Australian Centre for Research on Separation Science, University of Tasmania, Hobart, Tasmania, Australia.
J Sep Sci. 2013 Sep;36(17):2738-45. doi: 10.1002/jssc.201300383. Epub 2013 Jul 26.
A multidimensional gas chromatographic approach using planar microfluidic devices for Deans switching has been developed and implemented for the characterization of sterically hindered phenolic compounds used as antioxidants in fuels. Detection and quantitation was conducted with MS in selected ion monitoring mode. A complete analysis is conducted in less than 15 min with precision greater than 5.5% at 1 and 25 ppm w/w (ppm(w)). LODs of 50 ppb w/w (ppb(w)) or better in selected ion monitoring mode and a linear range of 100 ppb(w) to 100 ppm(w) with a correlation coefficient greater than 0.998 were attained for all analytes. Unique to this analytical configuration is the use of a mass spectrometer capable of monitoring the column effluent from either dimension by incorporating a high-temperature rotary valve and a three-port planar microfluidic device. High-molecular-weight (C25-C40) fuel contaminants eluting from the first column can be selectively sent to the mass spectrometer for profile characterization in scan mode. These compounds would otherwise be retained substantially by the low-phase-ratio analytical column employed in the second dimension.
已经开发并实施了一种使用平面微流控器件进行 Dean 切换的多维气相色谱方法,用于表征用作燃料抗氧化剂的空间位阻酚类化合物。采用 MS 在选择离子监测模式下进行检测和定量。在不到 15 分钟的时间内完成完整分析,在 1 和 25 ppm w/w(ppm(w))时的精密度大于 5.5%。在选择离子监测模式下,所有分析物的 LODs 均为 50 ppb w/w(ppb(w))或更好,线性范围为 100 ppb(w)至 100 ppm(w),相关系数大于 0.998。这种分析配置的独特之处在于使用了一种能够通过结合高温旋转阀和三端口平面微流控器件从两个维度监测柱流出物的质谱仪。从第一根柱子洗脱的高分子量(C25-C40)燃料污染物可以选择性地发送到质谱仪进行扫描模式下的轮廓表征。否则,这些化合物将被第二维度中使用的低相比率分析柱基本上保留。