Cacho J I, Campillo N, Viñas P, Hernández-Córdoba M
Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum", University of Murcia, E-30100 Murcia, Spain.
J Chromatogr A. 2015 Jun 19;1399:18-24. doi: 10.1016/j.chroma.2015.04.041. Epub 2015 Apr 28.
Headspace sorptive extraction (HSSE) was used to preconcentrate seven monoterpenes (eucalyptol, linalool, menthol, geraniol, carvacrol, thymol and eugenol) for separation by gas chromatography and mass spectrometry (GC-MS). Three commercially available coatings for the stir bars, namely Polydimethylsiloxane (PDMS), polyacrilate (PA) and Ethylene glycol-silicone (EG-Silicone), were tested, and the influential parameters both in the adsorption and the thermal desorption steps were optimized. PDMS provided the best sensitivity for linalool, geraniol, menthol and eucalyptol, whereas EG-Silicone was best for extracting the phenolic monoterpenes studied. Considering the average obtained slopes from all compounds, PDMS pointed as the best option, and the analytical characteristics for the HSSE-TD-GC-MS method using this coating were obtained. Quantification of the samples was carried out by matrix-matched calibration using a synthetic honey. Detection limits ranged between 0.007 and 0.032 ng g(-1), depending on the compound. Twelve honey samples of different floral origins were analyzed using the HSSE-GC-MS method, the analytes being detected at concentrations up to 64 ng g(-1).
顶空吸附萃取(HSSE)用于对7种单萜类化合物(桉叶油素、芳樟醇、薄荷醇、香叶醇、香芹酚、百里香酚和丁香酚)进行预浓缩,以便通过气相色谱和质谱联用(GC-MS)进行分离。测试了三种市售的搅拌棒涂层,即聚二甲基硅氧烷(PDMS)、聚丙烯酸酯(PA)和乙二醇-硅氧烷(EG-硅氧烷),并对吸附和解吸步骤中的影响参数进行了优化。PDMS对芳樟醇、香叶醇、薄荷醇和桉叶油素具有最佳灵敏度,而EG-硅氧烷对所研究的酚类单萜的萃取效果最佳。考虑到所有化合物获得的平均斜率,PDMS被认为是最佳选择,并获得了使用该涂层的HSSE-TD-GC-MS方法的分析特性。使用合成蜂蜜通过基质匹配校准对样品进行定量。检测限在0.007至0.032 ng g⁻¹之间,具体取决于化合物。使用HSSE-GC-MS方法分析了12个不同花源的蜂蜜样品,检测到的分析物浓度高达64 ng g⁻¹。