中文摘要：色谱分离前的样品制备在分析过程中起着重要作用。为避免耗时和人工处理样品制备的缺陷，因此优选自动在线技术，如在线SPE-HPLC。在这项研究中，选择两种不同的在线提取方法用于霉菌毒素/内分泌干扰物玉米赤霉烯酮的测定，使用具有选择性空腔和结合位点的分子印迹聚合物（MIP）进行提取或使用提供非选择性相互作用的反相吸附剂C18进行提取，两种方法已经被开发、验证和比较。比较了两种方法的验证特性，并评估了两种方法线性度、重复性、精确度和回收率，这几个方面几乎相等。回收率在99.0-100.1%范围内，两种方法的检测限相同（1.5μgL-1）。对于加料啤酒样品来说C18吸附剂的方法精确度更好（2.5 vs. 5.4%RSD）。两种提取方法的选择性没有显著差异。本研究讨论了与该实验发现相关的可能原因和进一步细节。最后，两种经过验证的方法都用于测定啤酒样品中的玉米赤霉烯酮污染。由于玉米赤霉烯酮的天然荧光，选择了荧光检测色谱分离（λ（ex）= 270nm和λ（em）= 458nm）。
外文摘要：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 mu g 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 (lambda (ex) = 270 nm and lambda (em,) = 458 nm) was selected.
外文关键词：Molecularly imprinted polymers; On-line extraction; On-line SPE chromatography; Solid-phase extraction; Mycotoxin; Zearalenone
作者：Lhotska, Ivona; Gajdosova, Barbora; Solich, Petr; 等.
作者单位：Charles University Prague
期刊名称：ANALYTICAL AND BIOANALYTICAL CHEMISTRY
期刊影响因子：3.307
出版年份：2018
出版刊次：14
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