Validation of an analytical method by HPLC for the quantification of yangambin from the Ocotea duckei species / Validación de un método analítico por HPLC para la cuantificación de yangambin de la especie Ocotea duckei

Ocotea duckei , known as Louro - de - cheiro, belongs to the Lauraceae family and presents lignoid yangambine (YAN) as the main plant marker. This work aimed to develop and validate an analytical method by high performance liquid chromatography for the quantification of YAN. The sample used was the crude eth anolic extract (CEE) obtained from aerial parts. In the developed method, a C18 column was used. The mobile phase was composed of acetonitrile and water (45:55), whereas the method parameters included mobile phase flow rate at 0.8 mL/min, oven temperature at 40°C, and monitoring at 205 nm. In the validation, the parameters of selectivity, linearity, precision, accuracy, robustness, limits of detection and quantification were evaluated. As a result, the developed method is in accordance with the guidelines f or validation of analytical methods and presented satisfactory chromatographic parameters for YAN determination. Thus, the present analytical methodology can be applied in the quality control of O. duckei raw materials.

Ocotea duckei , conocida como Louro - de - cheiro, pertenece a la familia Lauraceae y presenta la yangambina lignoide (YAN) como principal marcador vegetal. Este trabajo tuvo como objetivo desarrollar y val idar un método analítico por cromatografía líquida de alta resolución para la cuantificación de YAN. La muestra utilizada fue el extracto etanólico crudo (EEC) obtenido de partes aéreas. En el método desarrollado se utilizó una columna C18. La fase móvil c onsistió en acetonitrilo y agua (45:55), mientras los parámetros del método incluyeron el caudal de la fase móvil a 0,8 m L /min, la temperatura del horno a 40°C y la monitorización a 205 nm. En la validación se evaluaron los parámetros de selectividad, line alidad, precisión, exactitud, robustez, límites de detección y cuantificación. Como resultado, el método desarrollado está de acuerdo con las pautas para la validación de métodos analíticos y presentó parámetros cromatográficos satisfactorios para la deter minación de YAN. Por lo tanto, la presente metodología analítica se puede aplicar en el control de calidad de las materias primas de O. duckei.

A Metformin-Ferulic Acid Salt with Improved Biopharmaceutical Parameters.

Though ferulic acid presents great hypoglycemic potential, it possesses limited aqueous solubility, and low oral bioavailability. When associated with metformin, the first-choice drug in Type 2 diabetes treatment, FA demonstrates synergistic hypoglycemic effects, however, it also causes certain undesirable dose-related effects. This study aimed to develop a new ferulic acid - metformin multicomponent system, and incorporate it into a solid dosage form with improved biopharmaceutical parameters. A novel metformin: ferulate (1:1) salt (MFS) was produced, which was properly characterized using differing analytical techniques, including single crystal analysis. Also during the course of the study, a new polymorph of the metformin free base was observed. The MFS was obtained using solvent evaporation methods, which achieved high yields in reproducible process, as well as a 740-fold increase in ferulic acid aqueous solubility. The MFS tablets developed met quality control requirements for this dosage form, as well as revealing excellent performance in vitro dissolution tests, presenting dissolution efficiency values of 95.4 ± 0.5%. Additionally, physicochemical instability was not observed in a study at 40 °C for 3 months for both MFS powder and its tablet form. The MFS product developed is a promising candidate for further Type 2 diabetes clinical study.

A high-performance liquid chromatography method for simultaneous quantification of metformin and ferulic acid in solid dosage forms.

Metformin is one of the most commonly used drugs in the world for the treatment of type 2 diabetes, while ferulic acid is a molecule that stands out for its antioxidant potential. Recent studies demonstrate hypoglycemic synergy between these molecules. The objective of this study is to develop and validate an analytical methodology by high-performance liquid chromatography for the simultaneous quantification of these drugs in pharmaceutical formulations. The method used an octadecylsilane column and a mobile phase composed of 6 mM sodium lauryl sulfate in 15 mM phosphate buffer:ACN (65:35). Ferulic acid and metformin were monitored at 232 nm, with a mobile phase flow rate of 1 ml/min and oven temperature at 40°C. The method was linear in the range of 5-25 µg/ml for both molecules. In the presence of degradation products, satisfactory selectivity was achieved. Accuracy values were close to 100% and standard deviations in precision were less than 2%. In the robustness evaluation, the proposed variations did not interfere with the quantification. Therefore, it is concluded that the present method can be safely applied to the quality control of ferulic acid and metformin raw materials, as well as when they are combined in pharmaceutical formulations.

A New Ferulic Acid-Nicotinamide Cocrystal With Improved Solubility and Dissolution Performance.

Among the various strategies for increasing aqueous solubility of pharmaceutical substances, cocrystals have been emerging as a promising alternative. The ferulic acid (FEA) is a molecule with limited aqueous solubility, but with an interesting pharmacological activity, highlighting its antitumor potential. This study presents the characterization and physicochemical properties of a new cocrystal based on FEA and nicotinamide (NIC). The FEA-NIC cocrystal was obtained by solvent evaporation technique and physicochemically characterized by differential scanning calorimetry, powder X-ray diffraction, Fourier transform infrared spectroscopy, solid-state nuclear magnetic resonance and scanning electron microscopy. The content determination and dissolution profile in different media were analyzed by high-performance liquid chromatography. The results obtained with the characterization techniques indicated the obtainment of an anhydrous cocrystal of FEA and NIC at a 1:1 molar ratio. The method was reproducible and obtained a high yield, of approximately 99%. In addition, a 70% increase in the FEA solubility in the cocrystal and a better dissolution performance than the physical mixture in pH 6.8 were achieved.