Cho Sung-Min, Lee Han-Sol, Park Ji-Su, Lee Su-Jung, Shin Hye-Sun, Chung Yun-Mi, Choi Ha-Na, Jung Yong-Hyun, Oh Jae-Ho, Yun Sang-Soon
Food Safety Evaluation Department, Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju 28159, Korea.
Department of Integrated Biomedical and Life Science, Graduate School, Korea University, Seoul 02841, Korea.
Foods. 2021 Sep 3;10(9):2090. doi: 10.3390/foods10092090.
A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient ( = 0.9992-0.9998) in the 0.003-0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7-104.3% range. The relative standard deviations were ≤9.8% for intra- ( = 5) and inter-day ( = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).
利用改良的QuEChERS方法，开发了一种快速简便的分析方法，用于检测三氟苯嘧啶（triflumezopyrim），这是一种新型的中离子型杀虫剂，也是杜邦公司的商业化产品。通过调节pH值提高乙腈溶剂的萃取效率，并采用分散固相萃取进行净化处理。选用五种食品商品对当前优化方法进行验证，该方法在0.003 - 0.30 mg/kg校准范围内显示出良好的线性，相关系数优异（ = 0.9992 - 0.9998）。方法的检测限（LOD）和定量限（LOQ）分别确定为0.003和0.01 mg/kg。三氟苯嘧啶的平均回收率在89.7 - 104.3%范围内。在五个代表性样品中，浓度为0.01、0.1和0.5 mg/kg时，日内（ = 五）和日间（ = 十五）精密度的相对标准偏差均≤9.8%。计算了基质效应以确认在超高效液相色谱 - 串联质谱（UPLC-MS/MS）中分析物离子化过程中的影响。仪器分析的基质效应表明，三氟苯嘧啶对基质的敏感性较低。本研究中提出的分析方法有效地提高了农产品中三氟苯嘧啶测定的准确性、选择性和灵敏度；因此，它可作为建立最大残留限量（MRLs）的参考方法。
