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基于高效液相色谱与气相色谱-质谱联用的离线耦合法测定咖啡酿造物中的丙烯酰胺。

A new approach based on off-line coupling of high-performance liquid chromatography with gas chromatography-mass spectrometry to determine acrylamide in coffee brew.

机构信息

Instituto de Ciencia y Tecnología de Alimentos y Nutrición (ICTAN-CSIC), Consejo Superior de Investigaciones Científicas (CSIC), Madrid, Spain.

出版信息

J Sep Sci. 2013 Jan;36(2):320-4. doi: 10.1002/jssc.201200635. Epub 2012 Dec 10.

DOI:10.1002/jssc.201200635
PMID:23229640
Abstract

A new method based on off-line coupling of LC with GC in replacement of conventional sample preparation techniques is proposed to analyze acrylamide in coffee brews. The method involves the preseparation of the sample by LC, the collection of the selected fraction, its concentration under nitrogen, and subsequent analysis by GC coupled with MS. The composition of the LC mobile phase and the flow rate were studied to select those conditions that allowed separation of acrylamide without coeluting compounds. Under the conditions selected recoveries close to 100% were achieved while LODs and LOQs equal to 5 and 10 μg/L for acrylamide in brewed coffee were obtained. The method developed enabled the reliable detection of acrylamide in spiked coffee beverage samples without further clean-up steps or sample manipulation.

摘要

提出了一种基于离线 LC 与 GC 耦联的新方法,以替代传统的样品制备技术,用于分析咖啡提取物中的丙烯酰胺。该方法通过 LC 对样品进行预分离,收集选定的馏分,在氮气下浓缩,然后通过 GC 与 MS 进行分析。研究了 LC 流动相的组成和流速,以选择允许丙烯酰胺分离而没有共洗脱化合物的条件。在所选择的条件下,回收率接近 100%,而在煮咖啡中的丙烯酰胺的 LODs 和 LOQs 则分别为 5 和 10 μg/L。所开发的方法无需进一步的净化步骤或样品处理,即可可靠地检测加标咖啡饮料样品中的丙烯酰胺。

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