Determination of 13 Kinds of Sulfonylurea Herbicides Residues in Aquatic Products by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry / 分析化学

ABSTRACT

A sensitive method was proposed for determination of 13 kinds of sulfonylurea herbicides residues in aquatic products by solid phase extraction-ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (SPE-UPLC-MS/MS). The edible part of carp, penaeus vannamei,crab,clam and sea cucumber were collected and homogenized. Analytes was extracted with ethyl acetate,and then cleaned up by MAX solid phase extraction column. Qualitation of the analytes was achieved with multiple reaction monitoring (MRM) and the external standard method was used for quantification. The 13 kinds of sulfonylurea herbicides showed good linearity in the concentration range of 5.0-100.0 μg/L respectively. The detection limits of the 13 analytes were 1.0 μg/kg, and the limit of quantification was 2.0 μg/kg. The average recoveries ranged from 75.4% to 118.3% with relative standard deviations from 2.1% to 14.5%. The 13 target analytes were not detected in grass carp,carp,sea cucumber,prawn,turbot of breeding and crabs from the market. The halosulfuron-methyl was detected in the edible tissues of crabs exposed to a 1.0 mg/L halosulfuron-methyl solution for 24,48 and 72 h,and the concentrations were 6.20, 12.1 and 16. 6 μg/kg respectively. The method can be stable and sensitive, and is applied to the determination of 13 kinds of sulfonylurea herbicides residues in aquatic products.