Current Issue : January-March Volume : 2025 Issue Number : 1 Articles : 5 Articles
A novel high-performance liquid chromatography (HPLC) method with 4-N,Ndimethylaminobenzaldehyde as an internal standard was developed for the determination of Camphor with the main goal of facilitating the analysis of different cosmetic and pharmaceutical products that contain Camphor in analytical laboratories. The method can be applied to cosmetic and pharmaceutical samples such as gels, ointments, and creams containing Camphor. Chromatographic separation was carried out on the Symmetry® C18, 5 μm column (Waters), 250 × 4.6 equipped with guard column E, InertSustain C18, 5 μm, while using the flow of 1.4 mL/min, with a column temperature of 25 ◦C. The mobile phase consisted of 600 mL of acetonitrile, 400 mL of purified water, and 6 mL of glacial acetic acid. The method was evaluated in accordance with ICH Q2 (R2) guidelines for validation parameters: selectivity, linearity (range 0.10–3.00 mg/mL), the limit of detection (LOD = 0.028 mg/mL), the limit of quantification (LOQ = 0.085 mg/mL), accuracy (confidence intervals < 0.05%), repeatability (peak area ratio = 0.39–1.97), and intermediate precision (peak area ratio = 0.40–1.98). The method is applicable for detecting and quantifying Camphor in a variety of cosmetic and pharmaceutical products from different parts of the world, thus covering the concentrations required by different law legislations....
Objective: To evaluate and project the shelf life of GLPG4399, an early-phase clinical drug formulation by applying the Accelerated Stability Assessment Program (ASAP) approach. Methods: Forced degradation conditions were implemented to identify the stability-limiting degradation product. The drug and its degradation products were separated using a validated liquid chromatography method. Then, the selected clinical capsule formulation was placed in a glass vial and exposed to accelerated short-term conditions of combinations of high- and low-level heat and humidity in an open state for 5 weeks. The liquid chromatography results were evaluated using the ASAP, which is based on the moisture-modified Arrhenius principle. The resulting data were fitted using a suitable diffusion kinetics method. Results: The developed model was applied to predict the shelf life of the drug product when using clinically appropriate primary packaging (high-density polyethylene container). The derived stability parameters of the moisture-modified Arrhenius equation were the Arrhenius collision frequency, activation energy, and humidity sensitivity constant. The goodness of fit parameters R2 (>0.95) and goodness of prediction Q2 (>0.80) parameters for the selected model were acceptable. The results of the accelerated, short-term stability study were verified against real-time, long-term 12-month data. Conclusions: We demonstrated the application of the ASAP approach to evaluate the shelf life of a GLPG4399 solid capsule formulation. The studied ASAP approach can be extended to evaluate the stability and shelf-life estimations of other early-phase clinical formulations....
This study presents the development and validation of environmentally friendly analytical methods for quantifying Abiraterone Acetate (AA) in both its pure form and commercial pharmaceutical formulations. An optimized High-Performance Liquid Chromatography (HPLC) method was developed using an Agilent Extend C18 column (250 mm × 4.6 mm, 5 μm) at 25 ◦C. The mobile phase consisted of formic acid and ethanol in isocratic mode, with a flow rate of 1.0 mL min−1, and detection was performed at 253 nm. The spectrophotometric method involved a comprehensive evaluation of AA’s spectral properties in various solvents, with ultrapure water providing the most suitable spectra for analysis at 253 nm. Both methods were validated according to ICH guidelines, demonstrating selectivity, linearity, accuracy, precision, detection and quantification limits, and robustness, with correlation coefficients exceeding 0.999 across the 5–30 μg mL−1 concentration range. Comparative statistical analysis using Student’s t-test and Fisher’s F-test showed no significant differences between the two methods. The environmental impact of both methods was assessed using AGREE and GAPI software, confirming their sustainability. These validated methods offer reliable and eco-friendly approaches for the quantitative analysis of AA in tablet formulations, promoting safer and greener laboratory practices in pharmaceutical analysis....
The GPHF-Minilab™ is a portable toolkit for performing qualitative methods such as thin-layer chromatography (TLC) on common pharmaceuticals. It is particularly useful in resourcelimited locations where it is more challenging to monitor for substandard and falsified (SF) medicines. However, the GPHF-Minilab™ TLC methods are only semi-quantitative at best and thus have issues monitoring product quality effectively. We have improved on the GPHF-Minilab™ TLC method for metronidazole, a common antibiotic, by making it fully quantitative. Sample solutions were spotted on TLC plates alongside three metronidazole standards at different concentrations. After development, plates were imaged in a lightbox with two different smartphone cameras. Images were processed through the open-source program ImageJ and resulting pixel data from the standard spots were used to create a calibration curve, enabling quantitation of the sample. The USP Metronidazole Tablet high-performance liquid chromatography (HPLC) assay was used as the reference method. We validated this TLC method using 250 and 500 mg metronidazole tablets from different manufacturers and assessed linearity, range, accuracy, precision, intermediate precision, specificity, and robustness. These improvements should enhance the GPHF-Minilab™ TLC methods for metronidazole product screening. Additionally, the procedure is extensible to other analytes, although further validation would be required for each Minilab method....
A sequential injection analysis method for the determination of glutathione (GSH) in pharmaceuticals has been developed. It is based on the reduction of the Cu(II)-neocuproine complex by GSH and the formation of an orange-yellow colored Cu(I)-neocuproine complex with maximum absorbance at 458 nm. Under optimal conditions the method is characterized by a linear calibration range of 6.0 × 10−7–8.0 × 10−5 mol L−1 (Amax = 3270 CGSH − 0.0010; R2 = 0.9983), limit of detection of 2.0 × 10−7 mol L−1, limit of quantification of 6.7 × 10−7 mol L−1, repeatability (expressed as relative standard deviation) of 3.8%, and sampling rate of 60 h−1. The newly developed method has been successfully applied to the determination of GSH in pharmaceutical samples with no statistically significant difference between the results obtained and those produced by the standard Pharmacopoeia method....
Loading....