Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System
| Autor: | Rüstem Keçili, Hassan Y. Aboul-Enein, Göksel Arli, Murat Soyseven |
|---|---|
| Rok vydání: | 2020 |
| Předmět: |
Calibration curve
Pyridines Sensitive analysis 030226 pharmacology & pharmacy 01 natural sciences Analytical Chemistry 03 medical and health sciences chemistry.chemical_compound 0302 clinical medicine Impurity Limit of Detection Chromatography High Pressure Liquid Detection limit Active ingredient Chromatography 2-Chloropyridine Column temperature Chemistry 010401 analytical chemistry Reproducibility of Results General Medicine 0104 chemical sciences Volumetric flow rate Linear Models Drug Contamination Mutagens |
| Zdroj: | Journal of chromatographic science. 59(3) |
| ISSN: | 1945-239X |
| Popis: | A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX. |
| Databáze: | OpenAIRE |
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