Rapid analysis of forchlorfenuron in fruits using molecular complex-based dispersive liquid–liquid microextraction

Abstract

ABSTRACT The main sample preparation method for analysis of pesticide residues in fruits is QuEChERS. In this study, a novel sample preparation method using molecular complex-based dispersive liquid–liquid microextraction is introduced with detection of forchlorfenuron by high-performance liquid chromatography coupled with diode array and mass spectrometric detection. Sample treatment involves initial extraction of a 5 g sample with 3 mL acetonitrile, and then the selective concentration of the analyte is performed using 150 µL tributyl phosphate by forming intermolecular hydrogen bonds with the analyte. The extraction mechanism was proved using ATR-FTIR. Under the optimised conditions, recovery rates varied between 88% and 107% for various sample matrices spiked at three levels in the range 0.01–0.1 mg kg−1. Intra-day and inter-day repeatabilities were in the ranges of 2.2–8.0% and 1.6–9.5%, respectively. Detection limit and quantitation limit were 0.33 µg kg−1 and 1.09 µg kg−1 for diode-array detection; 0.01 µg kg−1 and 0.04 µg kg−1 for tandem mass spectrometry detection. This method was successfully applied for the analysis of 149 various fruits. The analyte was found in 4 of the 149 samples and the contents were not over the specific maximum residue limit established by domestic and international regulations. Graphical Abstract