Extração por fluido supercrítico de alguns inseticidas carbamatos em amostras de batata, com determinação por HPLC/fluorescência e confirmação por HPLC/espectrometria de massas


Autoria(s): Nunes, Gilvanda Silva; Santos, Teresa Cristina R.; Barceló, Damiá; Pimenta, Alexandre Santos; Ribeiro, Maria Lúcia
Contribuinte(s)

Universidade Estadual Paulista (UNESP)

Data(s)

20/05/2014

20/05/2014

01/05/2002

Resumo

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Six supercritical fluid extraction (SFE) methods were tested, by varying the following operational parameters: CO2 pressure, time and temperature of extraction, type and proportion of static modifier, and Hydromatrix®/sample rate into cell. Firstly, insecticide carbamates were extracted from spiked potatoes samples (fortification level of 0,5 mg.Kg-1) by using SPE procedures, and then final extracts were analyzed HPLC/fluorescence. Good performance was observed with SFE methods that operated with values of temperature and CO2 pressure of 50 ºC and 350 bar, respectively. Best efficiency was obtained when it was used acetonitrile as a modifier (3% on the cell volume), and Hydromatrix®/sample rate of 2:1. Static time was of 1 min; total extraction time was of 35 min; dynamic extraction was performed with 15 mL of CO2, and it was used methanol (2 mL) for the dissolution of the final residue. In such conditions, pesticide recoveries varied from 72 to 94%, depending on the analyzed compound. In higher extraction temperatures, a rapid degradation was observed for some compounds, such as aldicarb and carbaryl; presence of their metabolites was further confirmed by HPLC-APCI/MS in positive mode. Detection limits for chromatographic analysis varied from 0,2 to 1,3 ng.

Formato

214-220

Identificador

http://dx.doi.org/10.1590/S0100-40422002000200008

Química Nova. Sociedade Brasileira de Química, v. 25, n. 2, p. 214-220, 2002.

0100-4042

http://hdl.handle.net/11449/27577

10.1590/S0100-40422002000200008

S0100-40422002000200008

S0100-40422002000200008.pdf

Idioma(s)

por

Publicador

Sociedade Brasileira de Química

Relação

Química Nova

Direitos

openAccess

Palavras-Chave #SFE method #HPLC/FS #HPLC-APCI/MS #potatoes #pesticides #carbamate insecticides
Tipo

info:eu-repo/semantics/article