Simultaneous determination of pyrimethanil, cyprodinil, mepanipyrim and its metabolite in fresh and home-processed fruit and vegetables by a QuEChERS method coupled with UPLC-MS/MS

Abstract

A QuEChERS procedure for the simultaneous determination of pyrimethanil, cyprodinil, mepanipyrim and its metabolite (M31) in fresh and processed fruit and vegetables was developed using ultra-performance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS). The determination of the four target compounds was achieved in less than 6.0 min using an electrospray ionisation source in positive mode. The limits of detection (LODs) were below 0.4 μg kg⁻¹, while the limits of quantification (LOQs) did not exceed 1.5 μg kg⁻¹ for all studied matrices. Good linearity of the calibration curves was obtained over the range from 0.002 to 2 mg kg⁻¹, with correlation coefficients higher than 0.999. The average recoveries of this method in apple, peach, cabbage and tomato at the five spiked levels (0.002, 0.01, 0.05, 0.20 and 2.0 mg kg⁻¹) ranged from 81.5% to 107.3% with relative standard deviations (RSDs) in the range of 1.5–13.9% (n = 5) for all analytes. Residue levels of anilinopyrimidine fungicides in fresh and home-processed apple, peach, cabbage and tomato were also studied. The results indicate that residue levels are significantly reduced following washing, peeling and boiling, and there is no toxic metabolite of mepanipyrim (M31) which is detected during boiling. This study provides a theoretical basis for China to draw up maximum residue limits (MRLs) and protect consumers from the negative health effects of pesticide residues detected in fruit and vegetables.

Keywords:

• anilinopyrimidine fungicides
• fruits
• vegetables
• UPLC-MS/MS
• home processed

Acknowledgements

This work was supported by the National Natural Science Foundation of China (31272070), the Technology New Star Program of Beijing (2011099), and the Public Service Sector R&D Project (200903033).