본 연구에서는 HPLC-UVD/MS를 이용하여 농산물 중 valinamide carbamate계 살균제 iprovalicarb의 잔류 분석법을 확립하였다. 대표 농산물은 사과, 고추, 배추, 현미 및 콩을 선정하였고, acetonitrile를 이용하여 추출한 iprovalicarb는 nhexane/ dichloromethane(20/80, v/v) 혼합용매를 이용한 액-액 분배법과 florisil 흡착크로마토그래피법으로 정제하여 HPLCUVD/ MS의 분석시료로 사용하였다. Iprovalicarb의 정량분석을 위한 최적 HPLC-UVD 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.04 mg/kg 이었다. 각 대표 농산물에 대한 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과, 모든 처리농도에서 87.5~101.6% 수준의 회수율을 나타내었고, 반복 간 변이계수(CV)는 최대 7.7%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, LC/MS/SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 iprovalicarb의 HPLC-UVD/MS 분석법은 국내·외 농산물 잔류농약 검사 시 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

This experiment was conducted to establish an analytical method for residues of iprovalicarb, as recently developed a valinamide carbamate fungicide showing effect on pathogens of the oomycetes, in crops using HPLC-UVD/MS for the official purpose. Iprovalicarb residue was extracted with acetonitrile from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with large volume of saline water and directly partitioned into n-hexane/dichloromethane(20/80, v/v) 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. On an octadecylsilyl column in HPLC, iprovalicarb was successfully separated from coextractives of sample, and sensitively quantitated by ultraviolet absorption at 210 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with iprovalicarb at 3 concentration levels per crop in each triplication. Mean recoveries ranged from 87.5 to 101.6% 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 iprovalicarb was 0.04 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

ABSTRACT
 서 언
 재료 및 방법
  1. 시약 및 기구
  2. 농산물 시료
  3. HPLC-UVD/MS 기기분석 조건
  4. 표준검량선 및 분석정량한계(Limit of quantitation, LOQ)
  5. Iporvalicarb의 추출 및 분배
  6. Florisil 흡착 크로마토그래피
  7. 대표 농산물에 대한 iprovalicarb의 회수율 시험
 결과 및 고찰
  1. HPLC 분석조건 확립
  2. 시료 중 iprovalicarb의 추출 및 분배과정의 확립
  3. Florisil 흡착 크로마토그래피 정제조건의 최적화
  4. 농산물 시료 중 iprovalicarb의 분석 정량한계 및 회수율
  5. LC/MS를 이용한 잔류분의 재확인
 적 요
 REFERENCES

• 정명근(강원대학교 생약자원개발학과) | Myoung-Gun Choung (Department of Herbal Medicine Resource, Kangwon National University) Corresponding author