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用于移液器吸头固相萃取结合气相色谱法快速筛查芹菜中三氯杀螨醇的离子液体分子印迹聚合物

Ionic liquid molecularly imprinted polymers for application in pipette-tip solid-phase extraction coupled with gas chromatography for rapid screening of dicofol in celery.

作者信息

Yan Hongyuan, Yang Chen, Sun Yunyun, Row Kyung Ho

机构信息

Key Laboratory of Pharmaceutical Quality Control of Hebei Province & Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China.

Key Laboratory of Pharmaceutical Quality Control of Hebei Province & Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry of Education & College of Pharmacy, Hebei University, Baoding 071002, China.

出版信息

J Chromatogr A. 2014 Sep 26;1361:53-9. doi: 10.1016/j.chroma.2014.07.102. Epub 2014 Aug 7.

Abstract

A new type of ionic liquid molecularly imprinted polymers (IL-MIPs) synthesized by precipitation polymerization using 1-allyl-3-methylimidazolium bromide as an auxiliary solvent and α-chloro-dichlorodiphenyltrichloroethane (α-chloro-DDT) as the template was applied as a selective sorbent of minimized pipette tip-solid-phase extraction (PT-SPE) for rapid isolation and extraction of dicofol (DCF) from celery samples. The pretreatment procedure of celery samples involved only 2.0mg of IL-MIPs, 0.8 mL of acetonitrile-water (ACN-H2O; 1:1, v/v) (washing solvent), and 1.0 mL of acetone-10% acetic acid (HOAc) (elution solvent). Compared with molecularly imprinted polymers (MIPs), ionic liquid-non-imprinted polymers (IL-NIPs) and conventional sorbents such as C18, Si, NH2, and Al2O3-N, IL-MIPs showed higher adsorption and purification capacity to DCF in aqueous solution. Good linearity for DCF was observed in the range from 2.3 to 232.5 ng g(-1) (r(2)=0.9995). The average recoveries at three spiking levels ranged from 86.6% to 101.9% with relative standard deviations (RSDs) of ≤ 6.5% (n=3). The presented IL-MIPs-PT-SPE-GC/ECD method combines the advantages of MIPs, IL, and PT-SPE, and can be used in aqueous conditions with high affinity and selectivity to analytes of complex samples.

摘要

以1-烯丙基-3-甲基咪唑溴盐为辅助溶剂、α-氯二氯二苯三氯乙烷(α-氯-DDT)为模板,通过沉淀聚合法合成了一种新型离子液体分子印迹聚合物(IL-MIPs),将其作为微量移液器吸头-固相萃取(PT-SPE)的选择性吸附剂,用于从芹菜样品中快速分离和萃取三氯杀螨醇(DCF)。芹菜样品的预处理过程仅需2.0mg IL-MIPs、0.8mL乙腈-水(ACN-H₂O;1:1,v/v)(洗涤溶剂)和1.0mL丙酮-10%乙酸(HOAc)(洗脱溶剂)。与分子印迹聚合物(MIPs)、离子液体非印迹聚合物(IL-NIPs)以及传统吸附剂如C18、Si、NH₂和Al₂O₃-N相比,IL-MIPs在水溶液中对DCF表现出更高的吸附和净化能力。DCF在2.3至232.5 ng g⁻¹范围内呈现出良好的线性关系(r² = 0.9995)。三个加标水平下的平均回收率在86.6%至101.9%之间,相对标准偏差(RSDs)≤ 6.5%(n = 3)。所提出的IL-MIPs-PT-SPE-GC/ECD方法结合了MIPs、离子液体和PT-SPE的优点,可在水性条件下对复杂样品中的分析物具有高亲和力和选择性。

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