Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD
HPLC-UVD를 이용한 농산물 중 pyrifluquinazon 잔류시험법 개발 및 검증

Jung-Ah Do, Ji-Eun Kwon, Mi-Ra Kim, Eun-Mi Lee, Ju-Hee Kuk, Yoon-Jae Cho, Moon-Ik Chang, Kisung Kwon, Jae-Ho Oh
2013 Analytical Science and Technology  
Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with
more » ... onitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis. (RSD R (%)) > 0.01 mg/kg, ≤0.1 mg/kg 범위에서 3.40~15.4%로 코덱스 가이드라인 기준에 적합함을 확인 하였다. 또한 본 시험법의 재현성 및 선택성을 추가로 확보할 수 있도록 LC-MS를 통한 정성시험법을 추 가로 확립하였다. 본 시험법은 신규 등록된 pyrifluquinazon 분석을 위한 신속 정확한 공정 시험법으로 식 품공전에 등재되어 활용되고 있다.
doi:10.5806/ast.2013.26.3.174 fatcat:pkpzbu7bizc4jl3bxd5y634ygm