LC-MS/MS를 이용한 농산물 중 Dichlobentiazox 시험법 개발 및 검증 |
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분야 | 환경화학 |
저자목록 |
구선영1, 이한솔2, 박지수3, 이수정4, 신혜선5, 강성은6, 정윤미7, 최하나8, 윤상순9 *, 정용현10, 윤혜정11 |
논문게재정보 | 108p ~ 117p |
초록 | An analytical method was developed for the determination of dichlobentiazox in agricultural products using the QuEChERS (quick, easy, cheap, effective, rugged and safe) method and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile followed by magnesium sulfate anhydrous, sodium chloride, disodium hydrogencitrate sesquihydrate, and trisodium citrate dihydrate. After centrifugation, supernatant layer was cleaned up using dispersive solid phase extraction (d-SPE) such as MgSO4 (anhydrous magnesium sulfate) and C18 (octadecyl). The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using seven levels, from 0.0025 to 0.25 mg/L, and the coefficient of determination was above 0.99. The average recoveries at three different concentrations levels (LOQ, 10LOQ, and 50LOQ, n=5) were from 79.8 to 100.7% with relative standard deviation (RSD) of less than 3.5%. For inter-laboratory validation, the average recoveries were from 78.2% to 98.5% with coefficient of variation (CV) was less than 11.6%. All results were satisfied with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). This study was accurate, effective and sensitive for dichlobentiazox determination in agricultural commodities and could be useful for safety management of dichlobentiazox residues in agricultural products. |
논문파일 | |
키워드 | Pesticide residue, Dichlobentiazox, Analytical method, Agricultural product, LC-MS/MS |