International Topical Meeting on Nuclear Research Applications and Utilization of Accelerators

4-8 May 2009, Vienna

AP/AM-08

On the Direct Characterization and Quantification of Active Ingredients in Commercial Solid Drugs using PIXE, PIGE and TOF–SIMS Techniques

B. Nsouli1, K. Zahraman1, M. Roumié 1, F. Yazbi2, and J.P. Thomas3

1IBA laboratory, Lebanese Atomic Energy Commission (CNRS), Beirut, Lebanon
2Faculty of Pharmacy, Department of Pharmaceutical Analytical Chemistry, Beirut Arab University, Beirut- Lebanon
3Institut de Physique Nucléaire de Lyon, Université Claude Bernard Lyon, Villeurbanne, France

Corresponding Author: bnsouli@cnrs.edu.lb

The quantification of the active ingredient (AI) in drugs is a crucial and important step in the
drug quality control process. This is usually performed by using wet chemical techniques like
LC–MS, UV spectrophotometry and other appropriate organic analytical methods. In the case of an active ingredient contains specific heteroatoms (F, S, Cl, . . .), elemental IBA like PIXE and PIGE techniques, using small tandem accelerator of 1 — 2 MV, can be explored for molecular quantification. IBA techniques permit the analysis of the sample under solid form, without any laborious sample preparations. This is an advantage when the number of sample is relatively large.

In this work, we demonstrate the ability of the Thick Target PIXE and PIGE technique for rapid and accurate quantification of low concentration of different fluorinated, sulfured and chlorinated active ingredients in several commercial anti-hyperlipidemic and anti-inflammatory commercial drugs.

In this work we will demonstrate the ability of PIXE and PIGE techniques for rapid and accurate quantification of Celecoxib and Atorvastatin active ingredients contained in several solid commercial drugs. The experimental aspects related to the quantification validity are presented and discussed.

In addition, the Time of Flight Secondary Ion Emission using multicharged Ar ions with ~10 MeV energy, delivered by a 4 MV Vander Graaf single stage accelerator, was used for structural andchemical analysis for some cases of binary commercial drugs containing two different active ingredients. The aspect of sample preparation and the role of excipient will be highlighted and discussed.