I. U. CINQUIMA, Analytical Chemistry Group, Faculty of Sciences, University of Valladolid, Paseo de Belén 5, 47011 Valladolid, Spain.
I. U. CINQUIMA, Analytical Chemistry Group, Faculty of Sciences, University of Valladolid, Paseo de Belén 5, 47011 Valladolid, Spain.
Food Res Int. 2020 Apr;130:108904. doi: 10.1016/j.foodres.2019.108904. Epub 2019 Dec 17.
The objective of this study was to propose a novel method to determine residues of the bio-insecticide spinetoram, which is a mixture of two components (spinetoram J and L), in honey from multifloral, rosemary and heather botanical origins; liquid chromatography coupled to quadrupole time-of-flight mass spectrometry was the technique employed. An efficient sample treatment (recoveries between 82% and 95%) involving a solid-phase extraction with a polymeric sorbent has been recommended, and no matrix effect was observed. Chromatographic analysis (4 min) was performed in reverse phase mode by using a fused-core column (Kinetex® EVO C) with acetonitrile and ammonium formate as the mobile phase components, which was applied in isocratic elution mode. Method was validated according to the current European legislation. Not only was it selective, but it also displayed a wide linear range, good precision (relative standard deviation values lower than 9%) and sensitivity (low limits of detection (spinetoram J, 0.1-0.3 μg/kg; spinetoram L, 0.1-0.2 μg/kg) and quantification (spinetoram J, 0.3-1.2 μg/kg; spinetoram L, 0.4-0.7 μg/kg)). Several honey samples were analyzed with this method and no spinetoram residues were found above the limits of detection.
本研究旨在提出一种新方法，用于测定来自多种花卉、迷迭香和石南植物源蜂蜜中生物杀虫剂螺虫乙酯（由两种成分[螺虫乙酯 J 和 L]组成）的残留量；采用的技术是液相色谱-四极杆飞行时间质谱联用。推荐使用一种高效的样品处理方法（回收率在 82%至 95%之间），涉及一种带有聚合物吸附剂的固相萃取，且未观察到基质效应。采用反相模式，通过使用核壳柱（Kinetex® EVO C）进行色谱分析（4 分钟），流动相组分为乙腈和甲酸铵，采用等度洗脱模式。方法按照现行的欧洲法规进行了验证。该方法不仅具有选择性，而且还具有较宽的线性范围、良好的精密度（相对标准偏差值低于 9%）和灵敏度（低检测限（螺虫乙酯 J，0.1-0.3μg/kg；螺虫乙酯 L，0.1-0.2μg/kg）和定量限（螺虫乙酯 J，0.3-1.2μg/kg；螺虫乙酯 L，0.4-0.7μg/kg））。用该方法分析了几种蜂蜜样品，均未发现检测限以上的螺虫乙酯残留。
