Determination of triclopyr residue in cereal seeds by gas chromatography with derivatization
[Aims]This study aims to establish a method of gas chromatography with derivatization for the quantitative determination of triclopyr residue in cereal seeds.[Methods]Triclopyr was extracted by acetonitrile with 1％acetic acid.The extracted solution was evaporated under reduced pressure in water bath and dried with nitrogen at room temperature.The extract was dissolved in acetone,and then reacted with 14％boron trifluoride in methanol at 60 ℃ for 60 min.The derivative was extracted with n-hexane,detected by the gas chromatography coupled with electron capture detector(GC-ECD)and quantified by an external standard method.[Results]In the concentration range from 0.01 to 2.0 mg/L,the peak area values of triclopyr derivative showed good linearity with coefficient(r)of 0.9997.At the spiked levels from 0.01 to 1.0 mg/kg,the average recoveries of triclopyr in wheat,rice,millet and maize were in the range of 80.7％-101％,with the relative standard deviations(RSDs)of 1.42％-9.05％(n=5).The limit of quantification(LOQ)for triclopyr was 0.01 mg/kg in cereal seeds.[Conclusions]Triclopyr can be extracted by acetonitrile with acetic acid,derived to methyl ester and detected by GC-ECD.The proper analytical method has well separation,high sensitivity and good accuracy.It meets the requirements of pesticide residue analysis for monitoring the residue of triclopyr in cereal seeds.
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