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J Sep Sci ; 37(13): 1648-55, 2014 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-24723310

RESUMO

A poly(butyl methacrylate-co-ethylene dimethacrylate) monolithic column was fabricated and used as a novel sorbent for online solid-phase extraction coupled to liquid chromatography with tandem mass spectrometry for the simultaneous determination of Sudan I-IV in chili pepper powder. The prepared columns were characterized by scanning electron microscopy, nitrogen adsorption-desorption, and pressure drop measurements. Online solid-phase extraction was performed on the synthesized monolithic column using 10 mM ammonium acetate solution as the loading solution with the aid of an online cleanup chromatography system. The desorption of Sudan I-IV was achieved with acetonitrile as the eluting solution at the flow rate of 0.5 mL/min. The extracted analytes were subsequently eluted into a C18 analytical column for chromatographic separation using a mixture of 10% acetonitrile/90% formic acid (0.5%) solution as the mobile phase. Under the optimized conditions, the developed method had linear range of 1.0-50 µg/kg, a detection limit of 0.3 µg/kg, and a quantification limit of 1.0 µg/kg for each analyte. The intraday and interday recoveries of Sudan I-IV in chili pepper powder samples ranged from 94.8 to 100.9% and 94.9 to 99.4%, respectively. The intraday and interday precision were between 3.37-7.01% and 5.01-7.68%, respectively.


Assuntos
Capsicum/química , Cromatografia Líquida de Alta Pressão/métodos , Corantes/análise , Corantes/isolamento & purificação , Contaminação de Alimentos/análise , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Automação , Compostos Azo/análise , Compostos Azo/isolamento & purificação , Limite de Detecção , Metacrilatos/química , Naftóis/análise , Naftóis/isolamento & purificação , Extração em Fase Sólida/instrumentação
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