Guo Ping, Yuan Xucan, Zhang Jingjing, Wang Binjie, Sun Xiaoyang, Chen Xiaohui, Zhao Longshan
Department of Pharmaceutical Analysis, School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road in Shenhe District, Shenyang, Liaoning, 110016, China.
Anal Bioanal Chem. 2018 Jan;410(2):373-389. doi: 10.1007/s00216-017-0727-6. Epub 2017 Nov 9.
A highly binding dummy template surface of molecularly imprinted polymers (MWNTs-MIPs) was synthesized on multi-walled carbon nanotubes surface using 2-phenylpropionic acid as dummy template, 4-vinylpyridine as the functional monomer, ethylene glycol dimethacrylate as the cross-linker, and DMF as porogen by precipitation polymerization method. MIPs were characterized by FT-IR spectroscopy, scanning electron microscope, thermo-gravimetric analysis, and nitrogen adsorption-desorption experiment. Adsorption and selectivity experiments of MIPs and non-imprinted polymers (NIPs) verified that the MIPs had a good selectivity and adsorption properties for five 2-phenylpropionic acid nonsteroidal anti-inflammatory drugs (NSAIDs). Imprinted polymer was used as a sorbent material for μSPE in current work and μSPE-DLLME method was selected for pretreatment of water samples. The μSPE-DLLME method was successfully used for the pre-concentration of five non-steroidal anti-inflammatory drugs in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry. Efficiencies of μSPE and DLLME were thoroughly investigated and optimized in this study. The optimal results were obtained by using 3 mL of 1% formic acid-acetonitrile as elution solvent and dichloroethane and acetonitrile as extractant and disperser solvent, respectively. Limits of detection and quantification of five NSAIDs for different water matrices varied from 0.50 to 1.10 ng L and 0.93 to 2.20 ng L, respectively. Each target analyte had a good linearity in its corresponding concentration range. Enrichment factors of target analytes ranged from 91 to 215. Recoveries of the target analytes were between 72.43 and 113.99% at the concentration levels of 0.02, 0.1, and 0.5 μg L. The developed method was successfully applied to extraction and analysis of NSAIDs in different water samples with satisfactory results which could help us better understand their environmental fate and risk to ecological health. Graphical abstract Dummy-surface molecularly imprinted polymers as a sorbent of micro-solid-phase extraction combined with dispersive liquid-liquid microextraction for determination of five 2-phenylpropionic acid NSAIDs in aquatic environmental samples.
以2-苯丙酸为虚拟模板、4-乙烯基吡啶为功能单体、乙二醇二甲基丙烯酸酯为交联剂、N,N-二甲基甲酰胺为致孔剂，采用沉淀聚合法在多壁碳纳米管表面合成了具有高结合能力的分子印迹聚合物（MWNTs-MIPs）虚拟模板表面。通过傅里叶变换红外光谱、扫描电子显微镜、热重分析和氮吸附-脱附实验对MIPs进行了表征。MIPs和非印迹聚合物（NIPs）的吸附和选择性实验证实，MIPs对5种2-苯丙酸非甾体抗炎药（NSAIDs）具有良好的选择性和吸附性能。在当前工作中，将印迹聚合物用作微固相萃取的吸附剂材料，并选择微固相萃取-分散液液微萃取（μSPE-DLLME）方法对水样进行预处理。μSPE-DLLME方法成功用于不同环境水样中5种非甾体抗炎药的预富集，然后进行超高效液相色谱-串联质谱分析。本研究对μSPE和DLLME的效率进行了深入研究和优化。以3 mL 1%甲酸-乙腈为洗脱溶剂，二氯乙烷和乙腈分别为萃取剂和分散剂溶剂，获得了最佳结果。不同水基质中5种NSAIDs的检测限和定量限分别为0.501.10 ng/L和0.932.20 ng/L。各目标分析物在其相应浓度范围内具有良好的线性关系。目标分析物的富集因子为91215。在0.02、0.1和0.5 μg/L浓度水平下，目标分析物的回收率为72.43%113.99%。所建立的方法成功应用于不同水样中NSAIDs的萃取和分析，结果令人满意，有助于我们更好地了解它们的环境归宿和对生态健康的风险。图形摘要 虚拟表面分子印迹聚合物作为微固相萃取吸附剂结合分散液液微萃取用于测定水环境样品中的5种2-苯丙酸非甾体抗炎药。
