수출입 농산물의 잔류농약 검사를 위한 유기인계 농약 8종의 동시 분석

This experiment was conducted to establish a simultaneous analytical method for 8 kinds of organophosphorus pesticides of 3 different purposes with similar physicochemical characteristics as insecticide(chlorpyrifos-methyl, mecarbam, parathion- methyl, phenthoate, prothiofos and tebupirimfos), fungicide(iprobenfos), and herbicide (anilofos) in crops using GC-NPD/MS. All the pesticides residues were extracted with acetone from representative samples of five raw products which comprised mandarin, green pepper, kimchi cabbage, hulled rice and soybean. The extract was diluted with large volume of saline water and directly partitioned into n-hexane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/ acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized florisil column chromatography. The analytes were separated and quantitated by GLC with NPD using a DB-17 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with anilofos, chlorpyrifos-methyl, iprobenfos, mecarbam, parathion-methyl, phenthoate, prothiofos and tebupirimfos at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 80.5 to 105.0% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation(LOQ) of the analytes were 0.004(tebupirimfos, chlorpyrifos-methyl and parathion-methyl) and 0.008(iprobenfos, mecarbam, prothiofos, phenthoate and anilofos) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of anilofos, chlorpyrifos-methyl, iprobenfos, mecarbam, parathion-methyl, phenthoate, prothiofos, and tebupirimfos in import-export agricultural products.