Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-02-01 , DOI: 10.1007/s00216-018-0882-4 Bárbara Socas-Rodríguez , Javier Hernández-Borges , Antonio V. Herrera-Herrera , Miguel Ángel Rodríguez-Delgado
In this work, the suitability of Fe3O4 nanoparticles coated with polydopamine was evaluated as sorbent for the extraction of a group of 21 compounds with oestrogenic activity including seven phytoestrogens, six mycotoxins as well as four synthetic and four natural oestrogens from different types of milk, including sheep milk, in which the evaluation of oestrogenic compounds have never been developed before. Extraction was carried out using magnetic micro-dispersive solid-phase extraction after a previous deproteinisation step. Separation, determination and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole-tandem mass spectrometry. The methodology was validated for five milk samples using 17β-estradiol-2,4,16,16,17-d5 as internal standard for natural and synthetic oestrogens, β-zearalanol-10,10,11,12,12-d5 for mycotoxins and prunetin for phytoestrogens. Recovery values ranged from 70 to 120% for the five types of matrices with relative standard deviation values lower than 18%. Limits of quantification of the method were in the range 0.55–11.8 μg L−1 for all samples.
中文翻译:
核壳聚多巴胺包覆的磁性纳米粒子作为微分散固相萃取后超高效液相色谱串联质谱的萃取吸附剂,对牛,山羊,绵羊和人乳中的雌激素化合物进行多残留分析
在这项工作中,Fe 3 O 4的适用性评价用多多巴胺包被的纳米颗粒作为吸附剂可从一组不同类型的牛奶(包括羊奶)中提取一组具有雌激素活性的21种化合物,其中包括7种植物雌激素,6种霉菌毒素以及4种合成雌激素和4种天然雌激素。雌激素化合物从未开发过。在先前的脱蛋白步骤之后,使用磁性微分散固相萃取进行萃取。目标分析物的分离,测定和定量是通过超高效液相色谱与三重四极杆串联质谱联用实现的。使用17β-雌二醇-2、4、16、16、17-d 5对五个牛奶样品进行了方法学验证作为天然和合成雌激素的内标,霉菌毒素为β-泽拉洛尔10,10,11,12,12-d -d 5,植物雌激素为普鲁内汀。相对标准偏差值低于18%的五种基质的回收率范围为70%至120%。对于所有样品,该方法的定量限在0.55-11.8μgL -1范围内。