A fast method based on programmed temperature vaporization-mass spectrometry for the quantification of...

A rapid method has been developed for the determination of 17α-ethinylestradiol and drospirenone in contraceptive formulations. The method is based on the direct coupling of a programmed temperature vaporizer inlet to a quadrupole mass spectrometer via a deactivated fused silica tube (10 m × 0.18 mm) that is maintained at 275 °C throughout the entire analysis. The inlet is equipped with a baffled glass liner coated with Siltek™ and the injection is performed in split mode (ratio 1 : 10). The data acquisition time was only 1.0 min per sample, allowing for the high-throughput quantification of active principles in contraceptive pills in minimal time. The goal is to apply this strategy as a screening tool in quality control processes, limiting the use of the more costly and time-consuming chromatographic methods to those pills showing anomalous results, thus optimizing laboratory resources. Sample treatment involved a fast ultrasound-assisted solid-liquid extraction, and both sample preparation and instrumental conditions were optimized. The determination of the active principles was performed using the standard addition method. Accuracy, expressed as recovery percentage relative to the mass of active principle declared by the manufacturer, varied between 80% and 120%. Intra- and inter-day precision were adequate, with values of relative standard deviation (% RSD) equal to or less than 9% and 11%, respectively. Furthermore, the sustainability profile of the proposed rapid method was evaluated using the HEXAGON algorithm, which demonstrated that the PTV-MS method contributes to sustainable development by benefiting both the environment and society.