Validation of analytical methods: case study

The study continues the research previously published in the article «Validation of analytical methods: the international requirements» (Zavod. Lab. Diagn. Mater. 2018. Vol. 84. No. 12, pp. 25 – 31). We consider the procedure and the results of validation of the measurement procedure for determination of the residual content of enrofloxacin in food using high performance liquid chromatography with mass spectrometric detection. The program of experimental studies and calculation formulas necessary to assess the metrological characteristics of the method are presented. Validation included assessment of the detection limit, quantitation limit, decision limit, capability of enrofloxacin detection in food samples in accordance with GOST 32797–2014 «Food products, food raw materials. Method for the determination of the residual content of quinolones using high performance liquid chromatography with a mass spectrometric detector». The linearity of the calibration characteristic within the measurement range is demonstrated using the regression analysis procedure. The values of the accuracy indicators and the measurement range specified in GOST 32797–2014 were confirmed when the method was implemented in a testing laboratory.

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