Abstract
Avanafil (AVA), one of the most effective drugs prescribed for erectile dysfunction, is a pyrimidine-derivative PDE5 inhibitor. In the current work, new LC methods were developed and validated for quantitative determination of avanafil and qualitative determination of its degradation products. The quantitative determination of avanafil was carried out using liquid chromatography with photodiode array detection (LC-DAD) and liquid chromatography-tandem mass spectrometry LC-MS/MS methods, and fully validated according to the ICH Q2 (R1) guideline, while qualitative determination was performed using a liquid chromatography mass spectrometry-ion trap-time of flight (LCMS-IT-TOF) instrument. The separation of avanafil and its degradation products was carried out using the same reversed-phase chromatographic conditions, in which a second-generation C18-bonded monolithic silica column (Chromolith® High Resolution RP-18e, 100 × 4.6 mm, Merck KGaA) was used as stationary phase. Briefly, the methods enable quantitation of avanafil with high accuracy (recovery > 95%) and precision (RSD% < 2.0), within the ranges of 0.5–20 μg/mL for LC-DAD and 150–6000 ng/mL for LC-MS/MS. In the forced degradation studies, over and above currently existing data, a new oxidation-based degradation product, whose predicted m/z is 367.1168, was identified and its structure was confirmed by high-resolution mass spectrometric analysis. As the main advantage, either an LC-DAD or LC-MS/MS instrument can be chosen for interference-free quantitation of AVA, according to the facilities in quality-control laboratories.
Highlights
Erectile dysfunction (ED), one of the common sexual disturbances in the adult male, is described as a permanent or repetitive inability to attain and/or maintain penile erection for satisfactory sexual performance [1]
In accordance with the deficiencies in methods were of sophisticated analytical instrumentation and equipment to match and fulfillversatile, the the literature, the use presented study was realized with a main purpose to develop robust, recent requirements of the pharmaceutical industry standards: the use of monolithic silica columns selective, sensitive and validated LC methods, whose analysis time, cost and efficiency are optimized for higher efficiency and lower analysis costs, optional utilization of either liquid chromatography with photodiode array detection (LC-DAD) or LC–MS/MS
In this paper; quantitative analysis of AVA in pharmaceutical preparations, qualitative analysis of AVA and its degradation products, and identification of a novel degradation product were successfully performed by using the same analytical conditions on LC-DAD, LC-MS/MS and LCMS-IT-TOF
Summary
Erectile dysfunction (ED), one of the common sexual disturbances in the adult male, is described as a permanent or repetitive inability to attain and/or maintain penile erection for satisfactory sexual performance [1]. In accordance with the deficiencies inusing different instrumental configurations; besides, duewith to the therobust, topic isversatile, still suitable the literature, the presented study was realized a low mainamount purposeoftowork, develop selective, sensitive validated LC whose analysis time, cost and efficiency are optimized to research for better and identification ofmethods, some analytical properties. In accordance with the deficiencies in methods were of sophisticated analytical instrumentation and equipment to match and fulfillversatile, the the literature, the use presented study was realized with a main purpose to develop robust, recent requirements of the pharmaceutical industry standards: the use of monolithic silica columns selective, sensitive and validated LC methods, whose analysis time, cost and efficiency are optimized for higher efficiency and lower analysis costs, optional utilization of either LC-DAD or LC–MS/MS for use in routine analysis of AVA in tablet formulations. The degradation products were produced in forced degradation studies, qualitatively determined and accurately identified with LCMS-IT-TOF, and a novel degradation product, which was produced in oxidizing conditions, was identified for the first time
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