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基于固相萃取与 ICP-MS 联用的羧基功能化中空聚合物微球检测复杂食品基质中痕量金属元素

Carboxyl-functionalized hollow polymer microspheres for detection of trace metal elements in complex food matrixes by ICP-MS assisted with solid-phase extraction.

机构信息

State Key Laboratory of Food Nutrition and Safety, Tianjin University of Science and Technology, Tianjin 300457, China.

College of Food Science and Bioengineering, Tianjin Agricultural University, Tianjin 300384, China.

出版信息

Ecotoxicol Environ Saf. 2021 Jan 15;208:111729. doi: 10.1016/j.ecoenv.2020.111729. Epub 2020 Dec 8.

Abstract

In this work, carboxyl-functionalized hollow polymer microspheres (CHPMs) was successfully fabricated using poly (styrene-itaconic anhydride) particles as the core template and itaconic anhydride and trans-anethole cross-linked with divinylbenzene as the shell. The desirable microspheres and hollow structure of CHPMs were demonstrated by scanning and transmission electron microscopies, respectively. The characterized CHPMs as an adsorbent was packed into a solid phase extraction column to simultaneously detect the V(V), Cr(III), Cu(II), Cd(II), and Pb(II) in digested food samples by inductively coupled plasma-mass spectrometry (ICP-MS). A series of experimental parameters of solid-phase extraction (SPE) were investigated through vast experiments to improve sensitivity of the proposed method in metal ions detection. The detection limits of the method reached 0.8-3.2 ng L for the target elements, and the relative standard deviations (RSDs) ranging from 1.2% to 3.5% were obtained from eleven parallel experiments using a 1.0 μg L sample solution. The stability allowed the material to withstand more than 15 cycling while the recoveries remained above 88%. In food samples, the detection limits were at 0.20-0.80 μg kg, and satisfactory recoveries of 85-104% were obtained in spike tests of laver, fish as well as chicken.

摘要

在这项工作中,成功地使用聚(苯乙烯-马来酸酐)颗粒作为核模板,马来酸酐和反式茴香脑与二乙烯基苯交联作为壳,制备了羧基功能化的空心聚合物微球(CHPMs)。扫描和透射电子显微镜分别证明了所需的微球和 CHPMs 的空心结构。将表征的 CHPMs 作为吸附剂填充到固相萃取柱中,通过电感耦合等离子体质谱法(ICP-MS)同时检测消解食品样品中的 V(V)、Cr(III)、Cu(II)、Cd(II)和 Pb(II)。通过大量实验研究了固相萃取(SPE)的一系列实验参数,以提高该方法在金属离子检测中的灵敏度。该方法对目标元素的检测限达到 0.8-3.2ngL,使用 1.0μg L 样品溶液进行 11 次平行实验,得到的相对标准偏差(RSD)范围为 1.2%-3.5%。该材料的稳定性允许其承受超过 15 次循环,回收率仍保持在 88%以上。在食品样品中,检测限为 0.20-0.80μgkg,在紫菜、鱼和鸡肉的加标测试中,回收率为 85-104%。

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