Validation and Uncertainty Analysis of a Multiresidue Method for 67 Pesticides in Made Tea, Tea Infusion, and Spent Leaves Using Ethyl Acetate Extraction and Gas Chromatography/Mass Spectrometry

Abstract

A rapid, specific, and sensitive multiresidue method to determine 67 pesticides in made tea, tea infusion, and spent leaves was developed and validated for routine analysis by GC/MS with an approximately 29 min GC run time. The method was reproducible (HorRat < 0.5 at 50 ng/g) when validated at 50 and 100 ng/g. The samples were extracted with ethyl acetate-cyclohexane (9 + 1, v/v), and the extracts were cleaned up by dispersive SPE with primary-secondary amine sorbent + graphitized carbon black + Florisil. The recoveries of all the pesticides were within 70-120% with an RSD of < 20% at 50 ng/g and R2 > 0.99. The matrix effect on the signals of the compounds was corrected by using matrix-matched calibration standards. The LOQ met the requirements of the maximum residue limits for pesticides in tea as recommended by the European Union.