Meziani Amel, Verloy Sandrien, Ferroukhi Ouassila, Roca Sebastien, Curat Aurelien, Tisse Severine, Peulon-Agasse Valerie, Gardeniers Han, Desmet Gert, Cardinael Pascal
Univ Rouen Normandie, FR CNRS 3038, SMS, UR3233, Rouen F-76000, France.
Laboratoire de Chromatographie, Faculté de Chimie, USTHB, BP 32 EL-Alia, Alger 16111, Algeria.
Anal Chem. 2022 Oct 18;94(41):14126-14134. doi: 10.1021/acs.analchem.2c01264. Epub 2022 Oct 4.
The present study investigated the use of a dedicated gas chromatography (GC) column ( = 70 cm, 75 μm deep, and 6.195 mm wide) with radially elongated pillars (REPs) as the second column in a comprehensive two-dimensional gas chromatography (GC × μGC) system. Three stationary phases [apolar polydimethylsiloxane (PDMS), medium polar room-temperature ionic liquid (RTIL) based on monocationic phosphonium, and polar polyethylene glycol (PEG-1000)] have been coated using the static method at constant pressure or using an original vacuum pressure program (VPP) from 400 to 4 mbar. The best efficiency reached up to = 62,000 theoretical plates for a film thickness of 47 nm at 100 °C for an -octane peak ( = 0.16) at an optimal flow rate of 4.8 mL/min. The use of the VPP improved the efficiency by approximately 15%. Efficiencies up to 28,000 and 47,000 were obtained for PEG-1000 and RTIL, respectively. A temperature-programmed separation of a mixture of 11 volatile compounds on a PDMS-coated chip was obtained in less than 36 s. The PDMS-, PEG-1000-, and RTIL-coated chips were tested as the second column using a microfluidic reverse fill/flush flow modulator in a GC × μGC system. The REP columns were highly compatible with the operating conditions in terms of flow rate and with more than 30,000 plates for the -octane peak. Moreover, a commercial solvent called containing alkanes and aromatic compounds was injected in three sets of columns in normal and reverse modes, demonstrating the great potential of the chip as a second-dimension separation column.
本研究考察了在全二维气相色谱（GC×μGC）系统中，使用带有径向拉长柱（REP）的专用气相色谱（GC）柱（柱长 = 70 cm，深度 = 75 μm，宽度 = 6.195 mm）作为第二根色谱柱的情况。采用静态法在恒压下或使用从400至4 mbar的原始真空压力程序（VPP）涂覆了三种固定相[非极性聚二甲基硅氧烷（PDMS）、基于单阳离子鏻的中等极性室温离子液体（RTIL）和极性聚乙二醇（PEG - 1000）]。在100℃下，对于辛烷峰（保留时间 = 0.16），当膜厚为47 nm且最佳流速为4.8 mL/min时，最佳柱效达到了62,000理论塔板数。使用VPP可使柱效提高约15%。PEG - 1000和RTIL分别获得了高达28,000和47,000的柱效。在不到36 s的时间内，在涂覆PDMS的芯片上实现了11种挥发性化合物混合物的程序升温分离。在GC×μGC系统中，使用微流控反向填充/冲洗流量调制器，对涂覆有PDMS、PEG - 1000和RTIL的芯片作为第二根色谱柱进行了测试。REP柱在流速方面与操作条件高度兼容，对于辛烷峰柱效超过30,000塔板数。此外，一种含有烷烃和芳香族化合物的市售溶剂 在三组色谱柱中以正反向模式进样，证明了该芯片作为二维分离柱具有巨大潜力。
