Abstract: A method was developed for the determination of 20 kinds of pesticide residues in soybeans and corn with the technique of offline disperse solid-phase extraction and gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The pesticides interested were extracted twice from the samples with acetonitrile. The combined extract was concentrated to dryness and redissolved in acetonitrile, then cleaned up by dispersive solid-phase extraction with sorbents of N-propyl ethylene diamine （PSA）, graphited carbon black, and C18, and determined and confirmed by GC-NCI/MS. The recoveries of all pesticides were in the range of 70%-130% at three spiked levels （5, 10 and 20 μg/kg）, and the relative standard deviations were below than 17%. The linearity of the method was good in the concentration range of 20-400 μg/L, and limits of quantification (LOQs) were no more than 2 μg/kg. The method is selective well with no interference and suitable for the confirmatory of pesticide residues in soybeans and corn.

Key words: corn , disperse solid-phase extraction, pesticide residues, selected ion monitoring, soybean, gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS)