Simultaneous determination of chiral pesticide flufiprole enantiomers in vegetables, fruits, and soil by high-performance liquid chromatography
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A simple and reliable method for the simultaneous determination of chiral pesticide flufiprole enantiomers using high-performance liquid chromatography has been established. The separation and determination were performed using reversed-phase chromatography on a carbamoyl–cellulose-type chiral stationary phase, a Lux Cellulose-2 column. The effects of different mobile phase composition on separation were discussed. The absolute configuration of flufiprole enantiomers was measured through the combination of experimental and predicted ECD spectra. An Alumina-N solid-phase extraction (SPE) column was used in the cleanup of the vegetables, fruits, and soil samples. The method was evaluated by the specificity, matrix effect, linearity, precision, accuracy and stability. The mean recoveries of two enantiomers ranged from 86.8 to 98.9 %, with 1.1–6.4 % intra-day relative standard deviation (RSD) and 1.2 to 5.8 % inter-day RSD. Good linearity (R 2 > 0.998) was obtained for all analyte matrix calibration curves within the range of 0.2–20 mg L−1. The limit of detection for two enantiomers in the six matrices was 0.007–0.008 mg kg−1, whereas the limit of quantification of two enantiomers in fruits, vegetables, and soil was 0.021–0.025 mg kg−1. The results confirmed that this method was convenient and accurate for the simultaneous determination of flufiprole enantiomers in food and environmental samples.
KeywordsFlufiprole Enantioseparation HPLC Enantiomer analysis Absolute configuration
This work was supported by the National “863” High-Tech Research Program of China (2011AA100806) and the Special Fund for Agro-scientific Research in the Public Interest (201203022).
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