Foram avaliados dois métodos diferentes de preparo de amostras de carnes baseados na solubilização em meios alcalino ou ácido. O objetivo deste estudo foi determinar os teores de Na e K após solubilização com hidróxido de tetrametilamônio (TMAH) à temperatura ambiente, e com ácido fórmico e aquecimento em bloco de digestão a 50 ºC por cerca de 2 h. A solubilização alcalina se apresentou como uma metodologia simples e robusta e a melhor alternativa frente aos procedimentos de mineralização convencional, permitindo a solubilização completa das amostras usando pequenas quantidades de TMAH. O método foi validado empregando-se materiais de referência certificada assim como pela comparação com método de digestão convencional com ácido nítrico. Os limites de detecção obtidos foram de 0,8 e 2,0 mg g -1 para Na e K, respectivamente, e se mostraram adequados para o objetivo das análises.Two different sample preparation methods were evaluated for meat samples employing the solubilization in alkaline or acidic media. The aim of this study was to determine Na and K levels after sample solubilization with tetramethylammonium hydroxide (TMAH) at room temperature, and with formic acid and heating in a digester block at 50 ºC for ca. 2 h. The alkaline solubilization showed to be a simple and robust method and the better alternative in relation to the mineralization conventional procedures, allowing the complete solubilization of the samples even when small quantities of TMAH were used. The method was validated by using certified reference material as well as by comparing with samples digested with nitric acid. The limits of detection obtained were 0.8 and 2.0 μg g -1 for Na and K, respectively, and showed to be adequate for the analysis purposes.
Inorganic elements present in pharmaceutical products were determined by inductively coupled plasma-mass spectrometer (ICP-MS), employing microwave acid digestion as a sample preparation method. , were determined in acyclovir ointment and its constituents. Elemental impurities in the pharmaceutical samples were determined using an inductively coupled plasma-universal cell technology-mass spectrometer (ICP-UCT-MS) operated in kinetic energy discrimination (KED) and standard mode. The accuracy of the method was assessed by means of addition and recovery experiments. Except for Cr, spiked recoveries of the elements added to the samples before microwave acid digestion (MW-AD) step were between 95.1 and 126%, and after MW-AD step ranged from 85.6 to 132%. Limits of detection (LOD) obtained by proposed method is in agreement to those required by the U.S. Pharmacopeia Convention (USP), showing that the ICP-MS technique is well suited for quantification of these elements. The LOD's (ng L -
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