Determination of Atrazine and Its Metabolite Residues in Aquatic Products by Gas Chromatography£­Tandem Mass Spectrometry with Solid Phase Extraction

KeyWord:gas chromatography£­tandem mass spectrometry  atrazine  metabolites  solid phase extraction  aquatic products

Abstract:

      Atrazine£¨ATR£© is one of the most widely utilized triazine herbicides. The environmental pollution and potential risk to aquatic products safety caused by ATR and its residues are becoming more and more prominent£®In this study£¬a gas chromatography£­tandem mass spectrometry£¨GC£­MS/MS£© with solid phase extraction£¨SPE£© was developed for the quantitative determination of ATR and its main metabolites£¬including deethylatrazine£¨DEA£©£¬didealkylatrazine£¨DDA£© and deisopropylatrazine£¨DIA£© in aquatic products£®The parameters affecting the extraction and purification efficiency£¬such as type of extraction solvent£¬mode of purification method were optimized£®The analytes in aquatic products were extracted with acetonitrile£¬then purified on a GCB/NH2 solid phase extraction column£¬finally analyzed by GC£­MS/MS under multiple reaction monitoring£¨MRM£© mode£®Results showed that there were good linear relationships for ATR£¬DEA£¬DDA and DIA in the concentration range of 0.5£­100.0 ¦Ìg/L with their correlation coefficients£¨r2£© of 0.999 1£­0.999 9£®The limits of detection£¨LOD£© were between 0.02 ¦Ìg/kg and 0.13 ¦Ìg/kg. Meanwhile£¬the average recoveries for the samples at three spiked levels of 10.0£¬20.0 and 50.0 ¦Ìg/kg ranged from 83.6% to 98.4%£¬with relative standard deviations£¨RSD£¬n = 3£© of 3.6%£­8.1%£®Furthermore£¬the contaminant occurrence of ATR and its metabolites in aquatic organisms from the Xiangshan Harbor were analyzed£¬and ATR£¬DEA and DIA were all detected in the collected samples. Given the high detection rate of ATR and its metabolites£¬further investigation on aquatic products safety risks are needed£®With excellent accuracy£¬sensitivity and precision£¬the method provided a good technique support for the monitoring and risk evaluation of ATR and its metabolites in aquatic products.