlich isotherm model. The kinetic analysis of WB, SDS-mWB, and CTAB-mWB revealed that the pseudo-second-order kinetic model provides a thorough explanation for each of these adsorbents. It was found that CTAB-mWB can preferably be used for the removal of chromium(vi) due to its high affinity with adsorbate molecules and adsorption capacity.
RESUMO
The synthesis of MMT and poly(o-anisidine) (MMT/POA) clay nanocomposites was carried out by using the chemical oxidative polymerization of POA and MMT clay with POA, respectively. By maintaining the constant concentration of POA, different percentage loads of MMT clay were used to determine the effect of MMT clay on the properties of POA. The interaction between POA and MMT clay was investigated by FTIR spectroscopy, and, to reveal the complete compactness and homogeneous distribution of MMT clay in POA, were assessed by using scanning-electron-microscope (SEM) analysis. The UV-visible spectrum was studied for the optical and absorbance properties of MMT/POA ceramic nanocomposites. Furthermore, the horizontal burning test (HBT) demonstrated that clay nanofillers inhibit POA combustion.