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The extraction solution and cleanup procedure had been optimized, and good sensitivity, accuracy, and precision were obtained. The calibration curves of AGs were linearity (<jats:italic>R<\/jats:italic><jats:sup>2<\/jats:sup> &gt; 0.99) in the range of 2.0 to 200 \u03bcg\/L (or 5.0 to 500 \u03bcg\/L). The limits of detection of AGs were between 10 and 25 \u03bcg\/kg. The recoveries of AGs ranged from 74.9% to 94.3%, and the intraday and interday relative standard deviations were less than 15%. Finally, this method was successfully applied to determine ten AGs in 30 aquatic feed samples. 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