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基于磁性纳米颗粒的分散微固相萃取——一种测定猪肉样品中雌激素的新技术。

Magnetic nanoparticles based dispersive micro-solid-phase extraction as a novel technique for the determination of estrogens in pork samples.

作者信息

Wang Juan, Chen Zhiyan, Li Zhiming, Yang Yaling

机构信息

Faculty of Life Science and Technology, Kunming University of Science and Technology, Yunnan Province 650500, China.

Technology Centre of China Tobacco Guangxi Industrial Co., Ltd, Guangxi Nanning 530001, China.

出版信息

Food Chem. 2016 Aug 1;204:135-140. doi: 10.1016/j.foodchem.2016.02.016. Epub 2016 Feb 2.

Abstract

A simple and rapid magnetic nanoparticles (MNPs) based dispersive micro-solid-phase extraction (D-μ-SPE) method coupled with HPLC-DAD has been proposed for simultaneous determination of three estrogens (17β-estradiol (E2), estrone (E1) and diethylstilbestrol (DES)) in pork samples. In this paper, the synthesis of cetyltrimethyl ammonium bromide (CTAB)-coated Fe3O4@caprylic acid NPs as an efficient sorbent for its high surface area, excellent adsorption capacity, good dispersion ability and high super-paramagnetic property was successfully applied to adsorb estrogens. Vortex was used to enhance mass transfer rate as it provided mild and effective mixing of sample solution and increased the contact between analytes and MNPs. The parameters affecting the extraction efficiency were investigated in detail. The dosages of sorbent and eluate are 100μL and 500μL, respectively. The extraction equilibrium was achieved within 2min and the MNPs can be reused. The proposed technique provided high recoveries (93.3-106.7%), good linearity (0.9993-0.9999), low LODs (0.021-0.033ngmL(-1)) and repeatability (RSD%=1.87-2.92).

摘要

本文提出了一种基于磁性纳米颗粒(MNPs)的简单快速分散微固相萃取(D-μ-SPE)方法,并结合高效液相色谱-二极管阵列检测法(HPLC-DAD),用于同时测定猪肉样品中的三种雌激素(17β-雌二醇(E2)、雌酮(E1)和己烯雌酚(DES))。本文成功合成了十六烷基三甲基溴化铵(CTAB)包覆的Fe3O4@辛酸纳米颗粒,该纳米颗粒具有高比表面积、优异的吸附能力、良好的分散能力和高超顺磁性,可作为一种高效吸附剂用于吸附雌激素。涡旋用于提高传质速率,因为它能使样品溶液温和有效地混合,并增加分析物与MNPs之间的接触。详细研究了影响萃取效率的参数。吸附剂和洗脱液的用量分别为100μL和500μL。萃取平衡在2分钟内达到,MNPs可重复使用。该方法具有较高的回收率(93.3-106.7%)、良好的线性关系(0.9993-0.9999)、较低的检出限(0.021-0.033ngmL(-1))和重复性(RSD%=1.87-2.92)。

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