Current Issue : October-December Volume : 2025 Issue Number : 4 Articles : 5 Articles
Retinoids are used in cosmetics as anti-aging ingredients, along with other substances. However, due to limitations in use (such as photodegradation), it seems necessary to look for retinoid alternatives to be applied in cosmetic products. Bakuchiol, a natural alternative of retinoids, isolated from Psolarea corylifolia, is one such compound. It has great cosmetic potential and its mechanism of action is not yet fully explored. From the point of view of the bioactive compound, it is also essential to develop a method for rapid quality control of cosmetic preparations containing bakuchiol. The aim of this study was to apply and compare methods for the quantification of bakuchiol in cosmetic products using UV-Vis, 1H qNMR, and HPLC. The results show the possibility of using the 1H NMR method in the routine quality control of cosmetics with bakuchiol because of its comparable results with HPLC analysis and significantly shorter analysis time....
Compound Glycyrrhizin tablets (CGTs) are a combination of glycyrrhizin, glycine and methionine. Glycine and methionine have relatively high polarity and lack chromophore; therefore, it is difficult to simultaneously determine the various components using traditional reversed-phase chromatography and ultraviolet detectors. In addition, it is even more challenging to obtain a comprehensive and systematic impurity profiling for the CGTs. In this study, an ion-pair high-performance liquid chromatography (HPLC)–charged aerosol detection (CAD) method was established to determine the content of glycyrrhizin, glycine and methionine. The impurities of CGTs were also identified using mass spectrometry. By optimizing the content of trifluoroacetic acid (TFA) in the mobile phase and optimizing the CAD parameter settings, the developed method was verified in accordance with the guidelines outlined in ICH Q2 (R2). The results indicated that the method demonstrated high accuracy and sensitivity. Glycine, methionine and glycyrrhizin all showed a good linear relationship within the labeled range of 50–200%, and the average recoveries of the three components were 97.62–100.6%. The impurity detection was quantified via the principal component control method. The limit of detection (LOD) method showed an equivalent to 0.05% of the glycyrrhizin in CGTs, approximately 12.5 ng. The ion-pair HPLC–CAD method developed in this study simultaneously determined the content of the main component and the impurities of CGTs, without necessitating derivatization. This has provided a research basis for further improving the quality standards of CGTs....
The recent detection of N-nitroso-atenolol, a mutagenic and potentially carcinogenic impurity in atenolol-based pharmaceuticals, has raised serious safety concerns and emphasized the need for stringent analytical control. This study developed and validated a highly sensitive LC-MS/MS method for quantifying N-nitroso-atenolol in both active pharmaceutical ingredients (APIs) and finished products. Quantification was carried out using multiple reaction monitoring (MRM) under positive-mode electrospray ionization (ESI). Separation was performed on a C18 reversed-phase column with a gradient of water and methanol containing 0.1% formic acid. The method was validated to meet a specification limit of 15 ng/mg, with a linear range of 0.5–80 ng/mL, effectively covering 10–400% of the regulatory threshold. The method exhibited an excellent performance in terms of specificity, accuracy, precision, linearity, and robustness. It achieved a limit of detection (LOD) of 0.2 ng/mL (0.30 ng/mg) and a limit of quantification (LOQ) of 0.5 ng/mL (0.75 ng/mg), alongside a comprehensive uncertainty analysis with an expanded uncertainty of ±3.86 mg/kg. Application to commercial atenolol products confirmed the reliability and practical utility of the method. This validated approach offers a critical tool for pharmaceutical manufacturers and regulatory agencies to monitor and control N-nitroso-atenolol, ensuring compliance and enhancing patient safety....
Nimesulide is a popular non-steroidal anti-inflammatory drug (NSAID) and a cyclooxygenase-2 inhibitor available in more than 50 countries worldwide. A rapid and simple method for nimesulide determination is presented. Experimental parameters based on a previously published work were revised and adopted into a method with significantly better performance: pH was shifted from 8.10 to 9.25, borate background electrolyte concentration from 10 to 60 mM—resulting in a run time less than 4 min, and number of theoretical plates greater than 100,000. The method was validated and applied for the determination of nimesulide in three formulations with the active substance of nimesulide: tablets, gel, and powder (in sachets for oral suspension). Also, the tablets were tested for uniformity of content of single-dose preparations according to Ph. Eur....
The unregulated consumption of corticosteroids causes significant adverse effects on human health. Therefore, it is important to develop methodologies that allow their analysis in pharmaceutical matrices with competitive analysis times and costs. The determination of corticosteroids by micellar electrokinetic chromatography (MEKC) using a background electrolyte (BGE) composed of phosphate buffer and a micellar pseudostationary phase constituted by a mixture of surfactants is proposed as an alternative quantification technique. The variables involved in the BGE: phosphate concentration, surfactant (sodium dodecyl sulfate (SDS) or sodium lauryl ether sulfate (SLES)), sodium taurocholate (STC) and the pH value were optimized using a Taguchi L9 (34) experimental design. Employing the optimal BGE, the separation of the three corticosteroids is possible in a linear range of 1.05–10.0 mg L−1, with limits of detection (LOD) of 0.28–0.35 mg L−1. The relative standard deviation (RSD) values obtained for the repeatability (n = 3) and intermediate precision (n = 9) were less than 5.0%. Pharmaceutical formulations (ointments, injectable solution and ophthalmic solution) were analyzed using the proposed methodology (MEKC) and the official methodology (high-performance liquid chromatography, HPLC), and no significant differences were found between the corticosteroid contents obtained from both methods....
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