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基于磁铁矿纳米粒子/聚吡咯磁性固相萃取与液相色谱-串联质谱联用快速测定牛奶样品中的雌激素。

Rapid determination of estrogens in milk samples based on magnetite nanoparticles/polypyrrole magnetic solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry.

机构信息

Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan, People's Republic of China.

出版信息

J Agric Food Chem. 2011 Aug 24;59(16):8543-9. doi: 10.1021/jf201372r. Epub 2011 Jul 21.

DOI:10.1021/jf201372r
PMID:21749040
Abstract

In this study, a nanocomposite of polypyrrole-coated magnetite nanoparticles (denoted as MNPs/PPy) was prepared and employed as magnetic solid-phase extraction (MSPE) sorbent for extraction of estrogens from milk samples. Because the polypyrrole coating possessed a highly π-conjugated structure and hydrophobicity, MNPs/PPy showed excellent performance for the estrogen extraction. Estrogens could be captured directly by MNPs/PPy from milk samples without protein precipitation. Moreover, the extraction could be carried out within 3 min. Thus, a rapid, simple, and effective method for the analysis of estrogens in milk samples was established by coupling MNPs/PPy-based MSPE with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The limits of detections for estrogens investigated were in the range of 5.1-66.7 ng/L. The recoveries of estrogens (concentration range of 0.5-20 ng/mL) from milk samples were in the range of 83.4-108.5%, with relative standard deviations ranging between 4.2 and 15.4%.

摘要

在这项研究中,制备了聚吡咯包覆的磁性纳米粒子(表示为 MNPs/PPy)的纳米复合材料,并将其用作磁性固相萃取(MSPE)吸附剂,从牛奶样品中萃取雌激素。由于聚吡咯涂层具有高度的π共轭结构和疏水性,因此 MNPs/PPy 对雌激素的萃取表现出优异的性能。雌激素可以直接通过 MNPs/PPy 从牛奶样品中捕获,而无需进行蛋白质沉淀。此外,萃取可以在 3 分钟内完成。因此,通过将基于 MNPs/PPy 的 MSPE 与液相色谱-串联质谱(LC-MS/MS)相结合,建立了一种快速、简单、有效的牛奶样品中雌激素分析方法。所研究的雌激素的检测限范围为 5.1-66.7 ng/L。从牛奶样品中萃取雌激素(浓度范围为 0.5-20 ng/mL)的回收率在 83.4-108.5%之间,相对标准偏差在 4.2-15.4%之间。

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