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制备双官能单体分子印迹聚合物填充固相萃取用于提高牛奶中磺胺类药物定量分析的灵敏度。

Preparation of bifunctional monomer molecularly imprinted polymer filled solid-phase extraction for sensitivity improvement of quantitative analysis of sulfonamide in milk.

机构信息

Guangdong Provincial Key Laboratory of Food Quality and Safety/Guangdong Laboratory of Lingnan Modern Agriculture, South China Agricultural University, Guangzhou, 510642, China.

Zhongshan agricultural product quality and Safety Inspection Institute, Zhongshan, 528403, China.

出版信息

J Chromatogr A. 2023 Jul 5;1700:464046. doi: 10.1016/j.chroma.2023.464046. Epub 2023 May 4.

DOI:10.1016/j.chroma.2023.464046
PMID:37167804
Abstract

To solve the problems of unstable adsorption performance and high organic solvent consumption of traditional molecular imprinting materials, we developed a water-resistant and highly adsorptive molecularly imprinted sulfamethazine polymer (MIP) through a novel synthetic strategy consisting of the application of mixed functional monomers combined with hydrophobic crosslinkers. The results showed that the imprinting factor of the prepared MIP was increased from 0.93 to 4.38, and that the relative selection coefficient k' was 5.59. With the application of the material to be developed as a solid-phase extraction (SPE) filler for sulfonamides (SAs) in milk combined with UPLC-MS/MS, the validated method showed a sensitive quantification limit (0.89 µg/kg), a steady recovery (95.55%-97.97%) and an excellent precision (0.08%-2.92% RSD). Moreover, after 5 times usage, the recovery rate of MIP-SPE was still above 90%. Therefore, the prepared materials showed high performance of molecular adsorption and were water-resistant, which was also considered an excellent filler of SPE for SAs extraction in food or other fields.

摘要

为了解决传统分子印迹材料吸附性能不稳定和有机溶剂消耗量大的问题,我们开发了一种耐水且高吸附性的磺胺甲噁唑分子印迹聚合物(MIP),该聚合物采用混合功能单体结合疏水性交联剂的新型合成策略制备。结果表明,所制备的 MIP 的印迹因子从 0.93 增加到 4.38,相对选择系数 k'为 5.59。将所开发的材料作为固相萃取(SPE)填料用于牛奶中的磺胺类药物(SAs),并结合 UPLC-MS/MS,经验证的方法具有灵敏的定量限(0.89 µg/kg)、稳定的回收率(95.55%-97.97%)和优异的精密度(0.08%-2.92% RSD)。此外,经过 5 次使用后,MIP-SPE 的回收率仍高于 90%。因此,所制备的材料表现出高的分子吸附性能和耐水性,被认为是食品或其他领域中磺胺类药物提取 SPE 的理想填料。

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