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利用 HS-SPME/GC-MS 法测定白兰地中挥发性硫化合物(VSCs)的方法开发。

Development of the Method for Determination of Volatile Sulfur Compounds (VSCs) in Fruit Brandy with the Use of HS-SPME/GC-MS.

机构信息

Institute of Fermentation Technology and Microbiology, Faculty of Biotechnology and Food Sciences, Lodz University of Technology, Wolczanska 171/173, 90-924 Lodz, Poland.

出版信息

Molecules. 2020 Mar 9;25(5):1232. doi: 10.3390/molecules25051232.

Abstract

Volatile sulfur compounds (VSCs) play an important role in the aroma profile of fermented beverages. However, because of their low concentration in samples, their analysis is difficult. The headspace solid-phase microextraction (HS-SPME) technique coupled with gas chromatography and mass spectrometry (GC-MS) is one of the methods successfully used to identify VSCs in wine and beer samples. However, this method encounters more obstacles when spirit beverages are analyzed, as the ethanol content of the matrix decreases the method sensitivity. In this work, different conditions applied during HS-SPME/GC-MS analysis, namely: ethanol concentration, salt addition, time and temperature of extraction, as well as fiber coating, were evaluated in regard to 19 sulfur compounds. The best results were obtained when 50/30 μm Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) was used to preconcentrate the analytes from the sample at 35 °C for 30 min. The dilution of samples to 2.5% / ethanol and the addition of 20% / NaCl along with 1% EDTA significantly improves the sensitivity of extraction. The optimized method was applied to three fruit brandy samples (plum, pear, and apple) and quantification of VSCs was performed. A total of 10 compounds were identified in brandy samples and their concentration varied greatly depending on the raw material used from production. The highest concentration of identified VSCs was found in apple brandy (82 µg/L).

摘要

挥发性硫化合物(VSCs)在发酵饮料的香气特征中起着重要作用。然而,由于其在样品中的浓度较低,因此分析起来具有一定难度。顶空固相微萃取(HS-SPME)技术与气相色谱和质谱(GC-MS)相结合,是一种成功用于鉴定葡萄酒和啤酒样品中 VSCs 的方法。然而,当分析烈酒时,这种方法会遇到更多的障碍,因为基质中的乙醇含量会降低方法的灵敏度。在这项工作中,评估了 HS-SPME/GC-MS 分析过程中的不同条件,即:乙醇浓度、加盐、萃取时间和温度以及纤维涂层,针对 19 种硫化合物。当使用 50/30μm 二乙烯基苯/Carboxen/聚二甲基硅氧烷(DVB/CAR/PDMS)纤维从 35°C 的样品中预浓缩分析物 30 分钟时,可获得最佳结果。将样品稀释至 2.5%/乙醇并添加 20%/NaCl 以及 1%EDTA,可显著提高萃取的灵敏度。优化后的方法应用于三种水果白兰地样品(李子、梨和苹果),并对 VSCs 进行定量分析。在白兰地样品中鉴定出了 10 种化合物,其浓度因生产中使用的原料而异。在苹果白兰地中发现了最高浓度的鉴定出的 VSCs(82µg/L)。

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