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Rapid Extraction and Analysis of Volatile Solutes with an Effervescent Tablet.
Analytical Chemistry ( IF 6.7 ) Pub Date : 2020-01-15 , DOI: 10.1021/acs.analchem.9b05009
Decibel P Elpa,Shu-Pao Wu,Pawel L Urban

Extraction of volatile compounds from complex liquid matrices is a critical step in volatile compound analysis workflows. Recently, green chemistry principles are increasingly implemented in extraction processes. Some of the available approaches are solvent-free but still require concentration or trapping of analytes. Here, we propose effervescent tablet-induced extraction (ETIE) as a method of transferring volatile/semivolatile compounds from liquid matrices to the gas phase for analysis. This technique relies on the release of carbon dioxide produced in situ during a neutralization reaction, which occurs when a tablet is inserted into an aqueous sample matrix. In this process, many bubbles of carbon dioxide are instantly formed in the sample matrix. The bubbles rapidly extract and liberate volatile compounds from the sample. The gaseous effluent is then immediately transferred to a detector (atmospheric pressure chemical ionization mass spectrometry (MS) or gas chromatography (GC) hyphenated with MS). ETIE-GC-MS can be used for analysis of volatile compounds present in real samples. The method was validated for analysis of selected ethyl esters present in a yogurt drink. The calibration data set was linear over a range from 5 × 10-7 to 1 × 10-5 M. The limits of detection ranged from 1.51 × 10-7 to 6.82 × 10-7 M, while the recoveries ranged from 71 to 118%. Inter- and intraday precision of selected ethyl esters in aqueous solution was satisfactory (relative standard deviation, 3.6-18.3%). Furthermore, it is shown that ETIE improves the performance of headspace solid-phase microextraction while eliminating the need for heating and shaking samples.

中文翻译:

泡腾片快速提取和分析挥发性溶质。

从复杂的液体基质中提取挥发性化合物是挥发性化合物分析工作流程中的关键步骤。最近,在提取过程中越来越多地采用绿色化学原理。一些可用的方法是无溶剂的,但仍然需要浓缩或捕获分析物。在这里,我们提出泡腾片诱导提取(ETIE)作为将挥发性/半挥发性化合物从液相转移到气相进行分析的方法。该技术依赖于中和反应过程中原位产生的二氧化碳的释放,这是在将片剂插入水性样品基质中时发生的。在此过程中,许多二氧化碳气泡立即在样品基质中形成。气泡迅速从样品中提取并释放出挥发性化合物。然后将气态流出物立即转移到检测器(大气压化学电离质谱(MS)或用MS联用的气相色谱(GC))。ETIE-GC-MS可用于分析实际样品中存在的挥发性化合物。该方法经验证可用于分析酸奶饮料中存在的选定乙酯。校准数据集在5×10-7到1×10-5 M范围内是线性的。检测限在1.51×10-7到6.82×10-7 M范围内,而回收率在71到118之间%。所选乙酯在水溶液中的日间和日内精度令人满意(相对标准偏差为3.6-18.3%)。此外,表明ETIE改进了顶空固相微萃取的性能,同时消除了加热和摇动样品的需要。
更新日期:2020-01-16
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