HPLC-UVD를 이용한 살균제 fenpyrazamine의 시험법 개발 및 검증
Development and validation of an analytical method for fungicide fenpyrazamine determination in agricultural products by HPLC-UVD
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초록
Pyrazole계 살균제 fenpyrazamine은 복숭아 (2.0 mg/kg), 포도 (5.0 mg/kg) 및 감귤 (2.0 mg/kg)에잔류허용기준이 설정된 신규농약으로 농산물 중 fenpyrazamine 잔류량을 측정하기 위해 고성능 액체크로마토그래프를 이용한 정확하고 신뢰성 있는 효율적인 공정 시험법을 확립하고자 하였다. 추출용매는acetonitrile로 선정하였으며, 액-액 분배 단계에서 dichloromethane과 물의 분배로 극성불순물을 제거하였고, 정제단계에서는 silica cartridge를 이용하여 hexane/acetone 용매 조성으로 다양한 매트릭스 간섭 물질로부터 fenpyrazamine을 효과적으로 정제할 수 있었다. 확립된 시험법으로 7종의 대표농산물[과일류 (복숭아, 포도, 감귤), 채소류 (고추), 서류 (감자), 콩류 (대두), 곡류 (현미)]에 처리농도 0.05, 0.5, 5.0 mg/kg으로 각각 5 반복의 회수율 실험을 시행한 결과 회수율 범위가 71.8~102.7%이었고, 분석오차가 10% 미만으로 시험법의 정확성을 확인하였으며, LC-MS를 통한 재확인 과정을 수행함으로써 시험법의 신뢰성과 선택성을 확보할 수 있었다. 따라서 본 연구에서 개발한 시험법은 농산물에 잔류하는 fenpyrazamine을 분석하기 위한 공정 시험법으로 활용할 수 있을 것으로 판단된다.
Abstract
Fenpyrazamine which is a pyrazole fungicide class for controlling gray mold, sclerotinia rot, andMonilinia in grapevines, stone fruit trees, and vegetables has been registered in republic of Korea in 2013 andthe maximum residue limits of fenpyrazamine is set to grape, peach, and mandarin as 5.0, 2.0, and 2.0 mg/kg, respectively. Very reliable and sensitive analytical method for determination of fenpyrazamine residues isrequired for ensuring the food safety in agricultural products. Fenpyrazamine residues in samples were extractedwith acetonitrile, partitioned with dichloromethane, and then purified with silica-SPE cartridge and eluted withhexane and acetone mixture. The purified samples were determined by HPLC-UVD and confirmed with LCMSand quantified using external standard method. Linear range of fenpyrazamine was between 0.1~5.0 μg/mLwith the correlation coefficient (r) 0.999. The average recovery ranged from 71.8 to 102.7% at the spiked levelof 0.05, 0.5, and 5.0 mg/kg, while the relative standard deviation was between 0.1 and 7.3%. In addition, limitof detection and limit of quantitation were 0.01 and 0.05 mg/L, respectively. The results revealed that thedeveloped and validated analytical method is possible for fenpyrazamine determination in agricultural productsamples and will be used as an official analytical method.
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