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首页> 外文期刊>Analytical and bioanalytical chemistry >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
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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

机译:分子印迹与反相萃取用于测定Zealalenone:在线耦合SPE色谱系统中达到样品清洁效率的方法开发和临界比较

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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?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 ( λ ~(ex)?=?270?nm and λ ~(em,)?=?458?nm) was selected. Graphical abstract Determination of zearalenone in beer using an on-line extraction chromatography system.
机译:在色谱分离之前的样品制备在分析过程中起重要作用。为避免耗时和手动处理样品 - 预制,因此优选自动在线SPE-HPLC等在线技术。在本研究中,使用分子印迹聚合物(MIP)与选择性腔体和用于萃取的结合位点的两种不同的在线提取方法(ZEA)测定,或提供非选择性相互作用的反相吸附剂C18已经开发,验证,并比较了。比较验证特征,并评估两种方法在线性,可重复性,精度和恢复方面几乎相等。回收率在99.0-100.1%的范围内,并且两种方法发现相同的检测限额(1.5ΩΩ1_(?1))。对于尖刺啤酒样品计算的方法精度对于C18吸附剂(2.5 Vs.5.4%RSD)更好。观察到任何提取方法的选择性没有显着差异。讨论了与此发现相关的可能原因和进一步的细节。最后,应用两种验证的方法用于测定ZEA污染在啤酒样品中。由于ZEA的原生荧光,选择了荧光检测的色谱分离(λ〜(ex)?=Δ270≤nm和λ〜(em,)?= 458?nm)。使用在线提取色谱系统的图解抽象测定啤酒中的酸甲酮。

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