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Comprehensive tropane alkaloids analysis and retrospective screening of contaminants in honey samples using liquid chromatography-high resolution mass spectrometry (Orbitrap).
Food Research International ( IF 7.0 ) Pub Date : 2020-02-27 , DOI: 10.1016/j.foodres.2020.109130
Ana Romera-Torres 1 , Roberto Romero-González 1 , José Luis Martínez Vidal 1 , Antonia Garrido Frenich 1
Affiliation  

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 (75/25/0.1, 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 (R2>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 analysis.



中文翻译:

使用液相色谱-高分辨率质谱法(Orbitrap)进行全面的托烷生物碱分析并回顾性筛选蜂蜜样品中的污染物。

开发了一种广谱分析方法,并已用于测定蜂蜜样品中的托烷生物碱(TAs)。使用甲醇/水/甲酸(75/25 / 0.1,v / v / v)的混合物作为萃取溶剂的简单且快速的萃取程序,然后用石墨化黑碳(GBC)和硫酸镁进行净化对化合物进行了优化,并通过液相色谱与高分辨率质谱法(LC-HRMS-Orbitrap)进行了分析。所提出方法的验证提供了足够的线性度(R 2> 0.99),真实度(回收率71-120%)和精密度(相对标准偏差,RSD≤20.1%),定量限(LOQ)为20 µg / kg(山iso碱和东pol碱除外,均为40 µg / kg),并且显着的基质效应(≤-50%)。分析了19个蜂蜜样品,但只有一个阳性,含量为27 µg / kg东pol碱。此外,进行了靶向后筛选,并且47%的样品被不同的除草剂,杀虫剂和兽药污染。因此,所提出的分析方法是针对目标TA和目标后污染物分析的强大工具。

更新日期:2020-02-27
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