Microwave-assisted sample preparation of medicines for determination of elemental impurities in compliance with United States Pharmacopeia: How simple can it be?

Microwave-assisted sample preparation of medicines for determination of elemental impurities in compliance with United States Pharmacopeia: How simple can it be?
Anal Chim Acta. 2019 Aug 13;1065:1-11
Authors: Pinheiro FC, Barros AI, Nóbrega JA
Abstract
This work proposed a procedure for microwave-assisted sample preparation of medicines using diluted nitric acid followed by determination of elemental impurities using inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS) according to the United States Pharmacopeia Chapters 232 and 233. Three solutions, i.e. inverse aqua regia, 7.0 and 2.0 mol L-1 HNO3, were evaluated for microwave-assisted digestion of nine drugs samples. The applicability of each digestion procedure was assessed by comparison of analyte concentrations determined using total (reference procedure) and partial digestions (proposed procedure) as well as by determining dissolved carbon content and evaluating matrix effects. There were none significant differences at a 95% confidence level among the concentrations determined applying reference and proposed procedures. Internal standardization (ICP OES) and aerosol dilution (ICP-MS) were applied for minimization and correction of matrix effects. Addition and recovery experiments were performed according to oral permissible daily exposures values specific for each element and each sample was spiked w...

Source: Analytica Chimica Acta - April 23, 2019 Category: Chemistry Authors: Pinheiro FC, Barros AI, Nóbrega JA Tags: Anal Chim Acta Source Type: research