Abstract
In this study, two methods based on the use of diluted acids were developed: microwave-assisted wet digestion (MAWD) and microwave-assisted ultraviolet digestion (MAWD-UV). These methods are evaluated for the digestion of oral pharmaceutical drugs and further determination of elemental impurities from classes 1 (As, Cd, Hg and Pb) and 2A (Co, Ni and V) by inductively coupled plasma optical emission spectrometry (ICP-OES). Commercial drugs for the treatment of type 2 diabetes are used. No prior comminution is performed. For MAWD, the optimized conditions were 2 mol L−1 or 3 mol L−1 HNO3, 1 mL of 50% H2O2 and a 45 min or 55 min irradiation program. For MAWD-UV, the condition using 1 mol L−1 HNO3, 1.6 mL of 50% H2O2 and a 55 min irradiation program enabled the digestion of all samples. In this way, efficient methods are proposed for the digestion of commercial pharmaceutical tablets for further determination of class 1 and 2A elemental impurities (ICH Q3D guidelines).
Highlights
In recent years, an increasing interest in the determination of elemental impurities in pharmaceutical products has been observed in the literature, pushed by stricter limits introduced by several documents, such as the ICH Q3D guidelines [1] and United StatesPharmacopeia (USP) chapters 232 and 233, implemented in 2018 [2,3]
The aim of this study is to develop sample preparation methods for oral drugs used in the treatment of type 2 diabetes and the further determination of class 1 and 2A elemental impurities
With the proposed microwaveassisted wet digestion (MAWD) and MAWD-UV methods, it was possible to efficiently digest oral pharmaceutical drugs used in the treatment of type 2 diabetes for the further determination of class 1 and 2A elemental impurities by inductively coupled plasma optical emission spectrometry (ICP-OES)
Summary
Pharmacopeia (USP) chapters 232 and 233, implemented in 2018 [2,3]. These impurities have been separated in three classes (1, 2A and 2B, and 3) by ICH Q3D guidelines, according to their toxicity and probability of occurrence in the pharmaceutical product [1]. Elements Ba, Cr, Cu, Li, Mo, Sb and Sn form class 3, presenting low oral toxicity, but should be monitored in parenteral and inhalational routes of administration [1]. Classes 1 and 2A should be monitored through all routes of exposure, being the most critical for the oral route. Aside from the toxicological aspect, the control of elemental impurities is useful for the identification of possible faults in the production process and storage of pharmaceutical products [5]
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