Faraji Mohammad, Noorbakhsh Roya, Shafieyan Hooshang, Ramezani Mohammadkazem
Faculty of Food Industry and Agriculture, Department of Food science & Technology, Standard Research Institute (SRI), Karaj, P.O. Box 31745-139, Iran.
Faculty of Food Industry and Agriculture, Department of Food science & Technology, Standard Research Institute (SRI), Karaj, P.O. Box 31745-139, Iran.
Food Chem. 2018 Feb 1;240:634-641. doi: 10.1016/j.foodchem.2017.08.012. Epub 2017 Aug 3.
A QuEChERS based methodology was developed for the simultaneous identification and quantification of acetamiprid, imidacloprid, and spirotetramat and their relevant metabolites in pistachio by liquid chromatography-tandem mass spectrometry for the first time. First, sample extraction was done with MeCN:citrate buffer:NaHCO followed by phase separation with the addition of MgSO:NaCl. The supernatant was then cleaned by a primary-secondary amine (PSA), GCB, and MgSO. The proposed method provides a linearity in the range of 5-200µgL, and the linear regression coefficients were higher than 0.99. LOD and LOQ were obtained to be 2 and 5µgkg for the studied insecticides, respectively, with the exception of imidacloprid-olefin (5 and 10µgkg). Acceptable recoveries (91-110%) were obtained for all the analytes with good intra- and inter-precisions (0.4≥RSD ≤11.0). The method was then used for the pistachio samples collected from a field trial to estimate the maximum residue limits (MRLs) in next step.
首次开发了一种基于QuEChERS的方法，用于通过液相色谱-串联质谱法同时鉴定和定量开心果中的啶虫脒、吡虫啉、螺虫乙酯及其相关代谢物。首先，用乙腈：柠檬酸盐缓冲液：碳酸氢钠进行样品萃取，然后加入硫酸镁：氯化钠进行相分离。然后，上清液用伯仲胺（PSA）、石墨化炭黑（GCB）和硫酸镁进行净化。所提出的方法在5-200µg/L范围内具有线性，线性回归系数高于0.99。除吡虫啉-烯烃（5和10µg/kg）外，所研究杀虫剂的检出限和定量限分别为2和5µg/kg。所有分析物的回收率均在可接受范围内（91-110%），精密度良好（0.4≥相对标准偏差≤11.0）。该方法随后用于从田间试验收集的开心果样品，以估计下一步的最大残留限量（MRLs）。
