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Verifying the performance in the determination of ochratoxin by immunoaffinity column cleanup and high performance liquid chromatography in a laboratory using single laboratory validation

Ochratoxin A is a food contaminant which can appear in several foods and can be harmful not only to human health, but also to the economy. In order to quantify properly an analite, even when using standard methods, it is necessary to check the validation method requirements. Therefore, a single laboratory validation of the method using immunoaffinity column and high performance liquid chromatography in spiked samples of ground green coffee beans was conducted. The evolution of the measurements along the analyte was sigmoid, as expected, and the range showed botton between 0.489 and 1.59, and top between 220 and 300 μg.kg-1, top. Linear regression was not rejected in this range and there was no external significant interference in the model. The intercept was in the origin and the linear coefficient did not differ significantly from 1.00 (p < 0.05). The standard deviations depended on the concentrations of ochratoxin A, similarly to studies in the literature, and the estimated values of the relative standard deviation obtained were in accordance with the values from those studies. Therefore, the laboratory proved competence in this measurement process, especially for green coffee beans.

food safety; range; outliers; precision; metrology


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