Resumo

SCHETTINO, Beatriz et al. ANALYSIS OF ROBUSTNESS IN THE DETERMINATION OF FATTY ACIDS BY GAS CHROMATOGRAPHY ON GOAT MILK. Rev Salud Anim. [online]. 2011, vol.33, n.2, pp.83-89. ISSN 0253-570X.

The determination of fatty acid profiles in milk sample by gas chromatography includes various steps such as: extraction, esterification, separation, identification and quantification, each one must be optimized to achieve accurate and precise results. Robustness is one of the parameters that are required for the development of the validation protocol and indicates the sensitivity of the analytical method to minor variations and provides a reasonable indication of their reliability. The effect of seven variables in eight experiments were evaluated in accordance with the provisions Statistical Manual of the AOAC, the selected factors were: Volume of sodium methoxide (100 ± 10 mL); calcium chloride (0.2 ± 0.5g) and time (60 ± 20 min) in the derivatization procedure; injector temperature (250 ± 5°C); detector temperature (260 ± 5°C); temperature initial in the oven (50 ± 2°C) and two operators. The results of the analysis on short-chain fatty acids, medium, long, C16: 0 and C18: 1 in goat milk allowed to determine the influence of each parameter. The effects on the means showed that none of the changes made on the seven parameters studied to affected the results to be below those required acceptance limit (Ö2 x SD), so we can say that the method was robust to changes made operational.

Palavras-chave : robustness; fatty acid; goat milk.

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