Department of Chemistry and Physics (Analytical Chemistry Area), Agrifood Campus of International Excellence ceiA3, University of Almería, E-04120 Almería, Spain; Bio-clinical Analytical Laboratory (LAB), PITA (Almería Science and Technology Park), Albert Einstein 7, E-04131 Almería, Spain.
Bio-clinical Analytical Laboratory (LAB), PITA (Almería Science and Technology Park), Albert Einstein 7, E-04131 Almería, Spain.
Food Chem. 2020 Jun 15;315:126304. doi: 10.1016/j.foodchem.2020.126304. Epub 2020 Jan 28.
A reliable 16-min analytical method for the simultaneous determination of 250 pesticides in processed fruit using ultra-performance liquid chromatography, coupled to tandem mass spectrometry (UHPLC-MS/MS), was developed and validated according to SANTE 11813/2017 guidelines and accredited successfully based on ISO 17025. Extraction was achieved using a modified QuEChERS method, without any clean-up, including a dilution to obtain good peak shapes and to reduce matrix effects. Pesticides were quantified using matrix-matched calibration, and the method was validated in terms of relative retention time window, linearity (6-167 µg kg and 0.6-16.7 µg kg, coefficient R ≥ 0.98), trueness (recovery of 70-120%), selectivity, precision (RSD ≤ 20%), limits of quantification (LOQs = 0.6-6.0 µg kg) and uncertainty. Finally, the method was applied to the routine analysis of 103 samples of processed fruits, detecting the presence of several pesticide residues, such as fluopyram, spinosad or cyprodinil (0.006-0.22 mg kg).
建立并验证了一种可靠的 16 分钟分析方法，可用于使用超高效液相色谱-串联质谱法（UHPLC-MS/MS）同时测定加工水果中的 250 种农药。该方法符合 SANTE 11813/2017 准则，并成功根据 ISO 17025 进行了认可。提取采用改良的 QuEChERS 方法，无需任何净化，包括稀释以获得良好的峰形并降低基质效应。使用基质匹配校准定量测定农药，根据相对保留时间窗口、线性度（6-167μgkg 和 0.6-16.7μgkg，相关系数 R≥0.98）、准确度（回收率为 70-120%）、选择性、精密度（RSD≤20%）、定量限（LOQs=0.6-6.0μgkg）和不确定度对方法进行验证。最后，该方法应用于 103 份加工水果的常规分析，检测到几种农药残留的存在，如氟吡菌酰胺、多杀菌素或氰霜唑（0.006-0.22mgkg）。
