Abstract
Herein, we describe a practical online supercritical fluid extraction-supercritical fluid chromatography/mass spectrometry (SFE-SFC/MS) system with an integrated split-flow method and a pre-column trap method that is well suited for the continuous extraction and separation of a wide range of compounds, including hydrophilic ones. Although an SFE-SFC system with a splitting method is already commercially available, in this study, we added some new features to this system: 1) a splitting method that further reduces the amount of extractant introduced into SFC, 2) a trap column, connected before the analytical column, with a different separation mechanism than the analytical column in the system with the splitting method, and 3) a system for calculating the recovery rate of SFE during online SFE-SFC/MS. In the above setup, part of the analyzed extract is introduced into the separation section at a higher split ratio owing to the make-up pump flow rate, thus reducing the distortion of the target analyte peak shape caused by the use of a strong extractant. Furthermore, the separation efficiency is improved by the use of an additional pre-column capable of interacting with compounds weakly retained on the analytical column. Finally, we show that equalization of the SFE and autosampler injection conditions allows evaluation of the recovery rate of SFE during online SFE-SFC/MS.
| Original language | English |
|---|---|
| Pages (from-to) | 161-172 |
| Number of pages | 12 |
| Journal | Journal of Chromatography A |
| Volume | 1592 |
| DOIs | |
| Publication status | Published - May 10 2019 |
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All Science Journal Classification (ASJC) codes
- Analytical Chemistry
- Biochemistry
- Organic Chemistry
Cite this
Development of a practical online supercritical fluid extraction–supercritical fluid chromatography/mass spectrometry system with an integrated split-flow method. / Sakai, Miho; Hayakawa, Yoshihiro; Funada, Yasuhiro; Ando, Takashi; Fukusaki, Eiichiro; Bamba, Takeshi.
In: Journal of Chromatography A, Vol. 1592, 10.05.2019, p. 161-172.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Development of a practical online supercritical fluid extraction–supercritical fluid chromatography/mass spectrometry system with an integrated split-flow method
AU - Sakai, Miho
AU - Hayakawa, Yoshihiro
AU - Funada, Yasuhiro
AU - Ando, Takashi
AU - Fukusaki, Eiichiro
AU - Bamba, Takeshi
PY - 2019/5/10
Y1 - 2019/5/10
N2 - Herein, we describe a practical online supercritical fluid extraction-supercritical fluid chromatography/mass spectrometry (SFE-SFC/MS) system with an integrated split-flow method and a pre-column trap method that is well suited for the continuous extraction and separation of a wide range of compounds, including hydrophilic ones. Although an SFE-SFC system with a splitting method is already commercially available, in this study, we added some new features to this system: 1) a splitting method that further reduces the amount of extractant introduced into SFC, 2) a trap column, connected before the analytical column, with a different separation mechanism than the analytical column in the system with the splitting method, and 3) a system for calculating the recovery rate of SFE during online SFE-SFC/MS. In the above setup, part of the analyzed extract is introduced into the separation section at a higher split ratio owing to the make-up pump flow rate, thus reducing the distortion of the target analyte peak shape caused by the use of a strong extractant. Furthermore, the separation efficiency is improved by the use of an additional pre-column capable of interacting with compounds weakly retained on the analytical column. Finally, we show that equalization of the SFE and autosampler injection conditions allows evaluation of the recovery rate of SFE during online SFE-SFC/MS.
AB - Herein, we describe a practical online supercritical fluid extraction-supercritical fluid chromatography/mass spectrometry (SFE-SFC/MS) system with an integrated split-flow method and a pre-column trap method that is well suited for the continuous extraction and separation of a wide range of compounds, including hydrophilic ones. Although an SFE-SFC system with a splitting method is already commercially available, in this study, we added some new features to this system: 1) a splitting method that further reduces the amount of extractant introduced into SFC, 2) a trap column, connected before the analytical column, with a different separation mechanism than the analytical column in the system with the splitting method, and 3) a system for calculating the recovery rate of SFE during online SFE-SFC/MS. In the above setup, part of the analyzed extract is introduced into the separation section at a higher split ratio owing to the make-up pump flow rate, thus reducing the distortion of the target analyte peak shape caused by the use of a strong extractant. Furthermore, the separation efficiency is improved by the use of an additional pre-column capable of interacting with compounds weakly retained on the analytical column. Finally, we show that equalization of the SFE and autosampler injection conditions allows evaluation of the recovery rate of SFE during online SFE-SFC/MS.
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U2 - 10.1016/j.chroma.2019.01.044
DO - 10.1016/j.chroma.2019.01.044
M3 - Article
VL - 1592
SP - 161
EP - 172
JO - Journal of Chromatography A
JF - Journal of Chromatography A
SN - 0021-9673
ER -