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A new method to quantify the mycotoxin ochratoxin A (OTA) in coffee and tea samples is proposed based on second-order multivariate calibration and excitation-emission fluorescence matrix (EEFM) data. Experimental conditions were optimized by studying the effect of pH and various organized media on the fluorescence signal of OTA. For each analysed matrix (coffee grains and tea leaves), several sample pretreatments and calibration methods (external or standard addition) and data processing by chemometric models (e.g., parallel factor anal
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