A simple and sensitive method was developed and validated to simultaneously separate and determine the 2‐Methoxy‐3,5‐dimethylpyrazine, 2‐Isopropyl‐3‐methoxypyrazine, guaiacol, 2‐Isobutyl‐3‐methoxypyrazine, 2‐Methylisoborneol, geosmin, 2,4,6‐Trichloroanisole, 2,3,4,6‐Tetrachloroanisole, 2,4,6‐Tribromoanisole and Pentachloroanisole in cork stoppers via headspace solid‐phase microextraction (HS‐SPME) coupled with gas chromatography tandem mass spectrometry (GC–MS/MS). The influence of the fibre coating used, the extraction times and temperatures, the sodium chloride additions and the desorption temperatures were investigated. Once done, the optimial HS‐SPME conditions established were divinylbenzene/carboxenpolydimethylsiloxane/polydimethylsiloxane (DVB/CAR/PDMS) fibres, a 50°C extraction temperature, 60‐min extraction time, an ionic strength of 3‐g sodium chlorid and a 290°C desorption temperature. The method showed a good linearity (R² ≥ 0.994) within the tested range (from 0.1 to 50 ng L⁻¹) for all the compounds. Using TCA‐d10 and MIB‐d3 as internal standards the precision, expressed as repeatability and reproducibility RSD, was <10% in both. Note that the limits of quantifications (LOQs) are below the sensory threshold levels for such compounds in water and wine. Good recoveries were obtained for cork macerates (from 100.4% to 126%) and when compared with other reported methods using HS‐SPME in water and cork stopper samples, the present method had more analytes with the lowest limit of detection for most of the targeted compounds, along with good precision and recovery.

中文翻译：

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使用顶空固相微萃取气相色谱串联质谱法对引起软木塞异味的主要气味物质进行定量分析的开发和优化


开发并验证了一种简单、灵敏的方法，可同时分离和测定 2-甲氧基-3,5-二甲基吡嗪、2-异丙基-3-甲氧基吡嗪、愈创木酚、2-异丁基-3-甲氧基吡嗪、2-甲基异冰片、土臭素、2通过顶空固相微萃取 (HS-SPME) 与气相色谱串联质谱 (GC-质谱/质谱）。研究了所用纤维涂层、萃取时间和温度、氯化钠添加量和解吸温度的影响。完成后，建立的最佳 HS-SPME 条件为二乙烯基苯/羧烯聚二甲基硅氧烷/聚二甲基硅氧烷 (DVB/CAR/PDMS) 纤维、50°C 萃取温度、60 分钟萃取时间、3 g 氯化钠的离子强度和 290 °C 解吸温度。该方法在所有化合物的测试范围（0.1 至 50 ng L ^-1 ）内均表现出良好的线性（ R ² ≥ 0.994）。使用 TCA-d10 和 MIB-d3 作为内标，两者的精密度（以重复性和再现性 RSD 表示）均为 <10%。请注意，水和酒中此类化合物的定量限 (LOQ) 低于感官阈值水平。软木浸渍物获得了良好的回收率（从 100.4% 到 126%），与其他报道的在水和软木塞样品中使用 HS-SPME 的方法相比，本方法具有更多的分析物，并且大多数目标物的检测限最低。化合物，以及良好的精密度和回收率。