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1.
Artigo em Inglês | MEDLINE | ID: mdl-30211663

RESUMO

A general solid-phase extraction (SPE) method using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the determination of moroxydine residues in pig and chicken samples has been developed. After extraction and purification of real samples, moroxydine residues were detected using a hydrophobic interaction liquid chromatography column with an optimised mobile phase composition. The extraction reagents, the kind of SPE columns and the type of eluents were optimised to achieve the maximum extraction efficiency. The matrix effects from the animal tissue influenced the quality of the quantitative data obtained. Under the optimised conditions, the moroxydine residues in pig and chicken samples spiked at three levels (1.0 µg/kg, 5.0 µg/kg and 10.0 µg/kg) were determined with good recoveries (61.5%-105.4%) and adequate relative standard deviations (3.2%-13.0%). In pig and chicken samples, the limit of detection (LOD) was 0.3 µg/kg, and the limit of quantification (LOQ) was 1.0 µg/kg. A sufficiently linear relationship in the range of 1.0 µg/kg-20.0 µg/kg was achieved with a good correlation coefficient (R2 ≥ 0.99).


Assuntos
Antivirais/análise , Resíduos de Drogas/análise , Análise de Alimentos , Morfolinas/análise , Animais , Biguanidas , Galinhas , Cromatografia Líquida de Alta Pressão , Extração em Fase Sólida , Suínos , Espectrometria de Massas em Tandem
2.
Artigo em Inglês | MEDLINE | ID: mdl-23469982

RESUMO

Cyromazine and dicyclanil are both used as insect growth regulators. This paper describes an easy and innovative simultaneous extraction method for residues of cyromazine and dicyclanil in food of animal origin, and a confirmation procedure using UHPLC-MS/MS. The sample was extracted, deproteinised by 1% trichloracetic acid in water-acetonitrile, followed by selective defatting using hexane based on the degree of matrix complexity; cleaned-up on an mixed-mode cation exchange (MCX) cartridge; and quantified by using matrix-matched calibration. The mean recoveries were all between 62.0% and 99.2%, and the RSDs were all below 9.94%. The present method was rapid, sensitive and reliable, which was applied to the quantitative analysis of these residues in animal tissues.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Produtos da Carne/análise , Resíduos de Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Triazinas/análise , Animais , Calibragem , Hormônios Juvenis/análise , Limite de Detecção , Reprodutibilidade dos Testes
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