[关键词]
[摘要]
建立了超高效液相色谱质谱联用仪(UPLC-MS/MS)测定植物源性食品中百可得残留量的快速分析方法。利用QTRAP独有的增强分辨率扫描(ER)模式,解决了带多电荷的化合物找母离子的困难。考察了前处理、耗材选择及基质效应对回收率的影响,选择20%(V/V)甲醇水溶液[含1%(V/V)甲酸]提取,同时添加0.5 g盐酸胍、使用聚丙烯材质的实验耗材减少植物成分及实验耗材对目标物的吸附。经Kinetex F5色谱柱分离,在正离子、多反应监测模式下,进行定量分析。结果表明,百可得在0.1~100.0 μg/L范围内线性关系良好,相关系数高于0.998;分别以柑、芦笋等9种植物源性食品为样品基质,在3个不同添加水平下,百可得的平均回收率为75.2%~103.5%,相对标准偏差(RSD,n=6)为2.1%~14.3%;方法检出限为0.6 μg/kg,定量限2.0 μg/kg。该方法可用于植物源性食品中百可得残留量快速提取、定性与定量检测,具有操作简单、灵敏度高、成本低等优势,适合于大批量植物源性食品中百可得残留量的日常筛查与确证。
[Key word]
[Abstract]
A rapid analysis method for the determination of Bellkute residues in foods of plant origin by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The unique enhanced resolution scan (ER) mode of QTRAP was used to solve the difficulty of finding the parent (precursor) ions for multi-charged compounds. The effects of pretreatment, consumable selection, and matrix effects on the recovery rate were investigated, and 20% (V/V) methanol aqueous solution [containing 1% (V/V) formic acid] was selected for extraction. Guanidine hydrochloride (0.5 g) was added and polypropylene was used as the experimental material, to reduce the adsorption of the target by plant components and experimental consumables. The Kinetex F5 column was used for separation, and the quantitative analysis was performed in the positive ion and multiple reaction monitoring mode. The results showed that Bellkute had a good linear relationship in the range of 0.1~100.0 μg/L, and the correlation coefficient r was not lower than 0.998. Using nine plantderived foods such as citrus and asparagus and three spiking levels, the average recovery rate of Bellkute was determined to range from 75.2% to 103.5%, with the relative standard deviations (RSD, n=6) being 2.1%~14.3%, and the limit of detection (LOD) and limit of quantification (LOQ) being 0.6 μg/kg and 2.0 μg/kg, respectively. This method can be used for rapid extraction, and qualitative and quantitative detection of Bellkute residues in foods of plant origin, with advantages of simple operation, high sensitivity, and low cost, thereby being suitable for daily screening and confirmation of Bellkute residues in large quantities of foods of plant origin.
[中图分类号]
[基金项目]
广西重点研发计划项目(桂科AB24010126);广西壮族自治区市场监督管理局科技计划项目(GXSJKJ2024-1)