Multiresidue Method for the Rapid Determination of Pesticide Residues in Tea Using Ultra Performance Liquid Chromatography Orbitrap High Resolution Mass Spectrometry and In-Syringe Dispersive Solid Phase Extraction

Abstract

A method based on in-syringe dispersive solid phase extraction (IS-D-SPE) and ultra performance liquid chromatography Orbitrap high resolution mass spectrometry for the multiresidue analysis of 117 pesticides in tea was developed. Full scan mode was acquired over an <i>m</i>/<i>z</i> range of 100-800 with Orbitrap resolution at 70000, followed by full scan/dd-MS² mode for confirmation. The identification criteria of retention time and mass accuracy tolerance was ±0.20 min and ±5.0 ppm, respectively. MS/MS fragment ions obtained dd-MS² were necessary to identify the pesticides with the same molecular mass weight. The IS-D-SPE technique involved a mixture of 200 mg PSA, 100 mg C18, and 15 mg multiwalled carbon nanotubes for the cleanup of tea matrix. Good linearity (<i>R</i>² > 0.99) for 117 pesticides was obtained. Satisfactory recoveries in the range of 70-120% were obtained for 105 pesticides, while intraday and interday precisions were below 20%. Limits of quantification were generally 10 μg kg^-1. Finally, this method was employed to analyze 117 pesticides in 70 tea samples.