Method of manufacturing substances by supercritical fluid chromatography

A technology of supercritical fluid and chromatography, which is applied in the field of manufacturing substances through supercritical fluid chromatography, can solve the problems of not being suitable for industrial mass production, etc., and achieve the effects of increasing processing capacity, reducing peak tailing, and improving separation performance

Active Publication Date: 2012-05-16
DAICEL CHEM IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, among these techniques, studies have not been conducted considering the improvement of fractionation efficiency, especially the efficiency of fractionating a large amount of targeted substances from a sample by sequentially injecting the sample, and thus, these techniques are not suitable for industrial mass production.

Method used

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  • Method of manufacturing substances by supercritical fluid chromatography
  • Method of manufacturing substances by supercritical fluid chromatography
  • Method of manufacturing substances by supercritical fluid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] use for figure 1 In the supercritical fluid chromatography equipment exemplified in, flurbiprofen was separated from a sample containing flurbiprofen under the following conditions.

[0090] When 6.4 minutes had elapsed after the injection of the sample containing flurbiprofen, 100 μL of ethanol was immediately injected by switching the switching valve, returning the valve to its original state. In this case, the device had a dead volume, so ethanol eluted when 7.3 minutes had elapsed.

[0091] Due to the injection of ethanol, the peak components are extracted rapidly, thus, the peaks are sharpened, and the tailing is reduced and accelerated for 1 minute. The state of the peak is shown in figure 2 and image 3 .

[0092] Column: CHIRALPAK AD-H (0.46×25 cm), manufactured by DAICEL CHEMICAL INDUSTRIES, LTD.

[0093] Mobile phase: CO 2 / EtOH=95 / 5

[0094] Flow rate of mobile phase: 4mL / min

[0095] Temperature: 25°C

[0096] Pressure: 10MPa

[0097] Detection: 2...

Embodiment 2

[0102] Similar to Example 1, use in figure 1 The supercritical fluid chromatography equipment exemplified in the following conditions separates benzoin diethyl ether from a sample containing benzoin diethyl ether.

[0103] When 3.2 minutes had elapsed after the injection of the sample containing benzoin ether, 300 μL of tetrahydrofuran (THF) was immediately injected by switching the switching valve, returning the valve to its original state. In this case, the device had a dead volume, so THF eluted when 4.1 minutes had elapsed.

[0104] Due to the injection of THF, the peak components are extracted rapidly, thus, the peaks are sharpened and the tailing is reduced and accelerated for 1 minute. The state of the peak is shown in Figure 4 and Figure 5 .

[0105] Column: CHIRALPAK IA (0.46×25 cm), manufactured by DAICEL CHEMICAL INDUSTRIES, LTD.

[0106] Mobile phase: CO 2 / THF=90 / 10

[0107] Flow rate of mobile phase: 4mL / min

[0108] Temperature: 25°C

[0109] Pressur...

Embodiment 2

[0115] Similar to Example 2-(1), the difference is that methanol is used instead of THF as the solvent for injection, and benzoin ether is separated from the sample containing benzoin ether.

[0116] Due to the injection of methanol, the peak fractions are extracted rapidly, thus, the peaks are sharpened and the tailing is reduced and accelerated for 2 minutes. The state of the peak is shown in Figure 4 and Figure 5 .

[0117] (Reference Example 1)

[0118] The method for changing the composition of the mobile phase according to the present invention is applied to high performance liquid chromatography (HPLC), and under the following conditions, trans-stilbene oxide (t-SO) is removed from the sample containing t-SO separate.

[0119] When 5.8 minutes had elapsed after injection of the t-SO-containing sample, 30 μL of n-hexane / 2-propanol (IPA) was immediately injected by switching the switching valve, returning the valve to its initial state. In this case, the device had a...

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Abstract

Provided is a method of manufacturing target substances with use of supercritical fluid chromatography, by which the following are achieved: solution of a problem at the time of sequential injections of samples containing the target substances; an increase of a treatment amount of separation per unit time; and improvement of efficiency in separation. The method includes the steps of: injecting the sample containing the target substances into a mobile phase; and returning composition of the mobile phase to a pre-change state after changing the composition of the mobile phase.; The step of returning the composition of the mobile phase to the pre-change state after changing the composition of the mobile phase is performed during a period of time from detection of a peak of one of the target substances which is eluted latest from a column among the target substances separated by the supercritical fluid chromatography apparatus to injection of the next sample, whereby the problem is solved.

Description

technical field [0001] The present invention relates to a method of producing a substance by supercritical fluid chromatography and a supercritical fluid chromatography device. Background technique [0002] In supercritical fluid chromatography equipment, a supercritical fluid is used as the mobile phase. Supercritical fluids have higher diffusivity and lower viscosity than ordinary solvents. Therefore, by using a supercritical fluid chromatography device, for example, optical isomers that are difficult to separate can be separated at high speed. [0003] In such a supercritical fluid chromatography apparatus, a supercritical fluid formed of carbon dioxide or the like is used as a mobile phase, and after injecting a sample into the mobile phase and dissolving each component of the sample in the mobile phase, by adjusting The pressure, temperature, etc. of the mobile phase separate the components of the sample in the mobile phase. Alternatively, a mobile phase is formed by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/34B01D15/40
CPCB01D15/40B01D15/166G01N30/34G01N30/84
Inventor 宫泽贤一郎石黑武
Owner DAICEL CHEM IND LTD
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