Development and validation of the method for determination of amitraz in honey using high-performance liquid chromatography with mass spectrometric detection

Abstract

Method for determination of the insecticide amitraz residual content in honey has been developed and validated. The method is selective, express and easy-to-perform. The technique is based on the extraction of amitraz from alkalized aqueous solutions of honey with n-hexane and quantitative determination by high-performance liquid chromatography with mass spectrometric detection. Validation was performed using three types of honey at three levels of amitraz application 6, 120 and 220 µg/kg. The limit of quantification was 0.9 µg/kg, the calibration curves were linear in the concentration range from 2.5 to 125.0 ng/mL (the corresponding analyte content in honey is from 5.0 to 250.0 µg/kg), relative values of the standard deviations of repeatability and within-laboratory reproducibility did not exceed 3.4 and 5.9 %, respectively, the bias values varied from –8.2 to 5.6 %, the expanded uncertainty estimates of the results ranged from 12 to 16 % (P = 0.95). Instrumental limit of quantification, overall efficiency of the process and robustness were also evaluated during the validation process.