Determination of Carbamates Pesticide Residues in Chinese Herbal Pieces by GPC-SPE-UPLC-MS/MS / 中国药师

ABSTRACT

Objective:To set up an automatic gel permeation chromatography-solid phase extraction purification-ultra performance liquid chromatography-tandem mass spectrometry ( GPC-SPE-UPLC-MS/MS ) method for the quantitative determination of 14 carba-mates pesticide residues in Chinese herbal pieces. Methods:The samples were extracted by acetonitrile, and kept in constant volume with ethyl acetate-cyclohexane (1 1, v/v). The extract was purified by GPC combined with amino solid phase extraction column (Carb/NH2). After UPLC gradient elution separation on an Agilent Poroshell 120EC-C18 column using acetonitrile-0. 1% formic acid as the mobile phase,the target pesticides were determined by tandem mass spectrometry in a multi-reaction monitoring ( MRM) mode. Results:The 14 kinds of carbamates pesticides had good linear relationships within the range of determination (r>0. 9990), and the detection limit was 0. 02-0. 35μg·kg-1 . When the spiked levels were 1, 10 and 50μg·L-1 , the recoveries were 74. 2%-108. 8%, and the RSD was 1. 25%-6. 73%(n=6). Conclusion:The method simplifies the pretreatment operation and shortens the analysis time with good selectivity and high sensitivity, which can be used for the determination of carbamates pesticide residues in Chinese herbal pieces.