Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
Toxins (Basel). 2023 Feb 15;15(2):160. doi: 10.3390/toxins15020160.
Dispersive magnetic solid-phase extraction (DMSPE) technique is proposed as a new sensitive and effective sample treatment method for the determination of aflatoxins in paprika samples. DMSPE was followed by ultrahigh-performance liquid chromatography and high-resolution mass spectrometry detection (UHPLC-HRMS) using a non-targeted acquisition mode for the detection of main aflatoxins (aflatoxin G1, G2, B1 and B2) and derivatives. DMSPE was based on the use of magnetic nanocomposite coated with polypyrrole (PPy) polymer and the main experimental parameters influencing the extraction efficiency in adsorption and desorption steps have been studied and optimized. Analyses were performed using 250 µL magnetic PPy nanocomposite into the sample solution, adsorbing the analytes in 30 min and desorbing them with ethyl acetate (2 mL) in 15 min. The method has been validated, obtaining quantification limits between 3.5 and 4.7 µg kg and recoveries between 89.5-97.7%. The high recovery rate, wide detection range and the use for the first time of the reusable FeO@PPy nanomaterial in suspension for solid food matrices, guarantee the usefulness of the method developed for adequate control of aflatoxins levels in paprika. The proposed methodology was applied for the analysis of 31 samples (conventional and organic) revealing the absence of aflatoxins in the samples.
分散固相萃取（DMSPE）技术被提议作为一种新的灵敏有效的样品处理方法，用于测定辣椒粉中的黄曲霉毒素。DMSPE 后接超高效液相色谱和高分辨率质谱检测（UHPLC-HRMS），采用非靶向采集模式检测主要黄曲霉毒素（黄曲霉毒素 G1、G2、B1 和 B2）及其衍生物。DMSPE 基于使用涂有聚吡咯（PPy）聚合物的磁性纳米复合材料，研究并优化了影响吸附和解吸步骤中萃取效率的主要实验参数。分析使用 250 µL 磁性 PPy 纳米复合材料进入样品溶液，在 30 分钟内吸附分析物，并用乙酸乙酯（2 mL）在 15 分钟内洗脱。该方法已得到验证，定量限在 3.5 和 4.7 µg kg 之间，回收率在 89.5-97.7%之间。高回收率、宽检测范围以及首次将可重复使用的 FeO@PPy 纳米材料用于悬浮液中的固体食品基质，保证了所开发方法用于充分控制辣椒粉中黄曲霉毒素水平的有用性。所提出的方法已应用于 31 个样品（常规和有机）的分析，结果显示样品中不存在黄曲霉毒素。
