Rapid determination of ampyra in urine samples using dispersive liquid-liquid microextraction coupled with ion mobility spectrometry

J Pharm Biomed Anal. 2023 Feb 5:224:115185. doi: 10.1016/j.jpba.2022.115185. Epub 2022 Dec 1.

Abstract

Ampyra (AMP, 4-Aminopyridine) is a potassium channel blocker that attracts growing research interest due to its adverse effects at high doses. The fast analysis of AMP is challenging because it typically requires complex analytical techniques. In this research, we developed and validated a novel method to assess the fast and quantitative analysis of AMP from real samples. This method combines the strength of ion mobility spectrometry (IMS) for rapid detection and the dispersive liquid-liquid microextraction as a fast and effective preconcentration method for the preconcentration/extraction of AMP. In this method, Ag nanoparticles were used as modifier agents. Moreover, the proposed mechanism for interaction of AMP with AgNPs was investigated based on the quantum theory of atoms in molecules (QTAIM) analysis. Also, the sensitivity of the proposed method was improved through the application of a delay on the carrier gas flow after sample injection. Under the optimum conditions, the developed method detected AMP in the linear range of 0.4-16 μmol L-1 with a detection limit of 0.12 µmol L-1. Finally, the developed method was successfully employed to quantify AMP in urine samples. Method validation was performed by comparing our results with those obtained by HPLC-UV/Vis, confirming the applicability of the proposed method for the AMP analysis in real samples. The proposed method will open up a new door toward developing simple, fast, and effective analytical methods.

Keywords: Ag nanoparticles; Ampyra; Dispersive liquid-liquid microextraction; Ion mobility spectrometry; Real sample.

MeSH terms

  • 4-Aminopyridine
  • Ion Mobility Spectrometry
  • Limit of Detection
  • Liquid Phase Microextraction* / methods
  • Metal Nanoparticles*
  • Silver
  • Solvents / chemistry

Substances

  • Solvents
  • Silver
  • 4-Aminopyridine