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구두발표(OC)-농업화학 및 생태,식품분야 : LC-MS/MS를 이용한 녹차 중 디노테퓨란과 대사체 분석
무쉬픽 ( Musfiqur Rahman ),최정희 ( Jeong Heui Choi ),김성우 ( Sung Woo Kim ),임소정 ( So Jeong Im ),정다이 ( Da I Jung ),압두 ( Abd El Aty ),심재한 ( Jae Han Shim ) 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
A simultaneous analytical method was developed for dinotefuran and its metabolites (MNG, UF, and DN) in green tea using tandem mass spectrometry (LC/MS/MS). Matrix enhancement and suppression effect was observed for all of the analytes where recoveries were varied with these effects. Samples were extracted with QuEChERS extraction solvent acidic acetonitrile (ACN),partitioned with magnesium sulfate (MgSO4) and sodium acetate (NaOAc) and purified with dispersive solid phase extraction procedure (dSPE) using primary secondary amine (PSA) and C18 sorbent. We tried to increase the extraction efficiency by changing solvents and MeOH was found to be the best solvent for extraction of dinotefuran and its polar metabolites but due to having limitation to apply MeOH as a QuEChERS solvent for lacking of appropriate partitioning salt, ACN was selected as an extraction solvent. Recovery of DN was found < 70% when compared with matrix matched calibration, whereas it was within the range (70-120%) when compared with solvent calibration for matrix enhancement effect. The opposite situation was observed for MNG and dinotefuran due to matrix suppression effect. The recoveries of UF were consistent in spite of having little suppression effect. Calibration curves were linear over the calibration ranges for all the analytes with R2 ≥ 0.994. Limits of detection ranged from 0.0012 - 0.015 mg kg.1, whereas the limits of quantitation were 0.004 - 0.05 mg kg.1 for dinotefuran and its metabolites. The method was successfully applied to real samples, where dinotefuran and all metabolite residues were found in the field-incurred green tea samples.