Determination of 34 prohibited and restricted pesticide residues in Atractylodes by ultra-performance liquid chromatography-tandem mass spectrometry
Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the detection of 34 prohibited and restricted pesticide residues in Atractylodes,and 21 batches of commercially available Atractylodes were detected to preliminarily investigate the pesticide residues in commercial Atractylodes.Methods The samples were extracted with pure acetonitrile,the extracts were purified by Waters-HLB 3cc(60 mg)solid phase extraction column,separated by Waters-C18 column,0.1%formic acid water(containing 10 mmol/L ammonium formate)and acetonitrile were used as mobile phases(gradient elution),and quantitatively analyzed by external standard method in multi-reaction monitoring positive ion mode according to the retention time.Results The linear relationship of each component was good in their respective concentration ranges,the correlation coefficients were all greater than 0.998 0.The limits of detection were within 0.8-4.0 μg/kg,and the limits of quantification were within 2.0-10.0 μg/kg.The average recovery rate was 74.1%-97.4%,and RSD was 0.6%-6.4%(n=9).Seven pesticide residues were found in 13 batches of 21 Atractylodes macrocephalus samples.Conclusion This method is simple to operate,accurate in quantification,has high recovery rate and good repeatability,and is suitable for the detection of multiple residues of prohibited and restricted pesticides in Atractylodes.
AtractylodesPesticide residuesMatrixUltra performance liquid chromatography tandem mass spectrometry
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