The simplicity, sensitivity and expeditiousness of ion mobility spectrometry (IMS) make it especially useful for the determination of active principal ingredients (APIs) present at low concentrations in pharmaceuticals. However, the poor resolution of this technique precludes the identification and/or determination of substances with similar molecular weights, which exhibit also similar drift times and give overlapped peaks as a result. Oral contraceptives are pharmaceutical formulations containing two APIs of similar molecular weights at very low concentrations which therefore give strongly overlapped peaks hindering their determination by IMS. In this work, we assessed the potential of IMS for detecting and quantifying the contraceptives ethinylestradiol (ETE) and desogestrel (DES) in commercial tablets. To this end, we used various chemometric techniques including a second-derivative (TN2D) algorithm and the more powerful choice Multivariate Curve Resolution (MCR) to improve the resolution of IMS and enable the determination of both APIs. Quantitation was based on PLS1 models for each API. The models constructed involve a single PLS factor with a Y-explained variance above 98.4%, obtaining a RMSEP of 0.34 and 0.63 for ETE and DES, respectively. The ensuing method, which was validated for use in routine analyses, is quite expeditious (analyses take less than 1. min) and uses very small amounts of sample (a few microliters). Based on the results, IMS has a great potential for the qualitative and quantitative determination of APIs in low doses. © 2012 Elsevier B.V.
|Journal||Analytica Chimica Acta|
|Publication status||Published - 13 May 2012|
- Ion mobility spectrometry
- Multivariate calibration