I.U. CINQUIMA, Analytical Chemistry Group (TESEA), Faculty of Sciences, University of Valladolid, 47001 Valladolid, Spain.
I.U. CINQUIMA, Analytical Chemistry Group (TESEA), Faculty of Sciences, University of Valladolid, 47001 Valladolid, Spain.
Food Res Int. 2024 Nov;195:114955. doi: 10.1016/j.foodres.2024.114955. Epub 2024 Aug 22.
A new analytical method was developed and validated to determine fourteen bisphenols (A, B, C, E, F, M, P, S, Z, AF, AP, BP, FL, PH) in bee pollen using ultra-high-performance liquid chromatography-tandem mass spectrometry. Two different sample treatments were proposed and evaluated: one based on the QuEChERS (quick, easy, cheap, effective, rugged & safe) approach and the other utilizing microextraction with a supramolecular solvent (SUPRAS). In both cases, average analyte recovery ranged between 71 % and 114 %, and the matrix effect was between -45 % and +5 %, although it was not significant when using the QuEChERS-based method (<±20 %). The environmental impact of both sample treatments was assessed using different analytical metrics, with both procedures classified as environmentally friendly, though slightly better results were obtained for SUPRAS. The method was fully validated, showing that the QuEChERS approach had better overall performance, particularly regarding sensitivity and matrix effect. Consequently, the QuEChERS methodology was applied to determine bisphenols in thirty bee pollen samples from different Spanish regions. Residues of three bisphenols (M, P, and S) were detected, although only bisphenol S was quantified in several samples at low concentration levels (<7 μg kg), which is below the established specific migration limit (SML; 50 μg kg). However, regarding human health, the estimated daily intake, target hazard quotient, and hazard index assessed were higher than acceptable limits, suggesting a potential risk for human consumers.
建立并验证了一种新的分析方法,用于测定花粉中的 14 种双酚(A、B、C、E、F、M、P、S、Z、AF、AP、BP、FL、PH),采用超高效液相色谱-串联质谱法。提出并评估了两种不同的样品处理方法:一种基于 QuEChERS(快速、简单、廉价、有效、耐用和安全)方法,另一种利用超分子溶剂(SUPRAS)进行微萃取。在这两种情况下,平均分析物回收率在 71%至 114%之间,基质效应在-45%至+5%之间,尽管使用基于 QuEChERS 的方法时基质效应不显著(<±20%)。使用不同的分析指标评估了两种样品处理方法的环境影响,两种方法均被归类为环保方法,尽管 SUPRAS 方法的结果略好。该方法经过全面验证,表明 QuEChERS 方法具有更好的整体性能,特别是在灵敏度和基质效应方面。因此,该方法应用于测定来自西班牙不同地区的 30 个花粉样本中的双酚。检测到三种双酚(M、P 和 S)的残留,但仅在几个样本中以低浓度(<7μgkg)定量检测到双酚 S,低于规定的特定迁移限量(SML;50μgkg)。然而,就人类健康而言,评估的每日摄入量、目标危害系数和危害指数都高于可接受的限制,这表明对人类消费者存在潜在风险。