Simultaneous determination of 317 kinds of pesticide residues in pomelo flowers by ultra performance liquid chromatography-tandem mass spectrometry coupled with QuEChERS
Objective To establish a method for simultaneous determination of 317 kinds of pesticide residues in pomelo flowers by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)coupled with QuEChERS extraction.Methods Pomelo flowers samples were extracted with acetonitrile and salted with extraction salt pack,cleaned up by ethylenediamine-N-propylsilane silica gel(PSA)and graphitized carbon blank(GCB),the analytes were separated on an ACQUITY UPLC HSS T3 column to achieve the separation within 30 min.The 317 kinds of pesticides were detected in electron spray ionization with positive ion mode and electron spray ionization with negative ion mode with multiple reaction monitoring(MRM)mode and quantified by matrix matching curve external standard method.Results The 317 kinds of pesticides in pomelo flowers showed good linearity with correlation coefficients(r)greater than 0.995 within the range of 2.0-200.0 µg/L,and the limits of quantification were 0.002-0.010 mg/kg,the average recoveries at 3 spiked levels were 74.3%-120.3%,and the relative standard deviations were 0.36%-10.00%.Conclusion The method is simple,rapid,accurate and sensitive,can meet the rapid detection requirements of 317 kinds of pesticides in pomelo flowers and provide reliable data support for further standardizing for edible safety evaluation of pomelo flowers.
QuEChERSultra performance liquid chromatography-tandem mass spectrometrypomelo flowerspesticide residues