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分子印迹聚合物结合膜保护固相萃取检测茶叶样品中的三嗪类农药。

Molecularly imprinted polymers combined with membrane-protected solid-phase extraction to detect triazines in tea samples.

机构信息

College of Chemistry, Jilin University, Changchun, Jilin, 130012, China.

State Key Laboratory of Urban Water Resource and Environment, Harbin Institute of Technology, 202 Haihe Road, Nangang District, Harbin, 150090, Heilongjiang, China.

出版信息

Anal Bioanal Chem. 2018 Aug;410(21):5173-5181. doi: 10.1007/s00216-018-1171-y. Epub 2018 Jun 25.

Abstract

Spherical molecularly imprinted polymers (MIPs) were prepared by emulsion polymerization. The isothermal adsorption and selective adsorption indicated that the MIPs obtained exhibit excellent specific recognition for the template (atrazine) and its analogues. The MIPs were encapsulated in a polypropylene microporous membrane to fabricate MIP adsorption packages for the direct extraction of triazines in uncentrifuged and unfiltered tea extracts. The extraction conditions affecting the extraction efficiency, including the type and volume of extraction solvent, the number of MIP adsorption packages, the surface area of the MIP adsorption packages, the mass of MIPs in the MIP adsorption packages, the extraction time, the eluting solvent, and the eluting volume, were optimized. Under the optimal extraction and high-performance liquid chromatography-tandem mass spectrometry conditions, the method exhibited excellent linearity in the range from 0.5 to 250 ng g, with R ≥ 0.9992. The detection limit of the method was 0.09-0.18 ng g. The intraday and interday relative standard deviations ranged from 3.1% to 7.5% and from 3.1% to 7.9%, respectively. The method was successfully used to detect triazines in five tea samples. At a spiking concentration of 2 ng g, satisfactory recoveries ranging from (81 ± 3)% to (104 ± 7)% were obtained. The membrane-protected solid-phase extraction method based on molecularly imprinted material is expected to be widely used to enrich triazines in complex samples. Graphical Abstract Schematic illustration of the MIPs combined with membrane-protected solid-phase extraction of triazines in tea sample.

摘要

球形分子印迹聚合物(MIPs)通过乳液聚合制备。等温吸附和选择性吸附表明,所得到的 MIPs 对模板(莠去津)及其类似物表现出优异的特异性识别。将 MIPs 封装在聚丙烯微孔膜中,制备 MIP 吸附包,用于直接提取未离心和未过滤的茶提取物中的三嗪。优化了影响萃取效率的萃取条件,包括萃取溶剂的类型和体积、MIP 吸附包的数量、MIP 吸附包的表面积、MIP 吸附包中 MIP 的质量、萃取时间、洗脱溶剂和洗脱体积。在最佳萃取和高效液相色谱-串联质谱条件下,该方法在 0.5 至 250ng g 的范围内表现出优异的线性,R ≥ 0.9992。该方法的检测限为 0.09-0.18ng g。日内和日间相对标准偏差分别为 3.1%-7.5%和 3.1%-7.9%。该方法成功用于检测五种茶样中的三嗪。在 2ng g 的加标浓度下,获得了 81±3%至 104±7%的令人满意的回收率。基于分子印迹材料的膜保护固相萃取方法有望广泛用于富集复杂样品中的三嗪。

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