Development of comprehensive two‐dimensional packed column supercritical fluid chromatography

Abstract

Development of comprehensive two-dimensional packed column supercritical fluid chromatographyA comprehensive two-dimensional supercritical fluid chromatographic system with conventional packed columns was developed. The system used a computer-controlled ten-port valve, a capillary trap, and a restrictor. The mobile phase was pure carbon dioxide. The first dimension column was operated under constant pressure in the stopped-flow mode, while the second dimension column was operated in the constant flow mode. The effluent of the first column was depressurized through the restrictor and solute was trapped within the capillary trap. Then the trapped solute was transferred into the second column by switching the valve. Since the solute transfer process is very rapid, the valve can be switched back after a short injection period in order to collect next fraction. This allowed the sampling time to be changed without changing any of the other conditions, such as the second dimension run time. The system was applied to the separation of triglycerides in fats and oils. Separations were performed using the same ODS packing materials for both columns, and the first column was operated under subcritical conditions and the second column under supercritical conditions.

Development of Supercritical Fluid Extraction Coupled to Comprehensive Two-dimensional Supercritical Fluid Chromatography (SFE-SFC¥SFC)

“…A fundamental study on the trapping efficiency was reported in our previous paper. 9 By switching valve-1 to position-B, the trapped extracts were redissolved into liquid CO2 and transferred onto column-1, and then separated. At this moment, the extraction chamber flow was stopped, but the pressure was maintained.…”

“…8 In our previous work, SFC×SFC with packed columns as well as capillary columns were developed. [9][10][11] In this work we developed a SFE-SFC×SFC system, which has both advantages of SFE-SFC and SFC×SFC.…”

Comprehensive two-dimensional separation for the analysis of alkylphenol ethoxylates employing hydrophilic interaction chromatography coupled with ion mobility-mass spectrometry

“…It is recommended that the two dimensions be connected in an on-line manner, referred to as a comprehensive two-dimensional separation, rather than in an off-line or heart-cut manner, in order to approach the ideal multiplicative total of peak capacity. To date, a wide variety of separation techniques have been mutually interfaced to construct comprehensive two-dimensional separation systems [34][35][36][37]. Currently, LC in conjunction with ion mobility-mass spectrometry (IM-MS) is becoming increasingly popular for complex mixture analysis, due to complementary separation steps and elevated peak capacity.…”

Comprehensive Two-Dimensional Separation of Hydroxylated Polybrominated Diphenyl Ethers by Ultra-Performance Liquid Chromatography Coupled with Ion Mobility-Mass Spectrometry

“…It is recommended that the two dimensions be connected in an on-line manner, referred to as a comprehensive two-dimensional separation, rather than in an off-line or heart-cut manner, in order to approach the ideal multiplicative total of peak capacity. To date, a broad range of separation techniques such as LC, GC, capillary electrophoresis (CE), and supercritical fluid chromatography (SFC) have been mutually interfaced to construct comprehensive two-dimensional separation systems [31][32][33][34][35][36][37]. Currently, LC in conjunction with ion mobility separation and MS measurement is becoming increasingly popular for complex mixture analysis, due to complementary separation steps and elevated peak capacity.…”