Abstract:With the development of modern agriculture, pesticide is extensively used in agricultural production. The herbicide as an important part of pesticide has also been widely used, causing significant environmental and food safety concerns. Currently, effect of herbicide contamination on the aquatic food product is not well understood. Furthermore, detection of herbicide residues in aquatic products is lack of efficient multi-residue detection method. This study established a reliable method for determining 16 herbicide residues in animal origin aquatic products. The method involves gel permeation chromatography- solid phase and extraction-gas chromatography-mass spectrometry. The sample was extracted using dichloromethane and ethyl acetate mixed solution, followed by a clean-up step using gel permeation chromatography. The product was then purified by solid phase extraction column. Results were determined by monitoring selected ion and quantified by external marker method. Good linearity was observed in the range of 4-200 μg/L in pendimethalin and cyanizine, whereas other herbicides showed good linearity in the range of 2-100 μg/L, with correlation coefficient higher than 0.9970 in both cases. The quantitation limit for propazine, atrazine, terbutylazine, simazine, desmetryn, prometryn, ametryn and metolachlor was 1.0 μg/kg. The quantitation limit for acetochlor, alachlor, butachlor, pretilachlor, cyprazine and simetryn was 1.5 μg/kg, and the quantitation limit for pendimethalin and cyanizine was 2.0 μg/kg. Average recovery rates ranged in 67.2%-103.0% and relative standard deviation of the method was 5.1%-9.5%. The method had good reproducibility and high recovery rate. In terms of residue detection, the precision and accuracy can meet the testing requirements, and the method could be used for determining 16 herbicide residues in aquatic products. The established method was applied to detect herbicides in sea cucumber, oyster, scallop etc. The results showed that ametryn had the highest detection rate in these samples and followed by atrazine, terbutylazine, simetryn and acetochlor. This study established the method for simultaneous detection of herbicide residues in aquatic products and built the foundation for further study of the impact of herbicide pollution on the quality and safety of aquatic products.
