A simple, selective and sensitive procedure for the confirmation of 14 sulfonamide antibacterials in milk was developed. The milk samples were homogenized, extracted and deproteinized by acetonitrile and defatted by n-hexane. Analysis was performed by liquid chromatography with tandem mass spectrometry (LC-MS/MS) in positive mode for all 14 analytes. Mass spectral acquisition was performed in the multi reaction monitoring mode (MRM), selecting two structurally significant transitions per compound. The calibrations were performed in sample matrixes and the interference effect of sample matrixes on the ionization was effectively eliminated. Good linear relationship (R2=0.992～ 0.999) were observed at 6 concentrations of 2.5～100 ng/g. Satisfied recoveries (86.3～110.2%) of all sulfonamides were demonstrated in spiked milk at three levels from 5 to 20 ng/g. The limits of quantitation (LOQs) for sulfonamides ranged from 0.25～2.1 ng/g.

Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low(0.021-0.058㎎/㎏).

Organophosphate pesticides were extracted with 70% acetone and then transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil The final extract was analyzed by gas chromatography with nitrogen-phosphorus detector(GC/NPD). Recoveries of the 18 organophosphate pesticides were ranged from 88.7% to 100.0% for the narrow-bore capillary GC(Ultra-2). The minimum detectable level of this analytical method was 0.019 - 0.035 ㎎/㎏. Sample throughput(extraction, open-column chromatography, and GC analysis) was decreased considerably (8h per sample).