Usefulness of parallel factor analysis to handle the matrix effect in the fluorescence determination of tetracycline in whey milk

• Published in: Analytica chimica acta 2009-01, Vol.632 (1), p.42-51
• Main Authors: Rodríguez, Noelia, Real, Blanca D., Cruz Ortiz, M., Sarabia, Luis A., Herrero, Ana
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Animals; Calibration; Chemistry; D-optimal; Exact sciences and technology; Experimental design; Fluorescence spectrophotometry; Fluorescent Dyes - analysis; Fluorescent Dyes - chemistry; Milk - chemistry; Milk Proteins; Models, Biological; PARAFAC; Spectrometric and optical methods; Spectrometry, Fluorescence; Tetracycline; Tetracycline - analysis; Tetracycline - chemistry; Whey milk; Whey Proteins
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2008.10.051

The determination of tetracycline by fluorescence spectrophotometry in complex matrices has some difficulties, because the presence of other compounds in the matrix affects the analytical signal. In this work, the effect of some inorganic species that are present in whey milk on the fluorescence signal of tetracycline is studied using a D-optimal experimental design. Next, an experimental strategy is proposed in conjunction with Parallel Factor Analysis, PARAFAC, modeling that leads to suitably modeling the severe matrix effect in the determination of tetracycline in whey milk. A specific design is performed in such a way that the lack of trilinearity due to the effect of the presence of interferents on the signal is obviated. Then, ten test samples from three brands of milk, spiked with different quantities of tetracycline and measured in 2 days were analysed using this methodology (mean of the absolute value of the relative errors: 5.1%). The developed analytical method fulfils the property of trueness, the relative errors being, both in calibration and prediction, inside the interval set by Commission Decision 2002/657/EC at these concentration levels. Decision limits (CC α) at x 0 = 0 μg L −1 and at x 0 = 100 μg L −1 were 13.2 and 112.4 μg L −1 respectively, for α = 0.05; whereas detection capabilities (CC β) were 25.9 μg L −1 and 124.4 μg L −1 respectively for α = β = 0.05.