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分子印迹与反相萃取法测定玉米赤霉烯酮:在线 SPE 色谱系统中方法开发及样品净化效率的对比研究。

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.

机构信息

The Department of Analytical Chemistry, Faculty of Pharmacy, Charles University, Heyrovského 1203, 500 05, Hradec Králové, Czech Republic.

出版信息

Anal Bioanal Chem. 2018 May;410(14):3265-3273. doi: 10.1007/s00216-018-0920-2. Epub 2018 Feb 17.

DOI:10.1007/s00216-018-0920-2
PMID:29455282
Abstract

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). 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 (λ = 270 nm and λ = 458 nm) was selected. Graphical abstract Determination of zearalenone in beer using an on-line extraction chromatography system.

摘要

样品在色谱分离前的制备在分析过程中起着重要作用。为避免繁琐且耗时的手动样品前处理,因此优先采用自动化在线技术,如在线 SPE-HPLC。本研究开发并比较了两种不同的在线提取方法,用于真菌毒素/内分泌干扰物玉米赤霉烯酮(ZEA)的测定,一种是使用具有选择性空腔和结合位点用于提取的分子印迹聚合物(MIP),另一种是使用提供非选择性相互作用的反相固定相 C18。对验证特性进行了比较,并且这两种方法在线性、重复性、精密度和回收率方面几乎相等。回收率范围为 99.0-100.1%,两种方法的检出限相同(1.5μg L)。对于加标啤酒样品,C18 固定相的方法精密度(2.5% vs. 5.4% RSD)更好。两种提取方法的选择性没有明显差异。讨论了与这一发现相关的可能原因和进一步细节。最后,应用两种经过验证的方法测定啤酒样品中的 ZEA 污染。由于 ZEA 具有天然荧光,因此选择了具有荧光检测(λ=270nm 和 λ=458nm)的色谱分离。

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