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Semiquantitative X-ray Powder Diffraction Analysis in Counterfeit Medicines Investigation—The Viagra Example

Authors :
Armand Budzianowski
Karolina Pioruńska-Sędłak
Magdalena Popławska
Jan K. Maurin
Agata Błażewicz
Source :
Crystals, Vol 13, Iss 10, p 1485 (2023)
Publication Year :
2023
Publisher :
MDPI AG, 2023.

Abstract

Have you ever looked at a powder diffractogram during a routine qualitative test and wondered how much of a particular powder compound is in the powder material? Several methods can work this out, but none of them could be used in our case because something was missing from each in performing a rapid quantity test for an active ingredient in a tablet. A semiquantitative method of an X-ray powder diffraction analysis of products containing sildenafil citrate is proposed. This method utilizes calibration curves for the most common compositions encountered in falsified and not-registered Viagra analogues. Sildenafil doses are established for singularly prepared powder probes of a medicinal product, and two runs of data collection are used: the first, the fast one, for the qualitative analysis of the product, and the second for selected 2θ regions for the API and identified excipients. An example of a product composed mainly of sildenafil citrate, gypsum and microcrystalline cellulose is discussed in detail. The data obtained from X-ray experiments were compared with the results obtained from validated liquid chromatography coupled to a diode array detector and mass spectrometry methods.

Details

Language :
English
ISSN :
20734352
Volume :
13
Issue :
10
Database :
Directory of Open Access Journals
Journal :
Crystals
Publication Type :
Academic Journal
Accession number :
edsdoj.0766668eb37c4b9caf3891a06a7b23fc
Document Type :
article
Full Text :
https://doi.org/10.3390/cryst13101485