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

Hongping Chen; Guanwei Gao; Yunfeng Chai; Guicen Ma; Zhenxia Hao; Chen Wang; Xin Liu; Chengyin Lu

doi:10.1021/acsomega.7b00863

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

ACS Omega. 2017 Sep 30;2(9):5917-5927. doi: 10.1021/acsomega.7b00863. Epub 2017 Sep 18.

Authors

Hongping Chen¹, Guanwei Gao¹, Yunfeng Chai¹, Guicen Ma¹, Zhenxia Hao¹, Chen Wang¹, Xin Liu¹, Chengyin Lu¹

Affiliation

¹ Tea Research Institute, Chinese Academy of Agricultural Sciences, Key Laboratory of Tea Safety & Control, Key Laboratory of Tea Quality and Safety & Risk Assessment, Ministry of Agriculture, Hangzhou, 310008, China.

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 m/z 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 (R² > 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.