Abstract:
A screening and semi-quantitative method was developed for the analysis of 694 various contaminants in honey, jam, jelly and syrup samples by ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry. Sample preparation, which was optimised using split factorial design, was based on acetate-buffered version of QuEChERS, followed by a clean-up step and a concentration step to enhance sensitivity of analytes. The method was validated according to SANTE/11312/2021 guidelines. The screening detection and limits of identification were established as being less than or equal to 0.05 mg.kg-1 for 89% and 74% of the contaminants, respectively. The validated screening method was applied to 50 concentrated sugary products. Overall, 46% of the samples were positive to pesticide residues. Most of the positive samples (78%) contained mixtures of pesticide residues. Three time-and-cost saving convenient strategies suitable for high-throughput analysis were proposed for the targeted semi-quantification of the previously contaminants identified in samples.
摘要:
开发了一种筛选和半定量方法,用于分析蜂蜜中的694种污染物,果酱,通过超高效液相色谱和四极杆飞行时间质谱分析的果冻和糖浆样品。样品制备,使用分裂阶乘设计进行了优化,基于醋酸盐缓冲版本的QuEChERS,随后是净化步骤和浓缩步骤以增强分析物的灵敏度。该方法根据SANTE/11312/2021指南进行了验证。筛选检测和鉴定限确定为小于或等于0.05mg。89%和74%的污染物为kg-1,分别。将经过验证的筛选方法应用于50种浓缩含糖产品。总的来说,46%的样品对农药残留呈阳性。大多数阳性样品(78%)含有农药残留的混合物。提出了三种适用于高通量分析的节省时间和成本的便捷策略,用于对样品中先前鉴定的污染物进行针对性的半定量。