BMC Chemistry最新文献

A simple, rapid, sensitive, and reliable spectrofluorimetric approach has been developed for the analysis of delafloxacin (DEL) in human plasma. The proposed method is based on the formation of a micellar fluorescent complex through the interaction of DEL with 2% sodium dodecyl sulfate (SDS) using a phosphate buffer (pH 4.2), producing a pronounced emission at 470 nm upon excitation at 380 nm. The experimental conditions that affected the one-pot synthesis were investigated and optimized. The calibration curve exhibited a linear relationship over a concentration range of 2.0–120.0 ng mL^–1, with detection (LOD) and quantitation limits (LOQ) 0.6 and 1.9 ng mL^–1, respectively. The designed approach was validated following the ICH and FDA guidelines, producing a precise analysis of DEL in its tablets and plasma samples with high recovery percentage. The results provide that the method possesses excellent eco-friendly properties, highlighting its strong compatibility with the principles of green chemistry.

Simple, accurate, and precise UV spectrophotometric methods were developed and validated for the simultaneous determination of olanzapine (OLA) and fluoxetine (FLU) in bulk powders and combined pharmaceutical formulations without prior separation steps. The methods employed advanced mathematical manipulation techniques using both the Constant Multiplication method (CM) coupled with Spectrum Subtraction (SS) and the Factorized Zero-Order method (FZM), which was also coupled with SS. These approaches utilized normalized and factorized spectra, respectively, to resolve the overlapping spectral profiles of the two drugs. Unlike conventional methods reported in the literature, such as derivative spectrophotometry, our approach enabled the extraction of each component in its original zero-order form, exhibiting spectral features identical to those of pure standards, which enhances accuracy and precision. A direct comparative evaluation of CM–SS and FZM–SS is presented, highlighting their respective analytical merits. The proposed methods demonstrated linearity over concentration ranges of 1.5–14 µg/mL and 3.5–35 µg/mL for OLA and FLU, respectively, with limits of detection of 0.15 µg/mL (OLA) and 0.38 µg/mL (FLU), and limits of quantification of 0.47 µg/mL (OLA) and 1.15 µg/mL (FLU), confirming the high sensitivity of the methods. They were successfully applied for the simultaneous determination of OLA and FLU in synthetic mixtures and in their combined dosage form with excellent accuracy and precision. Furthermore, the environmental and practical merits of the methods were evaluated through the principles of Green Analytical Chemistry (GAC) and White Analytical Chemistry (WAC). The greenness of the proposed spectrophotometric method was evaluated by the Analytical Greenness Metric (AGREE). The overall method performance, including validation efficiency, ecological impact, and practicality, was systematically evaluated using the RGB-based WAC approach.

A series of novel heterocyclic compounds based on 5-methyl-1-(p-tolyl)-1H-1,2,3-triazole-4-carbohydrazide were designed, synthesized, and evaluated for antioxidant activity. The synthesized derivatives included phthalimide (NA-1, NA-2), cyanoacetamide (NA-3), pyridine-based (NA-4), and hydrazonoyl cyanide (NA-5 to NA-8) analogs. Structural confirmation was achieved through IR, NMR (¹H and ¹³C), and MS analyses. Antioxidant activity was assessed using the DPPH radical-scavenging assay, with ascorbic acid as a reference. Compounds NA-2 (IC₅₀ = 0.072 ± 0.272 mg/mL), NA-5 (IC₅₀ = 0.029 ± 0.135 mg/mL), and NA-6 (IC₅₀ = 0.096 ± 0.085 mg/mL) showed notable activity. DFT calculations suggested favorable electronic properties and hydrogen-bonding potential, supporting their antioxidant behavior. In silico pharmacokinetic analysis (SwissADME) showed acceptable drug-likeness with limited violations in some analogs with Lipinski’s rule of five, indicating acceptable drug-likeness. Bioavailability scores were generally 0.55, except NA-7 (0.11).

A Schiff base ligand, H₂L, was obtained from the condensation of pyridine-2,6-dicarbohydrazide and cinnamaldehyde and was further complexed with Co²⁺, Cu²⁺, and Cd²⁺ ions. The coordination complexes were then analyzed by normal spectroscopic/microscopic analyses (FT-IR, UV–visible, ¹H-NMR, ¹³C-NMR, ESR, PXRD, EDX, and TEM) and other conventional physicochemical analyses (C.H.N microanalysis, molar conductivity, and elemental analysis, molar conductivity) beside (TG/DTA) thermal analysis. Structural analysis revealed mononuclear octahedral geometries for the Co²⁺ and Cd²⁺ chelates through pincer ONO chelation, while the Cu²⁺ complex showed a ligand-supported dinuclear square planer arrangement via two NO hydrazone scaffolds. Computational studies based on the DFT theory postulated the reactivity and spectral trends for the free ligand and metal chelates. The electrochemical properties for the ligand and its complexes were analyzed using cyclic voltammetry and revealed quasi-reversible/irreversible electrochemical behaviors. Biological analyses confirmed the efficiency of the Schiff base and its metal complexes for antibacterial, antifungal, DPPH-antioxidant, and DNA-binding capabilities and exhibited in-vitro cytotoxicity towards HepG2 and MCF-7 cell lines.

In this work, a new, sensitive, precise, accurate, and eco-friendly spectrofluorometric method for the detection of Bosentan in human plasma and pharmaceutical dosage form was developed, using silver nanoparticles (AgNPs) as an efficient fluorescence sensing probe. The general concept used in this approach is based on collisional quenching of AgNPs fluorescence intensity. Over the concentration range of 0.02 to 0.12 µg/mL, the quenching impact of BOS on AgNPs increased as its concentration increased. The suggested method’s greenness was assessed using two metric systems: the Analytical Eco-scale (AES) with a score of 80 and the AGREE greenness assessment tool with a score of 0.68.

Graphical Abstract

A simple, fast, and eco-friendly high-performance liquid chromatography (RP-HPLC) method has been developed for the concurrent quantification of lidocaine and fluorescein, employing ultraviolet detection at a wavelength of 220 nm. The chromatographic separation was applied under isocratic conditions on an Inertsil^© C18 column (250 mm × 4.6 mm, 3.5 μm particle size), utilizing a mobile phase consisting of acetonitrile and water containing 0.3% triethylamine (adjusted to pH 3.5) in a volumetric ratio of 75:25%v/v. The analysis was performed at a constant flow rate of 1.0 mL/min. Method validation was conducted in accordance with the guidelines of International Council for Harmonisation (ICH), confirming that the procedure is accurate, precise, robust, and exhibits linearity within the concentration ranges of 20–280 µg mL^− 1 for lidocaine and 1–20 µg mL^− 1 for fluorescein. The detection limits were determined to be 5.27 µg mL^− 1 for lidocaine and 0.29 µg mL^− 1 for fluorescein, while the quantitation limits were 15.97 µg mL^− 1 and 0.88 µg mL^− 1, respectively. This analytical method was effectively applied to quantify both compounds in a combined ophthalmic formulation, yielding mean recovery values of 100.80 ± 0.67% for lidocaine and 100.13 ± 0.99% for fluorescein, thereby demonstrating its suitability for routine quality control purposes. The environmental impact of the proposed method was evaluated using Analytical Eco-Scale, GAPI, and AGREE tools, yielding an Eco-Scale score 78 and an AGREE score of 0.63, indicating acceptable greenness based on quantitative assessment.