Format

Send to

Choose Destination
J Chromatogr A. 2017 Sep 15;1515:218-231. doi: 10.1016/j.chroma.2017.07.077. Epub 2017 Jul 25.

Development of a split-flow system for high precision variable sample introduction in supercritical fluid chromatography.

Author information

1
Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan; Miyazaki Agricultural Research Institute, 5805 Shimonaka, Sadowara-cho, Miyazaki, Miyazaki 880-0212, Japan.
2
Shimadzu Corporation, 1, Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 604-8511, Japan.
3
General Incorporated Association Food Research Organization, 5805 Shimonaka, Sadowara-cho, Miyazaki, Miyazaki 880-0212, Japan.
4
Department of Biotechnology, Graduate School of Engineering, Osaka University, 2-1 Yamadaoka, Suita, Osaka 565-0871, Japan.
5
Division of Metabolomics, Medical Institute of Bioregulation, Kyushu University 3-1-1 Maidashi, Higashi-ku, Fukuoka 812-8582, Japan. Electronic address: bamba@bioreg.kyushu-u.ac.jp.

Abstract

In this study, we propose a novel variable sample injection system based on full-loop injection, named the split-flow sample introduction system, for application in supercritical fluid chromatography (SFC). In this system, the mobile phase is split by the differential pressure between two back pressure regulators (BPRs) after full-loop injection suitable for SFC, and this differential pressure determines the introduction rate. Nine compounds with a wide range of characteristics were introduced with high reproducibility and universality, confirming that a robust variable sample injection system was achieved. We also investigated the control factors of our proposed system. Sample introduction was controlled by the ratio between the column-side pressure drops in splitless and split flow, ΔPcolumnsideinsplitless and ΔPcolumnsideinsplit, respectively, where ΔPcolumnsideinsplitless is related to the mobile phase flow rate and composition and the column resistance. When all other conditions are kept constant, increasing the make-up flow induces an additional pressure drop on the column side of the system, which leads to a reduced column-side flow rate, and hence decreased the amount of sample injected, even when the net pressure drop on the column side remains the same. Thus, sample introduction could be highly controlled at low sample introduction rate, regardless of the introduction conditions. This feature is advantageous because, as a control factor, the solvent in the make-up pump is independent of the column-side pressure drop.

KEYWORDS:

Back pressure regulator; Make-up pump; Sample injection; Split-flow; Supercritical fluid chromatography

PMID:
28802523
DOI:
10.1016/j.chroma.2017.07.077
[Indexed for MEDLINE]

Supplemental Content

Full text links

Icon for Elsevier Science
Loading ...
Support Center