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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Modified graphene-silica as a sorbent for in-tube solid-phase microextraction coupled to liquid chromatography-tandem mass spectrometry. Determination of xanthines in coffee beverages
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Modified graphene-silica as a sorbent for in-tube solid-phase microextraction coupled to liquid chromatography-tandem mass spectrometry. Determination of xanthines in coffee beverages

机译：改性石墨烯 - 二氧化硅作为用于管中固相微萃取的吸附剂，偶联至液相色谱 - 串联质谱法。 咖啡饮料中的黄嘌呤测定

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Given the increasing need for analyzing natural or contaminating compounds in complex food matrices in a simple and automated way, coupling miniaturized sample preparation techniques with chromato-graphic systems have become a growing field of research. In this regard, given the low extraction efficiency of conventional sorbent phases, the development of materials with enhanced extraction capabilities is of particular interest. Here we present several synthesized graphene-based materials supported on aminopropyl silica as sorbents for the extraction of xanthines. The synthesized materials were characterized by infrared spectroscopy and scanning electron microscopy. Aminopropyl silica coated with graphene oxide and functionalized with octadecylsilane/end-capped (SiGOC18ecap) showed the best performance for xanthines extraction. Hence, this material was employed as an in-tube solid phase microextraction (in-tube SPME) device coupled online with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and applied for the analysis of xanthines in roasted coffee samples. Extraction parameters and detection conditions were optimized. The method showed low limits of quantification (0.3-1.0 mu g L-1), precision as relative standard deviation (RSD) values lower than 10%, recoveries between 73 and 109%, and pre-concentration factors from 5.6 to 7.2. Caffeine was determined in all ground roasted and instant coffee samples, in a wide range (0.9 to 36.8 mg g(-1)), and small amounts of theobromine and theophylline were also detected in some samples. This work demonstrated that functionalized graphene-based materials represent a promising new sorbent class for in-tube SPME, showing improved extraction capacity. The method was efficient, simple, and fast for the analysis of xanthines, demonstrating an excellent potential to be applied in other matrices. (C) 2020 Elsevier B.V. All rights reserved.
机译：鉴于以简单和自动化的方式分析复杂食物基质中的自然或污染化合物的越来越需要，偶联具有染色片图形系统的小型化样品制备技术已成为一种日益增长的研究领域。在这方面，考虑到常规吸附剂阶段的低提取效率，具有增强的提取能力的材料的发展特别感兴趣。在这里，我们在氨基丙基二氧化硅上呈现几种基于基于基于氨基丙基二氧化硅的材料，以萃取黄嘌呤。通过红外光谱和扫描电子显微镜表征合成材料。涂有石墨烯的氨基丙基二氧化硅胶和用十八烷基硅烷/端盖（SIGOC18ECAP）的官能化表现为黄嘌呤提取的最佳性能。因此，该材料用作在线耦合的内管固相微萃取（管SPME）装置，其在线耦合，具有超级性能液相色谱 - 串联质谱（UPLC-MS / MS），并施用于烤咖啡中的黄嘌呤分析样品。优化提取参数和检测条件。该方法显示出低定量限制（0.3-1.0μmg l-1），精确标准偏差（RSD）值低于10％，73至109％之间的回收率，5.6至7.2的预浓度因子。在宽范围内（0.9至36.8mg（-1）），在各种烘焙和速溶咖啡样品中测定咖啡因，在一些样品中也检测到少量的粗碱和茶碱。这项工作表明，官能化的石墨烯基材料代表了用于管道SPME的有希望的新吸附剂类，显示出改善的提取能力。该方法是高效，简单，快速的黄嘌呤分析，证明在其他基质中应用的优异潜力。 （c）2020 Elsevier B.v.保留所有权利。

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