Department of Chemistry, National Central University, Chungli 320, Taiwan.
J Chromatogr A. 2011 Aug 26;1218(34):5733-42. doi: 10.1016/j.chroma.2011.06.067. Epub 2011 Jun 23.
This study investigated the feasibility of analyzing a full range of ambient volatile organic compounds (VOCs) from C(3) to C(12) using gas chromatograph mass spectrometry (GC/MS) coupled with thermal desorption. Two columns were used: a PLOT column separated compounds lighter than C(6) and a DB-1 column separated C(6)-C(12) compounds. An innovative heart-cut technique based on the Deans switch was configured to combine the two column outflows at the ends of the columns before entering the MS. To prevent the resolved peaks from re-converging after combining, two techniques were attempted (hold-up vs. back-flush) to achieve the intended "delayed" elution of heavier components. Thus, the resulting chromatogram covering the full range of VOCs is a combination of two separate elutions, with the heavier section following the lighter section. With the hold-up method, band-broadening inevitably occurred for the delayed C(6)-C(7) DB-1 compounds while the light compounds eluted from the PLOT column. This broadening problem resulted in peak tailing that was largely alleviated by adding a re-focusing stage while the DB-1 compounds were back-flushed, and this modified technique is referred to as the back-flush method. With this modification, the separation of the C(6)-C(7) compounds improved dramatically, as revealed by the decrease in peak asymmetry (As) and increase in resolution. Linearity and precision for these peaks also improved, yielding R(2) and RSD values better than 0.9990 and 2.8%, respectively.
本研究旨在探讨使用气相色谱-质谱联用仪(GC/MS)结合热解吸技术分析从 C(3)到 C(12)的全范围环境挥发性有机化合物(VOCs)的可行性。使用了两根柱子:一根 PLOT 柱分离轻于 C(6)的化合物,一根 DB-1 柱分离 C(6)-C(12)的化合物。基于 Dean 开关配置了一种创新的切取技术,将两根柱子的流出物在进入 MS 之前在柱子的末端进行合并。为了防止在合并后分离出的峰重新汇聚,尝试了两种技术(保留时间与反吹)来实现较重组分的预期“延迟”洗脱。因此,涵盖全范围 VOCs 的所得色谱图是两个单独洗脱的组合,较重部分紧随较轻部分。采用保留时间法,从 PLOT 柱洗脱的轻化合物与随后洗脱的 DB-1 较重化合物 C(6)-C(7)的峰展宽不可避免。这种展宽问题导致峰拖尾,而在反吹时添加重新聚焦阶段则大大缓解了该问题,该改进技术称为反吹法。通过这种改进,C(6)-C(7)化合物的分离显著改善,表现为峰不对称性(As)降低和分辨率提高。这些峰的线性度和精密度也得到了改善,得到的 R(2)和 RSD 值均优于 0.9990 和 2.8%。