UFZ-Helmholtz Centre for Environmental Research, Department Monitoring and Exploration Technologies, Leipzig, Germany.
UFZ-Helmholtz Centre for Environmental Research, Department of Analytical Chemistry, Leipzig, Germany.
J Mol Recognit. 2018 Mar;31(3). doi: 10.1002/jmr.2629. Epub 2017 Mar 21.
In this study, a general simple and inexpensive method is introduced for the preparation of a paper-based selective disk-type solid phase extraction (SPE) technique, appropriate for fast and high throughput monitoring of target compounds. An ion exchange molecularly imprinted polymer (MIP) was synthesized for the extraction and analysis of acesulfame, an anthropogenic water quality marker. Acesulfame imprinting was used as an example for demonstrating the benefits of a nanosized, swellable MIP extraction sorbents integrated in an on-site compatible concept for water quality monitoring. Compared with an 8 mL standard SPE cartridge, the paper-based MIP disk (47 mm ø) format allowed (1) high sample flow rates up to 30 mL•min without losing extraction efficiency (2) extracting sample volumes up to 500 mL in much shorter times than with standard SPE, (3) the reuse of the disks (up to 3 times more than SPE cartridge) due to high robustness and an efficient post-cleaning, and (4) reducing the sampling time from 100 minutes (using the standard SPE format) to about 2 minutes with the MIP paper disk for 50 mL water sample. Different parameters like cellulose fiber/polymer ratios, sample volume, sample flow-rate, washing, and elution conditions were evaluated and optimized. Using developed extraction technique with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) analysis, a new protocol was established that provides detection and quantification limits of 0.015 μg•L and 0.05 μg•L , respectively. The developed paper disks were used in-field for the selective extraction of target compounds and transferred to the laboratory for further analysis.
在这项研究中,介绍了一种通用的简单且廉价的方法,用于制备基于纸张的选择性盘式固相萃取(SPE)技术,适用于快速和高通量监测目标化合物。合成了离子交换型分子印迹聚合物(MIP),用于萃取和分析人工水质标志物——乙酰磺胺酸。以乙酰磺胺酸印迹为例,展示了纳米级可溶胀 MIP 萃取吸附剂集成在现场兼容概念中用于水质监测的优势。与 8mL 标准 SPE 小柱相比,基于纸张的 MIP 盘(47mmø)格式允许(1)高样品流速高达 30mL·min,而不损失萃取效率;(2)与标准 SPE 相比,可在更短的时间内提取多达 500mL 的样品;(3)由于高稳健性和高效的后清洗,可以重复使用磁盘(比 SPE 小柱多 3 倍以上);(4)使用 MIP 纸盘时,将采样时间从 100 分钟(使用标准 SPE 格式)缩短至约 2 分钟,用于 50mL 水样。评估和优化了不同的参数,如纤维素纤维/聚合物比例、样品体积、样品流速、洗涤和洗脱条件。使用开发的萃取技术与高效液相色谱-串联质谱(HPLC-MS-MS)分析相结合,建立了一种新的方案,提供了 0.015μg·L 和 0.05μg·L 的检测限和定量限。开发的纸盘用于现场选择性萃取目标化合物,并转移到实验室进行进一步分析。