Validation and uncertainty analysis of a multiresidue method for 42 pesticides in made tea, tea infusion and spent leaves using ethyl acetate extraction and liquid chromatography-tandem mass spectrometry.

A rapid, specific and sensitive multiresidue method to determine 42 pesticides in made tea, tea infusion and spent leaves has been developed and validated for the routine analysis by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was reproducible (Horwitz ratio (HorRat) <0.5 at 50 ng/g) and validated by the analysis of sample spiked at 50 and 100 ng/g in made tea, tea infusion and spent leaves. The samples were extracted with ethyl acetate+cyclohexane (9:1; v/v), and the extracts were cleaned up by dispersive solid phase extraction with primary secondary amine sorbent+graphitized carbon black+Florisil. The recoveries of all the pesticides were between 70% and 120% with a relative standard deviation of less than 15% and correlation coefficient for each pesticide was R(2) > or =0.99. The matrix effect on signal of respective compounds was measured by comparing matrix-matched calibration standards with those in solvent-only. The limits of quantitation (LOQ) met the requirements of the maximum residue limits (MRLs) for pesticides in tea as recommended by the European Union.