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Molecularly imprinted vs. reversed-phase extraction for the determination of zearalenone: a method development and critical comparison of sample clean-up efficiency achieved in an on-line coupled SPE chromatography system
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-02-17 , DOI: 10.1007/s00216-018-0920-2
Ivona Lhotská , Barbora Gajdošová , Petr Solich , Dalibor Šatínský

Sample preparation prior to chromatographic separation plays an important role in the analytical process. To avoid time-consuming and manual handling sample-prep, automated on-line techniques such as on-line SPE-HPLC are therefore preferred. In this study, two different on-line extraction approaches for mycotoxin/endocrine disruptor zearalenone (ZEA) determination using either molecularly imprinted polymer (MIP) with selective cavities and binding sites for extraction or a reversed-phase sorbent C18 providing non-selective interactions have been developed, validated, and compared. The validation characteristics were compared and the two methods were evaluated as being almost equal in terms of linearity, repeatability, precision, and recovery. Recoveries were in the range of 99.0–100.1% and limits of detection were found the same for both methods (1.5 μg L−1). Method precision calculated for spiked beer samples was better for C18 sorbent (2.5 vs. 5.4% RSD). No significant differences in the selectivity of either extraction method were observed. The possible reasons and further details associated with this finding are discussed. Finally, both validated methods were applied for the determination of ZEA contamination in beer samples. Due to ZEA’s native fluorescence, chromatographic separation with fluorimetric detection (λex = 270 nm and λem, = 458 nm) was selected.

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Graphical abstract

Determination of zearalenone in beer using an on-line extraction chromatography system.



中文翻译:

分子印迹与反相萃取测定玉米赤霉烯酮:在线偶联SPE色谱系统中方法开发和样品净化效率的关键比较

色谱分离之前的样品制备在分析过程中起着重要作用。为避免耗时和手动处理样品制备,因此首选自动化在线技术,例如在线SPE-HPLC。在这项研究中,使用具有选择性腔和结合位点的分子印迹聚合物(MIP)或提供非选择性相互作用的反相吸附剂C18来测定霉菌毒素/内分泌干扰物玉米赤霉烯酮(ZEA)的两种不同的在线提取方法具有以下特点:被开发,验证和比较。比较了验证特征,并评估了两种方法的线性,可重复性,精密度和回收率几乎相等。回收率在99.0–100之间。-1)。对于加标啤酒样品,计算出的方法精度对于C18吸附剂更好(2.5 vs. 5.4%RSD)。两种提取方法的选择性均未观察到显着差异。讨论了与该发现相关的可能原因和更多细节。最后,两种验证的方法都用于测定啤酒样品中的ZEA污染。由于ZEA的天然荧光,用荧光检测色谱分离(λ EX  = 270 nm和λ EM,  = 458纳米)被选中。

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图形概要

使用在线萃取色谱系统测定啤酒中的玉米赤霉烯酮。

更新日期:2018-02-17
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