title: Determination of elemental impurities in pharmaceutical products and related matrices by ICP-based methods: a review.
abstract: Interest in the determination of elemental impurities in pharmaceuticals has increased in recent years because of changes in regulatory requirements and the need for changing or updating the current limit tests recommended in pharmacopeias. Inductively coupled plasma (ICP) optical emission spectrometry and ICP mass spectrometry are suitable alternatives to perform multielemental analysis for this purpose. The main advantages and limitations of these techniques are described, covering the applications reported in the literature in the last 10 years mainly for active pharmaceutical ingredients, raw materials, and pharmaceutical dosage forms. Strategies used for sample preparation, including dissolution in aqueous or organic solvents, extraction, wet digestion and combustion methods are described, as well as direct solid analysis and ICP-based systems applied for speciation analysis. Interferences observed during the analysis of pharmaceutical products using ICP-based methods are discussed. Methods currently recommended by pharmacopeias for elemental impurities are also covered, showing that the use of ICP-based methods could be considered as a trend in the determination of these impurities in pharmaceuticals. However, the development of a general method that is accurate for all elemental impurities and the establishment of an official method are still challenges. In this regard, the main drawbacks and suitable alternatives are discussed.
authors.affiliation: Departamento de Tecnologia e Ciência dos Alimentos, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil.
authors.forename: Juliano S
authors.initials: JS
authors.lastname: Barin
authors.affiliation: Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil.
authors.forename: Paola A
authors.initials: PA
authors.lastname: Mello
authors.affiliation: Centro de Ciências Químicas, Farmacêuticas e de Alimentos, Universidade Federal de Pelotas, Pelotas, RS, 96160-000, Brazil.
authors.forename: Marcia F
authors.initials: MF
authors.lastname: Mesko
authors.affiliation: Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil.
authors.forename: Fabio A
authors.initials: FA
authors.lastname: Duarte
authors.affiliation: Departamento de Química, Universidade Federal de Santa Maria, Santa Maria, RS, 97105-900, Brazil. ericommf@gmail.com.
authors.forename: Erico M M
authors.initials: EM
authors.lastname: Flores
mesh_terms: D013058:Mass Spectrometry / Q000379:methods*; D004364:Pharmaceutical Preparations / Q000737:chemistry*
chemical_list: D004364:Pharmaceutical Preparations
keywords: Atomic spectrometry; Determination of elemental impurities; Heavy metals; Pharmaceutical analysis; Pharmacopoeia; Sample preparation