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Selective extraction of aliphatic amines by functionalized mesoporous silica-coated solid phase microextraction Arrow

机译:通过功能化介孔二氧化硅包被的固相微萃取选择性萃取脂肪胺

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摘要

Mesoporous silica-coated solid phase microextraction (SPME) Arrow systems were developed for capturing of low-molecular-weight aliphatic amines (LMWAAs) from complicated sample matrices. Specifically, silicas of type MCM-41, SBA-15 and KIT-6 were chosen as substrates to afford size-exclusion selectivity. They possess ordered multidimensional pore-channel structures and mesopore sizes between 3.8 and 8.2 nm. Their surface acidity was enhanced by grafting them with a layer of titanium hydrogenphosphate (-TP). This enhanced the chemical selectivity for basic LMWAAs. The siliceous coatings increased the extraction of ethylamine, diethylamine (DEA) and triethylamine (TEA) by factors of 18.6–102.5, 4.8–10.8 and 2.6–4.0, respectively, when compared to the commercial SPME Arrow with polydimethylsiloxane/divinylbenzene coating. Among them, the MCM-41 and MCM-41-TP coated SPME Arrows demonstrated exceptional selectivity towards LMWAAs that were quantified by gas chromatography-mass spectrometry (GC-MS). The total peak area ratios of LMWAAs/ten competing compounds were 25.4 and 36.3, respectively. The extraction equilibrium was reached within 20–30 min. The MCM-41 and MCM-41-TP derived SPME Arrows gave very similar results (18.4 ± 2.1–376 ± 12 ng g−1 to DEA and TEA) when applied to urban mushroom samples. SPME Arrow with MCM-41 coatings followed by GC-MS was applied also to the analysis of atmospheric air and urine samples resulting in high selectivity due to the size and mesoporous structure of the functionalized silica, and its chemical interactions with the LMWAAs. >Graphical abstractScheme of synthesis of the MCM-41 silicas, and the preparation of solid phase microextraction Arrow coatings. They were employed for selective capturing of aliphatic amines from complex sample matrices, followed by gas chromatography-mass spectrometry.
机译:开发了介孔二氧化硅包覆的固相微萃取(SPME)Arrow系统,用于从复杂的样品基质中捕获低分子量脂肪胺(LMWAAs)。具体而言,选择MCM-41,SBA-15和KIT-6类型的二氧化硅作为底物,以提供尺寸排阻选择性。它们具有有序的多维孔道结构,介孔尺寸在3.8至8.2 nm之间。通过将它们接枝一层磷酸氢钛(-TP)可以提高其表面酸度。这增强了对基本LMWAA的化学选择性。与带有聚二甲基硅氧烷/二乙烯基苯涂层的市售SPME Arrow相比,硅质涂层将乙胺,二乙胺(DEA)和三乙胺(TEA)的提取分别提高了18.6-102.5、4.8-10.8和2.6-4.0。其中,MCM-41和MCM-41-TP涂层的SPME Arrows表现出对LMWAA的出色选择性,该选择性通过气相色谱-质谱(GC-MS)进行了定量。 LMWAA /十种竞争化合物的总峰面积比分别为25.4和36.3。在20–30分钟内达到提取平衡。当将MCM-41和MCM-41-TP衍生的SPME箭应用于城市蘑菇样品时,得到的结果非常相似(DEA和TEA的18.4±2.1-376±12 ng g -1 )。由于功能化二氧化硅的尺寸和介孔结构及其与LMWAA的化学相互作用,带有MCM-41涂层和GC-MS的SPME Arrow还可用于分析大气和尿液样品,从而具有很高的选择性。 <!-fig ft0-> <!-fig @ position =“ anchor” mode =文章f4-> <!-fig mode =“ anchred” f5-> >图形摘要<!-无花果/图形|无花果/替代品/图形模式=“ anchred” m1-> <!-标题a7-> MCM-41二氧化硅的合成方案以及固相微萃取箭涂层的制备。它们用于从复杂样品基质中选择性捕获脂肪胺,然后进行气相色谱-质谱分析。

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