Determination of Imidacloprid Residues and Pyrimethanil Residues in Green Vegetable (Brassica rapa var. chinensis) by Ultra Performance
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Abstract:
A method for simultaneous determination of imidacloprid residues and pyrimethanil residues in green vegetable (Brassica rapa var. chinensis) by using Ultra performance liquid Chromatography-Tandem Mass Spectrometry (UPLC/MS/MS) was established in this paper. The green vegetable (Brassica rapa var. chinensis) samples were extracted by acetonitrile and purified by an amino solid phase extraction (SPE) column (eluted by acetonitrile + toluene (3+1)), and then the gradient elution was applied in ultra performance liquid chromatography separation by using the acetonitrile -0.1% formic acid solution as mobile phase. Samples were detected by mass spectrometry multi reaction monitoring model, using retention time and sub-ion ratio as qualitative analysis and the external standard method as quantitative analysis. Tandem mass spectrometry with electrospray ionization and multiple reaction monitoring interface in an external standard manner. The results showed that the limits of quantitation (LOQ) of imidacloprid and pyrimethanil were 3.1×10-6 mg/kg and 3.6×10-7 mg/kg respectively, and the correlation coefficients of two pesticides were more than 0.9995 in the linear range of 0.0005~0.5 mg/L. In addition, the average recoveries were 99.1 %~105.8 % for imidacloprid and 99.1 %~110.0 % for pyrimethanil in the range of 0.02-0.2 mg / kg, and the relative standard deviations (RSD) were less than 1.23 % and 1.64 %, respectively. The proposed method had the advantages of simple operation, wide linear range, high sensitivity and reliabilty, which met the requirements for the detection of such drug residues in vegetables at home and abroad.
