국내 사용금지 잔류성 유기염소계 살충제의 동시분석법 확립

This experiment was conducted to establish a simultaneous analytical method for 19 kinds of organochlorine insecticides (aldrin, α-BHC, β-BHC, γ-BHC, δ-BHC, cis-chlordane, transchlordane, p,p'-DDT, o,p'-DDT, p,p'-DDE, p,p'-DDD, dieldrin, endrin, δ-keto-endrin, heptachlor, heptachlor epoxide, α-endosulfan, β-endosulfan, and endosulfan sulfate) forbidden in Korea using GC-ECD/MS. These insecticide residues were extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. 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 quantitated by GLC-ECD/MS, using a DB-5 capillary column. The crops were fortified with each insecticide at 3 levels per crop. Mean recovery ratio were ranged from 76.5% to 116.0% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Quantitative limits of 19 kinds of organochlorine insecticides were ranged 0.003~0.01 mg/kg in crop samples. A GC-ECD/MS with selected-ion monitoring method was also provided to confirm the suspected residues. The proposed simultaneous analysis method was reproducible and sensitive enough to determine the residues of 19 kinds of organochlorine insecticides forbidden in Korea.