Determination of 2,4-D Butylate Residue in Husked Rice,Wheat and Maize by Dispersive Solid Phase Extraction-Triple Quadrupole Gas Chromatograph Mass Spectrometer
A method for the analysis of 2,4-D butylate residues in husked rice,wheat and maize was established by dispersive solid phase extraction-triple quadrupole gas chromatograph mass spectrometer.The samples were soaked in water,extracted with acidified acetonitrile,purified by C18,primary secondary amine and magnesium sulfate,dried by nitrogen and filled to specified volume with ethyl acetate,analyzed by triple quadrupole gas chromatograph mass spectrometer and multiple reaction monitoring mode,with matrix matched standard curve,and quantified by internal standard method.After optimizing the mass spectrometry parameters,extraction and purification conditions,and matrix effects,the linear relationship of 2,4-D butylate was good in the range of 0.001 mg·L-1 to 0.500 mg·L-1,and the R2 was greater than 0.999,the limit of detection of the method was 0.001 mg·kg-1,and the quantification limit was 0.005 mg·kg-1,the average recovery rate under the three spiked gradients of 0.005 mg·kg-1,0.050 mg·kg-1 and 0.500 mg·kg-1 was between 91.9%and 108.0%,and the relative standard deviation was between 2.59%and 6.35%(n=6).This method is simple and easy to perform and is highly sensitive,can effectively determine the 2,4-D butylate residues in husked rice,wheat and maize.
2,4-D butylatedispersive solid phase extractiontriple quadrupole gas chromatograph mass spectrometergrain
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