GUECKO, Departamento de Ciências e Engenharia do Ambiente, FCT, Universidade Nova de Lisboa, Campus de Caparica, Portugal.
J Chromatogr A. 2010 Mar 12;1217(11):1845-55. doi: 10.1016/j.chroma.2010.01.045. Epub 2010 Jan 22.
The chemical composition of the needles of P. pinea, P. pinaster, P. halepensis, P. nigra, P. brutia, P. patula, P. radiata, P. taeda, P. elliotti, P. kesiya, P. sylvestris and P. eldarica was investigated. Headspace solid-phase microextraction and steam distillation extraction were used to collect the volatile fractions. Samples were analyzed using one-dimensional gas chromatography (1D-GC) and comprehensive two-dimensional gas chromatography (GCxGC) associated with a quadrupole and a time-of-flight mass detectors. Results showed that the analytical capabilities of 1D-GC are partially limited by the separation power of the columns. The higher sensibility and the absence of peak skewing of the time-of-flight mass analyzer, with the use of automated peak finding and deconvolution algorithms, allowed for the detection of trace components with qualitative full spectra and the extraction of true mass spectra from coeluting compounds, promoting their reliable identification and thus significantly improving results obtained by 1D-GC/MS, when using a quadrupole mass analyzer. The use of GC x GC resulted in enhanced separation efficiency and increased signal to noise ratio (sensitivity) of the analytes, maximizing mass spectra quality and improving compound detection and identification. This work shows the use of 1D-GC/ToFMS for the analysis of pine needles volatiles, achieving the detection of 177 compounds, that is more than twice the number previously identified by standard 1D-GC/MS. The analysis by GC x GC for the same sample allowed the detection of 212 compounds. The enantioselective GC x GC analysis performed for all the Pinus spp. under study achieved the detection of 422 different compounds. Cross-over phenomena according to operational conditions are highlighted and discussed.
研究了欧洲赤松、湿地松、地中海柏木、黑松、欧洲黑松、辐射松、火炬松、湿地松、南亚松、云南松、樟子松和长叶松的针叶的化学成分。采用顶空固相微萃取和水蒸气蒸馏提取法收集挥发性成分。使用一维气相色谱（1D-GC）和全二维气相色谱（GCxGC）结合四极杆和飞行时间质谱检测器对样品进行分析。结果表明，1D-GC 的分析能力部分受到柱分离能力的限制。飞行时间质谱分析仪的灵敏度更高，峰形无偏，使用自动峰查找和解卷积算法，可以检测痕量成分，获得全谱定性和共洗脱化合物的真实质谱图，从而促进其可靠鉴定，从而显著提高使用四极杆质量分析仪时 1D-GC/MS 的结果。GCxGC 的使用提高了分离效率和分析物的信噪比（灵敏度），最大限度地提高了质谱质量，提高了化合物的检测和鉴定能力。这项工作展示了使用 1D-GC/ToFMS 分析松针挥发物，实现了对 177 种化合物的检测，这是以前使用标准 1D-GC/MS 鉴定的化合物数量的两倍多。对相同样品进行的 GC x GC 分析可检测到 212 种化合物。对所有研究的 Pinus spp.进行的对映选择性 GC x GC 分析可检测到 422 种不同的化合物。根据操作条件突出和讨论了交叉现象。
