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

机译:HS-SPME / GC-MS用于水果白兰地中挥发性硫化合物(VSCs)测定方法的开发

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摘要

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).
机译:挥发性硫化物(VSC)在发酵饮料的香气中起重要作用。但是,由于它们在样品中的浓度低,因此很难进行分析。顶空固相微萃取(HS-SPME)技术与气相色谱和质谱(GC-MS)结合是成功鉴定葡萄酒和啤酒样品中VSC的方法之一。但是,当分析烈性饮料时,该方法遇到更多障碍,因为基质中的乙醇含量降低了方法的灵敏度。在这项工作中,针对19种含硫化合物评估了HS–SPME / GC–MS分析中应用的不同条件,即:乙醇浓度,盐分添加,提取的时间和温度以及纤维涂层。当使用50/30μm二乙烯基苯/羧甲基/聚二甲基硅氧烷(DVB / CAR / PDMS)在35°C下预浓缩样品中的分析物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和1%EDTA可以显着提高提取的灵敏度。将优化方法应用于三个水果白兰地样品(李子,梨和苹果),并对VSC进行定量。在白兰地样品中总共鉴定出10种化合物,其浓度根据生产中使用的原材料而有很大差异。苹果白兰地中检出的VSC含量最高(82 µg / L)。

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