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1.
Talanta ; 85(3): 1500-7, 2011 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-21807215

RESUMO

Pesticides residues in aquatic ecosystems are an environmental concern which requires efficient analytical methods. In this study, we proposed a generic method for the quantification of 13 pesticides (azoxystrobin, clomazone, diflufenican, dimethachlor, carbendazim, iprodion, isoproturon, mesosulfuron-methyl, metazachlor, napropamid, quizalofop and thifensulfuron-methyl) in three environmental matrices. Pesticides from water were extracted using a solid phase extraction system and a single solid-liquid extraction method was optimized for sediment and fish muscle, followed by a unique analysis by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Limits of quantification were below 5 ng L(-1) for water (except for fluroxypyr and iprodion) and ranged between 0.1 ng g(-1) and 57.7 ng g(-1) for sediments and regarding fish, were below 1 ng g(-1) for 8 molecules and were determined between 5 and 49 ng g(-1) for the 5 other compounds. This method was finally used as a new routine practice for environmental research.


Assuntos
Sedimentos Geológicos/química , Músculos/química , Resíduos de Praguicidas/análise , Praguicidas/análise , Poluentes Químicos da Água/análise , Acetamidas/análise , Acetamidas/isolamento & purificação , Aminoimidazol Carboxamida/análogos & derivados , Aminoimidazol Carboxamida/análise , Aminoimidazol Carboxamida/isolamento & purificação , Animais , Benzimidazóis/análise , Benzimidazóis/isolamento & purificação , Carbamatos/análise , Carbamatos/isolamento & purificação , Fracionamento Químico/métodos , Cromatografia Líquida/métodos , Monitoramento Ambiental/métodos , Peixes , Hidantoínas/análise , Hidantoínas/isolamento & purificação , Isoxazóis/análise , Isoxazóis/isolamento & purificação , Metacrilatos/análise , Metacrilatos/isolamento & purificação , Naftalenos/análise , Naftalenos/isolamento & purificação , Niacinamida/análogos & derivados , Niacinamida/análise , Niacinamida/isolamento & purificação , Oxazolidinonas/análise , Oxazolidinonas/isolamento & purificação , Resíduos de Praguicidas/isolamento & purificação , Praguicidas/isolamento & purificação , Compostos de Fenilureia/análise , Compostos de Fenilureia/isolamento & purificação , Propionatos , Pirimidinas/análise , Pirimidinas/isolamento & purificação , Quinoxalinas , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos , Estrobilurinas , Compostos de Sulfonilureia/análise , Compostos de Sulfonilureia/isolamento & purificação , Espectrometria de Massas em Tandem/métodos , Tiofenos , Poluentes Químicos da Água/isolamento & purificação
2.
J Chromatogr A ; 1218(34): 5743-56, 2011 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-21783197

RESUMO

One of the factors that may explain nowadays honeybees' colonies losses is the increasing presence of chemicals in the environment. The aim of this study is to obtain a global view of the presence of environmental contaminants in beehives and, develop a fast, cheap and sensitive tool to analyze environmental contaminants in apiarian matrices. A multi residue analysis was developed to quantify 80 environmental contaminants, pesticides and veterinary drugs, belonging to different chemical classes, in honeys, honeybees and pollens. It consists in a single extraction, based on a modified "QuEChERS method", followed by gas chromatography coupled with Time of Flight mass spectrometry (GC-ToF) and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The "QuEChERS method" combines salting-out liquid-liquid extraction with acetonitrile and a dispersive-SPE clean up. It was adjusted to honey and especially to honeybee and pollen, by adding a small fraction of hexane in acetonitrile to eliminate lipids that interfere with mass spectrometry analysis. This method, combined with accurate and sensitive detection, allowed quantification and confirmation at levels as low as 10 ng/g, with recoveries between 60 and 120%. Application to more than 100 samples of each matrix was achieved for a global view of pesticide presence in the honeybee environment. Relatively high percentages of honeys, honeybees and pollens were found to be contaminated by pesticides used to combat varroa but also by fungicides like carbendazim and ubiquitous contaminants.


Assuntos
Abelhas/química , Cromatografia Gasosa/métodos , Cromatografia Líquida/métodos , Poluentes Ambientais/análise , Mel/análise , Pólen/química , Extração em Fase Sólida/métodos , Espectrometria de Massas em Tandem/métodos , Animais , Resíduos de Drogas/análise , Sensibilidade e Especificidade
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