DESENVOLVIMENTO E VALIDAÇÃO DE MÉTODO ANALÍTICO POR DISPERSÃO DA MATRIZ EM FASE SÓLIDA E CROMATOGRAFIA EM FASE GASOSA ACOPLADA A ESPECTROMETRIA DE MASSAS PARA DETERMINAÇÃO DE PESTICIDAS EM AMOSTRAS DE OVOS DE GALINHA (GALLUS GALLUS DOMESTICUS). / DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR SCATTERING MATRIX SOLID PHASE AND GAS CHROMATOGRAPHY COUPLED TO A MASS SPECTROMETRY DETERMINATION OF PESTICIDES IN SAMPLES OF CHICKEN EGGS (GALLUS GALLUS DOMESTICUS).

AUTOR(ES)

Michel Rubens dos Reis Souza

FONTE

IBICT - Instituto Brasileiro de Informação em Ciência e Tecnologia

DATA DE PUBLICAÇÃO

30/07/2012

RESUMO

The eggs are of great nutritional value. Its biochemical composition indicates the source of proteins, lipids, vitamins and minerals. However, undesirable chemical compounds can form part of this constitution. The pesticides, when applied irregularly, can represent a serious health risk to consumers if detected above the maximum residue limits, can be identified in egg white and yolk. The objective of this study was to develop and to validate an analytical method for matrix solid phase dispersion and gas chromatography coupled with mass spectrometry for determination of atrazine, pirimicarb, lindane, permethrin, deltamethrin, cypermethrin, ethion, bifenthrin and alachlor in chicken eggs (Gallus gallus domesticus) marketed in the city of Aracaju-SE, Brazil. Among the sorbents were tested: silica, neutral alumina, Florisil and C18. The various combinations matrix/dispersant/co-column were analyzed. The system: matrix of lyophilized egg (0,25 g)/dispersant Florisil (1,5 g)/auxiliary column C18 (0,5 g) was more efficient. The acetonitrile (10 mL) was chosen as the eluting solvent. The recoveries (n = 3) ranged from 69,6 a 103,8% with relative standard deviation ranging from 16,2 a 45,5%. The validation of the analytical method was performed through the following parameters: the selectivity, its showing that the method is selective for all pesticides; the linearity, in terms of linear coefficient of the calibration curve, above 0,99 for all pesticides, for a given concentration range from 0,01 to 2,0 μg g-1; the sensibility, with the pesticide bifenthrin as the more sensitive and less sensitive to cypermethrin; the limits of detection and quantification limits in the intervals of 0,003 to 0,015 μg g-1 and 0,01 to 0,05 μg g-1, respectively; the recovery (n = 3), to levels 0,5, 1,0 and 1,5 μg g-1 ranged from 61,6 to 95%; the accuracy in terms of relative standard deviation (RSD) in the range of 0,13 to 29,92%; and application in real samples that showed in one of samples the pesticide bifenthrin in a concentration of 0,004 μg g-1, below the limit of quantification (

ASSUNTO(S)

ovo de galinha pesticidas dmfs cg/em liofilização quimica chicken eggs pesticides mspd gc/ms liofilization

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