Lasheras Roberto Jesús, Lázaro Regina, Burillo Juan Carlos, Bayarri Susana
Laboratorio Agroambiental, Unidad Técnica de Residuos Fitosanitarios, Gobierno de Aragón, Avenida de Montañana 1005, 50071 Zaragoza, Spain.
Instituto Agroalimentario de Aragón-IA2, Veterinary Faculty, Universidad de Zaragoza-CITA, 50013 Zaragoza, Spain.
Foods. 2021 Sep 24;10(10):2262. doi: 10.3390/foods10102262.
In the current study, the QuEChERS extraction method with slight modifications, followed by liquid and gas chromatography-tandem mass spectrometry, was applied for the determination of 399 pesticide residues in 91 raw honey samples from northeastern Spain. The quality control procedure established in Document No. SANTE/12682/2019 was successfully followed: the responses in reagent blank and blank honey samples were below 30% of the reporting limit (0.01 mg kg) for all analysed compounds, the correlation coefficients (R) were higher than 0.99 in most calibration curves, the deviation of back-calculated concentration from the true concentration was below ±20% (using the standard of 50 μg L concentration), and the recoveries of spiked samples on matrix were within the range of 70-120% for almost all analytes. Only chlorfenvinphos (2-7.8 ng/g) and coumaphos (8.8-37 ng/g) were detected in 13 samples, and neither were observed to exceed their maximum residue limits (MRLs). Dietary risk assessment for pesticide residues in honey above their lowest calibrated level (LCL) was performed, and two different age groups, adults and infants, were considered as populations at risk. The contribution of honey lay far below the acceptable daily intake (ADI) for both pesticide residues. Therefore, according to our results, honey is unlikely to pose concerns for consumer health in terms of its contribution to dietary long-term exposure. However, to maintain the level of compliance, pesticide residues in honey should be continuously monitored.
在本研究中,采用经轻微改良的QuEChERS提取方法,随后结合液相色谱 - 串联质谱法和气相色谱 - 串联质谱法,对来自西班牙东北部的91份生蜂蜜样品中的399种农药残留进行测定。成功遵循了文件编号为SANTE/12682/2019中规定的质量控制程序:所有分析化合物在试剂空白和空白蜂蜜样品中的响应均低于报告限(0.01 mg/kg)的30%,大多数校准曲线的相关系数(R)高于0.99,反算浓度与真实浓度的偏差低于±20%(使用50 μg/L浓度的标准品),并且几乎所有分析物在基质加标样品中的回收率在70 - 120%范围内。仅在13个样品中检测到了毒虫畏(2 - 7.8 ng/g)和蝇毒磷(8.8 - 37 ng/g),且均未超过其最大残留限量(MRLs)。对蜂蜜中高于其最低校准水平(LCL)的农药残留进行了膳食风险评估,并将两个不同年龄组,即成年人和婴儿,视为有风险的人群。两种农药残留的蜂蜜摄入量贡献均远低于可接受每日摄入量(ADI)。因此,根据我们的结果,就其对膳食长期暴露的贡献而言,蜂蜜不太可能对消费者健康构成担忧。然而,为保持合规水平,应持续监测蜂蜜中的农药残留。