Determination of Clothianidin and Sulfoxaflor Residues in Pumpkin by QuEChERS-liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A QuEChERS-liquid chromatography-tandem mass spectrometry method was established for the simultaneous determination of clothianidin and sulfoxaflor residues in pumpkin. The clothianidin and sulfoxaflor were extracted with acetonitrile from the samples subjected to homogenization, purified by the matrix solid-phase dispersion method, filtered through a 0.22 μm filter membrane and analyzed by LC-MS /MS. The detection was performed after separation using a C18 chromatographic column, electrospray ionization, positive ion scanning mode and dynamic multi-reaction monitoring mode, and quantification was conducted by the matrix-matched external standard calibration. A linear relationship was found within the range of 2.5~100 μg/L for clothianidin and 0.5~20 μg/L for sulfoxaflor, with their correlation coefficients as 0.9994 and 0.9988, respectively. The average recoveries were 88.5%~111.2% at the three spiking levels of 5, 10 and 50 μg/kg for clothianidin, and 1, 2 and 10 μg/kg for sulfoxaflor, with the relative standard deviations in the range of 1.12%~6.92%. The limits of quantification (LOQs) were 1.0 and 5.0 μg/kg for clothianidin and sulfoxaflor respectively. The method is rapid, simple, sensitive, and reproducible, and can meet the requirements for the determination of clothianidin and sulfoxaflor residues in pumpkin.
