Dow Chemical Canada ULC , Highway 15 , Fort Saskatchewan , Alberta T8L 2P4 , Canada.
Australian Centre for Research on Separation Science (ACROSS) , University of Tasmania , Private Bag 75 , Hobart , Tasmania 7001 , Australia.
Anal Chem. 2019 Sep 3;91(17):11223-11230. doi: 10.1021/acs.analchem.9b02159. Epub 2019 Aug 20.
A 3D-printed microreactor for post-column reactions was successfully integrated with comprehensive two -dimensional gas chromatography. A two-stage post-column reaction provided a carbon-independent response, enhanced the flame ionization detection uniformity, and improved the detector sensitivity. These enhancements are critical to overcome challenges in analyses using comprehensive two-dimensional gas chromatography and flame ionization detection, which aim to separate and quantify multiple components. Post-column reaction flame ionization detection eliminated the requirement of multilevel and multicompound calibration, it enabled the determination of target analytes with a single-carbon-containing calibration compound with an accuracy of ±10%, and it improved the sensitivity for compounds that were not efficiently ionized by flame ionization detection. Extra column band-broadening caused by the incorporation of the 3D-printed microreactor was minimized using optimized reactor operating parameters and intercolumn connectivity. Chromatographic fidelity was in the practical domain of comprehensive 2D gas chromatography. Typical peak widths at half-height using the described approach ranged from 165 to 235 ms for probe compounds with retention factors spanning 5 < < 40.
成功地将用于柱后反应的 3D 打印微反应器与全二维气相色谱集成。两段柱后反应提供了与碳无关的响应，增强了火焰离子化检测的均匀性，并提高了检测器的灵敏度。这些增强对于克服使用全二维气相色谱和火焰离子化检测进行分析的挑战至关重要，这些挑战旨在分离和定量多种成分。柱后反应火焰离子化检测消除了多级和多化合物校准的要求，它能够使用单一含碳校准化合物准确地测定目标分析物，准确度为 ±10%，并提高了火焰离子化检测效率不高的化合物的灵敏度。通过优化反应器操作参数和柱间连接，最大限度地减少了 3D 打印微反应器引入的额外柱带展宽。色谱保真度在全二维气相色谱的实际范围内。使用描述的方法，探针化合物的典型半峰宽在 165 到 235 毫秒之间，保留因子跨度为 5 < < 40。
