A fast and direct method for determination of milk adulteration by monitoring of calcium and sodium concentrations variations was described. Milk samples were furnished by a dairy company located at São Carlos (São Paulo State, Brazil) and spiked with tap-water, whey, hydrogen peroxide, synthetic urine, urea and synthetic milk in the ranged from 5% to 50% (v/v), expect for caustic soda. Caustic soda was added in the milk until establish the original pH. The milk samples were analyzed by using flame atomic absorption spectrometry (FAAS) and no acid digestion process was required. Results showed a significant decrease in the Na and Ca concentrations with addition of synthetic milk and tap-water, a nonlinear variation with addition of synthetic urine, whey and hydrogen peroxide and a largest increase in the Na concentration with addition of NaOH. Correlation between Na and Ca concentrations in pure and adulterated milk were evaluated by paired t-test at a 95% confidence level. Results showed that the method proposed is efficient to identify samples adulterated with tap-water, caustic soda, synthetics milk and urine.
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