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首页> 外文期刊>Journal of mass spectrometry: JMS >Development and optimization of a quantitative analysis of main odorants causing off flavours in cork stoppers using headspace solid-phase microextraction gas chromatography tandem mass spectrometry
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Development and optimization of a quantitative analysis of main odorants causing off flavours in cork stoppers using headspace solid-phase microextraction gas chromatography tandem mass spectrometry

机译：具有顶空固相微萃取气相色谱串联质谱法测定软木塞中的主要气味的定量分析，导致软木塞止血剂的定量分析

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摘要

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 degrees C extraction temperature, 60-min extraction time, an ionic strength of 3-g sodium chlorid and a 290 degrees C desorption temperature. The method showed a good linearity (R-2 >= 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.
机译：建立并验证了一种简单、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-甲基异龙脑、土工胺、2,4,6-三氯苯胺、2,3,4,6-四氯茴香醚、，通过顶空固相微萃取（HS-SPME）结合气相色谱-串联质谱（GC-MS/MS）分析软木塞中的2,4,6-三溴苯胺和五氯苯甲醚。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，确定的最佳HS-SPME条件为二乙烯基苯/碳氧基聚二甲基硅氧烷/聚二甲基硅氧烷（DVB/CAR/PDMS）纤维、50℃的萃取温度、60分钟的萃取时间、3-g氯化钠的离子强度和290℃的脱附温度。该方法在所有化合物的测试范围（从0.1至50 ng L-1）内显示出良好的线性（R-2>=0.994）。使用TCA-d10和MIB-d3作为内标，以重复性和再现性RSD表示的精密度均<10%。请注意，定量限（LOQ）低于水和葡萄酒中此类化合物的感官阈值水平。软木浸渍物的回收率良好（从100.4%到126%），与其他报告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，对大多数目标化合物的最低检测限，以及良好的精密度和回收率。

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