Department of Chemistry, University of La Rioja, Logroño, La Rioja, Spain.
J Sep Sci. 2009 Nov;32(21):3746-54. doi: 10.1002/jssc.200900347.
A headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS) method was optimised and validated for the determination of 4-ethylguaiacol, 4-ethylphenol, 4-vinylguaiacol and 4-vinylphenol, involved in the presence of Brett character, in ciders. The influence of different parameters on extraction efficiency (fibre coating, salt addition, exposure time, extraction temperature and sample volume/total volume ratio) was evaluated. Divinylbenzene/carboxen/PDMS was selected as extraction fibre and the other optimised parameters were as follows: 10 mL of cider, temperature 70 degrees C, extraction time 60 min and addition of 0.4 g/mL of NaCl. The proposed method showed satisfactory linearity. The detection limits obtained were 0.01 microg/L for 4-ethylguaiacol, 0.02 microg/L for 4-ethylphenol, 0.08 microg/L for 4-vinylguaiacol and 0.03 microg/L for 4-vinylphenol. These detection limits were lower than those obtained in previous studies on the determination of volatile phenols in other alcoholic beverages. Good recoveries of over 95% were observed for all compounds, and the repeatability obtained was considered acceptable, ranging between 4 and 10%. To demonstrate the feasibility of the procedure, the method was applied to the analysis of commercial ciders. To our knowledge, this is the first time that the headspace solid-phase microextraction procedure has been optimised to determine specifically the Brett character responsible compounds in cider.
采用顶空固相微萃取（HS-SPME）结合气相色谱-串联质谱（GC-MS/MS）方法对苹果酒中与布雷特特征有关的 4-乙基愈创木酚、4-乙基苯酚、4-乙烯基愈创木酚和 4-乙烯基苯酚进行了优化和验证。评估了不同参数对萃取效率（纤维涂层、加盐、暴露时间、萃取温度和样品体积/总体积比）的影响。选用二乙烯基苯/Carboxen/PDMS 作为萃取纤维，其他优化参数如下：苹果酒 10 mL，温度 70℃，萃取时间 60 min，添加 0.4 g/mL NaCl。该方法具有良好的线性。得到的检测限分别为 4-乙基愈创木酚 0.01μg/L，4-乙基苯酚 0.02μg/L，4-乙烯基愈创木酚 0.08μg/L，4-乙烯基苯酚 0.03μg/L。这些检测限低于以前关于其他酒精饮料中挥发性酚类物质测定的研究。所有化合物的回收率均超过 95%，重复性可接受，范围在 4%至 10%之间。为了证明该程序的可行性，将该方法应用于商业苹果酒的分析。据我们所知，这是首次优化顶空固相微萃取程序来专门测定苹果酒中与布雷特特征有关的化合物。
