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Development of Head Space Sorptive Extraction Method for the Determination of Volatile Compounds in Beer and Comparison with Stir Bar Sorptive Extraction

机译:顶空吸附萃取法测定啤酒中挥发性化合物的开发及与搅拌棒吸附萃取法的比较

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摘要

A headspace sorptive extraction method coupled with gas chromatography–mass spectrometry (HSSE–GC–MS) was developed for the determination of 37 volatile compounds in beer. After optimization of the extraction conditions, the best conditions for the analysis were stirring at 1000 rpm for 180 min, using an 8-mL sample with 25% NaCl. The analytical method provided excellent linearity values ( > 0.99) for the calibration of all the compounds studied, with the detection and quantification limits obtained being low enough for the determination of the compounds in the beers studied. When studying the repeatability of the method, it proved to be quite accurate, since RSD% values lower than 20% were obtained for all the compounds. On the other hand, the recovery study was successfully concluded, resulting in acceptable values for most of the compounds (80–120%). The optimised method was successfully applied to real beer samples of different types (ale, lager, stout and wheat). Finally, an analytical comparison of the optimised HSSE method, with a previously developed and validated stir bar sorptive extraction (SBSE) method was performed, obtaining similar concentration values by both methods for most compounds.
机译:开发了一种顶空吸附萃取法与气相色谱-质谱联用(HSSE-GC-MS),用于测定啤酒中的37种挥发性化合物。优化提取条件后,使用含25%NaCl的8-mL样品以1000 rpm搅拌180分钟,以进行最佳分析。该分析方法为所有所研究化合物的校准提供了极好的线性值(> 0.99),并且所获得的检测和定量限足够低,无法确定所研究啤酒中的化合物。在研究该方法的可重复性时,由于所有化合物的RSD%值均低于20%,因此证明了该方法的准确性。另一方面,回收率研究成功完成,大多数化合物的回收率均可接受(80%至120%)。该优化方法已成功应用于不同类型(啤酒,啤酒,黑啤酒和小麦)的真实啤酒样品。最后,对优化的HSSE方法与先前开发并验证的搅拌棒吸附萃取(SBSE)方法进行了分析比较,两种方法对大多数化合物均获得了相似的浓度值。

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