Capriotti Anna Laura, Cavaliere Chiara, Foglia Patrizia, La Barbera Giorgia, Samperi Roberto, Ventura Salvatore, Laganà Aldo
Department of Chemistry, University of Rome "La Sapienza", Rome, Italy.
J Sep Sci. 2016 Dec;39(24):4794-4804. doi: 10.1002/jssc.201600879. Epub 2016 Nov 21.
Recently, magnetic solid-phase extraction has gained interest because it presents various operational advantages over classical solid-phase extraction. Furthermore, magnetic nanoparticles are easy to prepare, and various materials can be used in their synthesis. In the literature, there are only few studies on the determination of mycoestrogens in milk, although their carryover in milk has occurred. In this work, we wanted to develop the first (to the best of our knowledge) magnetic solid-phase extraction protocol for six mycoestrogens from milk, followed by liquid chromatography and tandem mass spectrometry analysis. Magnetic graphitized carbon black was chosen as the adsorbent, as this carbonaceous material, which is very different from the most diffuse graphene and carbon nanotubes, had already shown selectivity towards estrogenic compounds in milk. The graphitized carbon black was decorated with Fe O , which was confirmed by the characterization analyses. A milk deproteinization step was avoided, using only a suitable dilution in phosphate buffer as sample pretreatment. The overall process efficiency ranged between 52 and 102%, whereas the matrix effect considered as signal suppression was below 33% for all the analytes even at the lowest spiking level. The obtained method limits of quantification were below those of other published methods that employ classical solid-phase extraction protocols.
近年来，磁性固相萃取因其相较于传统固相萃取具有多种操作优势而受到关注。此外，磁性纳米颗粒易于制备，且在其合成过程中可使用多种材料。尽管牛奶中已出现霉菌雌激素残留，但文献中关于牛奶中霉菌雌激素测定的研究却很少。在本研究中，我们希望开发出首个（据我们所知）用于从牛奶中萃取六种霉菌雌激素的磁性固相萃取方法，随后进行液相色谱和串联质谱分析。我们选择磁性石墨化炭黑作为吸附剂，因为这种碳质材料与最常见的石墨烯和碳纳米管有很大不同，已显示出对牛奶中雌激素化合物的选择性。通过表征分析证实，石墨化炭黑已用Fe₃O₄修饰。仅使用在磷酸盐缓冲液中进行适当稀释作为样品预处理，避免了牛奶脱蛋白步骤。整个过程的效率在52%至102%之间，而即使在最低加标水平下，所有分析物的基质效应（视为信号抑制）均低于33%。所获得的方法定量限低于其他采用传统固相萃取方法的已发表方法。
