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| Determination of Amide Herbicides and Their Metabolites by GC－MS in Aquatic Products |
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| DOI： |
| KeyWord:gas chromatography－mass spectrometry（GC－MS） amide herbicides aquatic products pesticide residues |
| Author | Institution |
| PENG Zhong-xiao，ZHANG Hua-wei，LI Jia-wei，GONG Xiang-hong，ZHANG Xiu-zhen，XU Ying-jiang，WANG Dan，LIU Yong-chun |
1. College of Food Science and Technology，Shanghai Ocean University，Shanghai ，China; 2. Shandong Marine Resource and Environment Research Institute，Yantai ，China |
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| Abstract: |
| A method was established for the simultaneous determination of 5 amide herbicides，i.e. acetochlor，alachlor，metolachlor，butachlor and pretilachlor，as well as their metabolites including 2-ethyl-6-methylaniline（MEA） and 2， 6-diethylaniline and（DEA） in aquatic products by gas chromatography－mass spectrometry（GC－MS）．Based on previous studies，the pretreatment conditions and chromatographic conditions were optimized in this paper．The appropriate characteristic ions were selected to achieve the chromatographic separation and determination for five amide herbicides and their metabolites in aquatic products．In the sample pretreatment，the mixing parameters for the extractant were optimized，the appropriate eluent and elution volume were selected，and the heating program for the chromatographic column was optimized to make the separation effect better．Specific method and process were as following：the sample was firstly extracted with dichloromethane－ethyl acetate（3∶2，by volume），then concentrated with nitrogen blowing，purified by HLB solid phase extraction，eluted with 3 mL n-hexane，and finally quantified by GC－MS detection．Results showed that，after optimizing the detection conditions，there were good linear response values in the mass concentration range of 1.0－25 μg/L for MEA，DEA and metolachlor，and 2.0－50 μg/L for the other four herbicides．Meanwhile，the correlation coefficients（r2） were greater than 0.998 8．The spiked recoveries for Mactraveneriformis at low，medium and high levels ranged from 69.7% to 111%，with the relative standard deviations（RSDs） of 0.40%－7.6%．The recoveries for Sebastes schlegelii ranged from 65.3% to 118%，with the RSDs of 1.7%－9.3%．The recoveries for Portunustrituberculatus ranged from 61.4% to 113%，with the RSDs of 0.90%－7.1%．The limits of detection（LODs） and limits of quantification（LOQs） for MEA，DEA and metolachlor were 0.5 μg/kg and 1.5 μg/kg，respectively．The LODs and LOQs for the remaining four herbicides were 1.0 μg/kg and 3.0 μg/kg，respectively．This method was used to detect Mactraveneriformis，Scophthalmus maximus，Fenneropenaeuschinensis and Cynoglossussemilaevis samples in the coastal waters of Shandong Province．The metabolite MEA was detected in one of the Mactraveneriformis samples with a detection rate of 2.5%．The sensitivity and precision of this method could meet the requirements for pesticide residue detection，and was suitable for the detection on 5 kinds of amide herbicides and their metabolites in aquatic products． |
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