Current Pharmaceutical Analysis - Volume 20, Issue 6, 2024

The objective of the research was the development and validation of a simple, sensitive, accurate, robust, and precise UV-spectroscopic method for the quantitative determination of chlorogenic acid loaded in solid-lipid nanoparticles as per the guidelines of the International Conference on Harmonization.

The solid-lipid nanoparticles of chlorogenic acid were prepared using the hot melt emulsification method and the high-speed homogenizer method. Glyceryl monostearate was used as a solid lipid, and Tween 80 was used as a surfactant for the preparation of chlorogenic acid-loaded solid lipid nanoparticles. The method was validated in terms of linearity, accuracy, precision, robustness, ruggedness, limit of detection, and limit of quantification.

The chlorogenic acid exhibited absorption maxima at the wavelength of 330 nm. The regression equation from the calibration curve was y=0.006x + 0.0193 with a correlation coefficient of 0.9989. The percentage recovery was found to be 99.92, 99.80, and 99.86, respectively (within the acceptable limit of 98-102%), which validated the accuracy of the method. Furthermore, the method exhibited precision, robustness, and ruggedness, as illustrated by a relative standard deviation (RSD) of less than 2%. The limit of detection and limit of quantification were found to be 6.97 and 21.13 μg/ml, respectively.

It was concluded that the proposed spectrophotometer analytical method for the determination of Chlorogenic acid was found reliable, accurate, consistent, precise, accurate, and robust. Therefore, the proposed analytical technique could be an integral part of further evaluation and characterization of Chlorogenic acid-solid lipid nanoparticles.

In the current study, a simple and cost-effective stability-indicating RP-HPLC method was developed and validated to estimate the mesalamine from both bulk and pharmaceutical dosage forms.

An isocratic HPLC method using a reverse phase HiQSilC18 column (250 x 4.6 mm, 5µm) and a mobile phase methanol: ammonium acetate buffer (90:10 v/v) were employed as the mobile phase with a flow rate of 1 mL/min at 25°C. Detection was carried out at 305 nm, and the injection volume was 20μl. The developed method was validated as per ICH Q2 guidelines. Mesalamine has been subjected to various stress testing conditions, such as hydrolysis of acid and base, thermal degradation, oxidation, and photolysis. Also, methods have been validated with regard to linearity, accuracy, precision, and robustness.

The RT of mesalamine was determined to be 3.550 min ± 0.024 minutes, providing a reliable marker for its identification. The method was found to be linear between 5-30 μg/mL concentration with (R²) of 0.994. This demonstrated the method's ability to measure varying concentrations of mesalamine accurately. Additionally, the percentage recovery of mesalamine was approximately 100%, confirming the accuracy of the developed method. The parameters for system suitability have also been found to be within acceptable limits. Force degradation studies reinforced the method's selectivity and sensitivity in detecting mesalamine under various degradation scenarios. Notably, mesalamine significantly degraded in an acidic environment.

In conclusion, our proposed RP-HPLC method provides a sensitive, accurate, and precise means of analyzing mesalamine in both bulk and pharmaceutical dosage forms.

Carbamide peroxide (CP) is a hydrogen peroxide derivative bonded with urea. It is a solid substitute for liquid hydrogen peroxide in the chemical, cosmetics, and pharmaceutical industries, mainly as a disinfectant and bleaching application. However, it has an unstable nature, and there are scant studies on CP thermal analysis.

This study focuses on CP thermal analysis and degradation behavior.

CP was characterized by differential scanning calorimetry, thermogravimetric analysis, Fourier-transformed infrared, diffraction by X-ray, as well as, thermal and photodegradation was determined by ultraviolet spectrophotometer.

CP was characterized with a sharp endothermic event (88.50°C; ΔH= -643.20 J.g^-1), and a thermal decomposition behavior in a four-steps process. The pattern diffraction presented sharp peaks at 2θ: 15.2, 25.1 and 26.°C The Arrhenius plot obtained by isothermal thermogravimetric analysis showed a linear relation with temperature in two steps. The first step the activation energy values was Ea = 45.73 J.mol^-1.K^-1. The thermal degradation recovery was 3.29% after 5 days, and 11.31% against 97.4% under the dark control to photostability.

The study contributed to characterizing the CP and the results suggest that degradation depends on the surface transition state and the ternary formed system (CP-urea-water) and that the temperature influenced this system. The data were obtained through quick and easy techniques, which use wispy raw material and presented a significant result that can be used by the entire industry in the development of new formulations.