Subject Area物理化学
Solvent removal interface for micro-column two-dimensional NPLC/RPLC
Guan YF(关亚风)
Conference NameThe 24th MSB 2009
Conference Date2009-10-19
Conference Place中国
Funding Organization大连化物所
AbstractFor the construction of two-dimensional liquid chromatography (LC) system, the compromise of the separation efficiency and selectivity on each dimension is usually unavoidable. Our previous work has reported a two-dimensional LC system constructed by using high temperature normal phase LC (HTNPLC) as the first dimension (1st-D) and a reverse phase LC (RPLC) as the second dimensional (2nd-D) with sample loop-valve interface. The increase of the column temperature could lead to a decrease in retention and the dielectric constant of water, so low organic solvent content of mobile phase of the primary column could be realized, which finally brought the system with improved efficiency of the separation. In our present work, a vacuum assisted dynamic evaporation loop-type valve interface for micro-column two-dimensional NPLC/RPLC was developed and evaluated. The interface removes the solvent of the eluent from the 1st-D (NPLC column of 250 × 4.6 mm I.D. 5 m CN phase) as it is entering the 10 L fraction loop, and retains the non-evaporable analytes on the wall of the loop. Because of the small volume of the loop as compared with the 1 mL/min flow rate, the solvent was dynamically evaporated by vacuum as the solvent entering the loop (evaporation time was equal to fraction collection time). The mobile phase from the 2nd-D (RPLC column of 250 × 4.6 mm I.D. 5 m C18 phase) then enters the loop, and dissolves the analytes deposited on the wall of the loop, and carries them into the 2nd-D column for further separation. The temperature of the loop is maintained at isothermal in a water bath. The dynamic evaporation process can take as long as required, and there is no limit on collection time for the interface. The two dimensions are at their optimal chromatographic conditions by using the system. Furthermore, it was observed that the sample loss due to evaporation in the interface was depended on the boiling point of the compound. For non-volatile sample, the sample loss was negligible. The solvent removal interface solves the problems of solvent exchange, increases the concentrations of the analytes in fractions from the 1st-D, and reduces the transfer volumes from mL down to 10 to 20 L. The chromatographic performance of this 2D-LC system was enhanced without the compromise of separation efficiency and selectivity on each dimension.
Document Type会议论文
Corresponding AuthorGuan YF(关亚风)
Recommended Citation
GB/T 7714
Guan YF. Solvent removal interface for micro-column two-dimensional NPLC/RPLC[C],2009:96/1.
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