Liquid chromatography–tandem mass spectrometry quantification of acetamiprid and thiacloprid residues in butterbur grown under regulated conditions

Abstract

An analytical method was developed to quantify the residual levels of the neonicotinoid insecticides, acetamiprid and thiacloprid, in field-incurred butterbur samples using liquid chromatography–tandem mass spectrometry (LC–MS/MS). Samples were extracted with acetonitrile and partitioned with dichloromethane. After partitioning, purification was conducted using a Florisil® cartridge. Linearity of a matrix-matched calibration curve of the two compounds over a concentration range of 0.004–0.4 μg/g was excellent, with determination coefficients (R2) ≥ 0.9998. The limits of detection (LOD) and quantitation (LOQ) for both acetamiprid and thiacloprid were 0.0006 and 0.002 mg/kg, respectively. The average recoveries for acetamiprid and thiacloprid at two spiking levels (0.02 and 0.1 mg/kg, i.e., 10 × LOQ and 50 × LOQ) were between 78.23 to 82.17%, with relative standard deviations (RSDs) ≤ 7.22%. The method was successfully applied to field-incurred samples treated with a commercial pesticide product, either once (zero or 7 days before harvest) or twice (0 and 7, 7 and 14, or 14 and 21 days before harvest). The highest and lowest residues were obtained for the 7 and 0 days’ treatment and the 21 and 14 days’ treatment, respectively. The developed method is simple and accurate and can be extrapolated to other leafy vegetables.