Department of Chemistry and Physics, Research Centre CIAIMBITAL, University of Almería, Agrifood Campus of International Excellence, ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
Department of Chemistry and Physics, Research Centre CIAIMBITAL, University of Almería, Agrifood Campus of International Excellence, ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
Food Res Int. 2020 Jul;133:109130. doi: 10.1016/j.foodres.2020.109130. Epub 2020 Feb 27.
A wide-scope analytical method was developed and validated for the determination of tropane alkaloids (TAs) in honey samples. A simple and fast extraction procedure, using a mixture of methanol/water/formic acid (75/25/0.4, v/v/v) as extraction solvent, followed by a clean-up with graphitized black carbon (GBC) and magnesium sulphate was optimized, and compounds were analysed by liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS-Orbitrap). Validation of the proposed method provided adequate linearity (R > 0.99), trueness (recoveries 71-120%) and precision (relative standard deviation, RSD ≤ 20.1%), with limits of quantitation (LOQs) at 20 µg/kg (except anisodamine and scopolamine at 40 µg/kg) and a significant matrix effect (≤-50%). Nineteen honey samples were analysed, but only one was positive, containing 27 µg/kg of scopolamine. Additionally, a post-targeted screening was performed, and 47% of samples were contaminated with different herbicides, insecticides and veterinary drugs. Therefore, the proposed analytical method is a powerful tool for both targeted TAs and post-targeted contaminant analyses.
建立并验证了一种用于蜂蜜样品中托烷生物碱（TAs）测定的宽范围分析方法。优化了一种简单快速的提取方法，使用甲醇/水/甲酸（75/25/0.4，v/v/v）混合物作为提取溶剂，然后用石墨化黑碳（GBC）和硫酸镁进行净化，并用液相色谱-高分辨质谱（LC-HRMS-Orbitrap）进行分析。所提出方法的验证提供了充分的线性（R＞0.99）、准确度（回收率为 71-120%）和精密度（相对标准偏差，RSD≤20.1%），定量限（LOQs）为 20μg/kg（除了莨菪碱和东莨菪碱为 40μg/kg），基质效应显著（≤-50%）。分析了 19 个蜂蜜样品，但只有一个样品呈阳性，含有 27μg/kg 的东莨菪碱。此外，还进行了靶向后筛选，47%的样品受到不同除草剂、杀虫剂和兽药的污染。因此，所提出的分析方法是针对 TAs 和靶向后污染物分析的有力工具。
