The aim of this study was to create nanoparticles of human serum albumin immobilized with anti-TB drugs (rifampicin, isoniazid) using the desolvation method. Central Composite Design (CCD) was applied to study the effect of albumin, urea, L-cysteine, rifampicin and isoniazid concentration on particle size, polydispersity and loading degree of the drugs. The optimized nanoparticles were spherical in shape with an average particle size of 216.7 ± 3.7 nm and polydispersity of 0.286 ± 4.9. The loading degree of rifampicin and isoniazid in the optimized nanoparticles were 44% and 27%, respectively. The obtained nanoparticles were examined by Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC); the results showed the absence of drug–polymer interactions. The drug release from the polymer matrix was studied using dialysis membranes.
Despite the large number of works on the synthesis of polylactide-co-glycolide (PLGA) nanoparticles (NP) loaded with antituberculosis drugs, the data on the influence of various factors on the final characteristics of the complexes are quite contradictory. In the present study, a comprehensive analysis of the effect of multiple factors, including the molecular weight of PLGA, on the size and stability of nanoparticles, as well as the loading efficiency and release of the antituberculosis drug rifampicin (RIF), was carried out. Emulsification was carried out using different surfactants (polyvinyl alcohol, Tween 80 and Pluronic F127), different aqueous-to-organic phase ratios, and different solvents (dichloromethane, dimethyl sulfoxide, ethyl acetate). In this research, the PLGA nanoemulsion formation process was accompanied by ultrasonic dispersion, at different frequencies and durations of homogenization. The use of the central composite design method made it possible to select optimal conditions for the preparation of PLGA-RIF NPs (particle size 223 ± 2 nm, loading efficiency 67 ± 1%, nanoparticles yield 47 ± 2%). The release of rifampicin from PLGA NPs was studied for the first time using the flow cell method and vertical diffusion method on Franz cells at different pH levels, simulating the gastrointestinal tract. For the purpose of the possible inhalation administration of rifampicin immobilized in PLGA NPs, their mucoadhesion to mucin was studied, and a high degree of adhesion of polymeric nanoparticles to the mucosa was shown (more than 40% within 4 h). In the example of strain H37Rv in vitro, the sensitivity of Mycobacterium tuberculosis to PLGA-RIF NPs was proven by the complete inhibition of their growth.
Salvia dumetorum Andrz. ex Besser is a promising non-pharmacopoeial plant species with traditional medicinal potential. This study aimed to determine the optimal microwave-assisted extraction (MAE) conditions for obtaining a polyphenol-rich ethanolic extract from the S. dumetorum leaves. Dried and powdered leaves were extracted using 40% ethanol with different power of microwaves varying from 200 to 800 W and time of extraction 2–8 min. The extract was filtered, concentrated, and evaluated for yield, identification of phenolic compounds using high-performance liquid chromatography (HPLC), total phenolic content (TPC), and total flavonoid content (TFC). Extraction yields ranged from 2.20% to 25.80% based on dry weight. TPC and TFC were determined using Folin–Ciocalteu and aluminum chloride colorimetric assays, respectively, and are expressed as mg GAE/g and mg RUE/g of dry extract. The antioxidant activity of the extracts was evaluated using the DPPH (2,2-diphenyl-1-picrylhydrazyl radical) assay. According to HPLC analysis, the main phenolic components of the extracts were rosmarinic acid (1.78–2.95 mg/mL), chlorogenic acid (0.31–0.54 mg/mL), caffeic acid (0.11–0.20 mg/mL), rutin (up to 0.47 mg/mL) and ferulic acid (0.13–0.33 mg/mL); traces of myricetin were found only in isolated samples. The optimum extraction conditions were found to be 400 W microwave power, 8 min extraction time, one MAE cycle, and a 1:30 g/mL solvent-to-material loading ratio; TPC and TFC were evaluated as 35.23 ± 0.50 mg GAE/g DW and 19.94 ± 0.14 mg RuE/g DW, respectively, indicating the highest yield of polyphenolic compounds, antioxidant potential inhibiting 96.68% ± 0.27 of DPPH radicals, and IC50 = 10.24 µg/mL. These findings highlight the efficiency of MAE in producing a bioactive ethanolic extract of S. dumetorum, which can be further explored for potential applications as a natural antioxidant in pharmaceutical or cosmetic formulations.
Laser-Induced Breakdown Spectroscopy (LIBS) has proven to be a versatile analytical technique for the detection of trace elements in various sample matrices, including hydrocarbon materials. This study focuses on optimizing LIBS parameters to enhance the accuracy and sensitivity of vanadium (V) detection in coal and hydrocarbon-based samples. A probabilistic-deterministic design of experiments (PDDoE) was employed to fine-tune key factors such as lamp energy, delay, and the number of laser impulses. Optimal settings (lamp energy: 20 J, Q-SW1: 111 µs, ΔQ-SW: 3 µs, delay: 1 µs, and 100 impulses) significantly improved the intensity of vanadium spectral lines, particularly in samples with low concentrations, achieving a limit of detection (LoD) of 0.03 % for vanadium. Calibration models were developed using Partial Least Squares Regression (PLS-R) and Multiple Linear Regression (MLR) methods. These models achieved an accuracy of 95–98 % for vanadium quantification in coal ash and hydrocarbon samples. Validation of the developed method was performed using Atomic Absorption Spectroscopy (AAS), demonstrating good correlation between predicted and experimental values. Although the method requires sample preparation and shows lower accuracy than traditional AAS, it offers a practical solution for cases where sample dissolution is difficult, such as the analysis of glasses, enamels, and geological materials. Furthermore, the method demonstrated satisfactory results in field applications, where rapid on-site analysis with portable LIBS devices was required.
1 January 2021 in Bulletin of the Karaganda University. "Chemistry" Series
The research aims to optimize and minimize the number of experiments to obtain polylactide-co-glycolide (PLGA) nanoparticles (NPs) immobilized with antituberculosis (anti-TB) drug — isoniazid (INH) by applying the Taguchi method and Design Expert statistical software. Several experiments were performed with varying parameters, namely polymer/drug ratio, polyvinyl alcohol (PVA) concentration, the ratio of organic solvent to the aqueous phase, and solvent type. Three different levels and a fractional factorial design were derived for each parameter, particularly the standard orthogonal array (OA) L9. Drug-loaded nanoparticles were prepared by the double emulsion method. The results were obtained from 9 runs indicated particle sizes ranging from 152.2±6.4 nm to 496.4±9.5 nm. These results were used to predict the optimum conditions for synthesizing INH-PLGA particles. The calculated data correlate well with the experimental data. INH-PLGA NPs were obtained with a mean size and polydispersity of nanoparticles of 152.2±2.25 nm and 0.279±0.03, respectively. Scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry were carried out to characterize the obtained nanoparticles. The degree of drug release from PLGA NPs was studied, and the results showed that PLGA prolonged the release of INH from the polymer matrix