Lee Jonghwa, Kim Jeong-Han
Department of Agricultural Biotechnology and Research Institute of Agriculture and Life Sciences, Seoul National University, Seoul 08826, Korea.
Molecules. 2020 Apr 22;25(8):1938. doi: 10.3390/molecules25081938.
A simultaneous analytical method for the organophosphorus insecticide fenthion and its five metabolites (fenthion oxon, fenthion oxon sulfoxide, fenthion oxon sulfone, fenthion sulfoxide, and fenthion sulfone) was developed based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Five matrices (brown rice, chili pepper, orange, potato, and soybean) were selected to validate the method. The target compounds were analyzed using positive electrospray ionization in the multiple reaction monitoring mode. For the best sensitivity in regard to the detector response, water and methanol containing formic acid (0.1%) were selected as the mobile phase. The optimum extraction efficiency was obtained through a citrate-buffered QuEChERS (quick, easy, cheap, effective, rugged, and safe) method. Recovery tests were carried out at three spiking levels ( 3). At all fortification levels, the accuracy and precision results were between 70% and 120% with a relative standard deviation of ≤15%. The limit of quantitation was 0.01 mg/kg, and the correlation coefficients () of the matrix-matched calibration curves were >0.99. Significant signal suppression in the detector responses were observed for all matrices, suggesting that a compensation method, such as matrix-matched calibration, is required to provide accurate quantitative results. The applicability of the presented method was confirmed for the simultaneous analysis of fenthion and its metabolites in various crops.
基于超高效液相色谱-串联质谱法（UHPLC-MS/MS）开发了一种同时分析有机磷杀虫剂倍硫磷及其五种代谢物（倍硫磷氧、倍硫磷氧亚砜、倍硫磷氧砜、倍硫磷亚砜和倍硫磷砜）的方法。选择了五种基质（糙米、辣椒、橙子、土豆和大豆）来验证该方法。在多反应监测模式下使用正电喷雾电离对目标化合物进行分析。为了使检测器响应具有最佳灵敏度，选择含有甲酸（0.1%）的水和甲醇作为流动相。通过柠檬酸缓冲的QuEChERS（快速、简便、廉价、有效、耐用且安全）方法获得了最佳提取效率。在三个加标水平（3）下进行了回收率测试。在所有强化水平下，准确度和精密度结果在70%至120%之间，相对标准偏差≤15%。定量限为0.01 mg/kg，基质匹配校准曲线的相关系数（）>0.99。在所有基质中均观察到检测器响应中的显著信号抑制，这表明需要一种补偿方法，如基质匹配校准，以提供准确定量结果。所提出方法的适用性在同时分析各种作物中的倍硫磷及其代谢物方面得到了证实。
