# US 12,222,333 B2 · Preparative chromatograph and preparative method using preparative chromatograph

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- Number: US 12,222,333 B2
- Document ID: US12222333B2
- Status: Granted
- Kind: B2
- Application number: 17/725,892
- Filed: 2022-04-21
- Published: 2022-10-27
- Granted: 2025-02-11
- Earliest claimed: 2021-04-26
- Assignees: Shimadzu Corporation
- Applicants: Shimadzu Corporation
- Inventors: Kosuke Nakajima
- Web page: https://patentgrep.com/patent/US12222333B2

## CPC

- G01N 30/14: by elimination of some components
- B01D 15/40: using supercritical fluid as mobile phase or eluent
- G01N 30/32: of pressure or speed (G01N30/36 takes precedence)
- G01N 30/38: Flow patterns
- G01N 30/82: Automatic means therefor
- G01N 2030/027: {Liquid chromatography}
- G01N 2030/326: {pumps}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)

## Abstract

A preparative chromatograph includes a separation column, and a detector provided downstream of the separation column. Furthermore, the preparative chromatograph includes a fractionator including a gas-liquid separator configured to separate a fluid containing components of a sample into a gas and a liquid, the fractionator being provided downstream of the detector. The preparative chromatograph is configured to supply carbon dioxide to a flow path between the separation column and the fractionator.

## Claims

### Claim 1

A preparative chromatograph comprising:
a separation column configured to separate components of a sample;
a detector provided downstream of the separation column, the detector being configured to detect the components of the sample separated by the separation column; and
a fractionator including a gas-liquid separator configured to separate a fluid containing the components of the sample into a gas and a liquid, the fractionator being provided downstream of the detector, the fractionator being configured to fractionate the components of the sample separated by the separation column based on a detection result of the detector;
wherein
the preparative chromatograph is configured to supply carbon dioxide to a flow path between the separation column and the fractionator.

### Claim 2 (depends on 1)

The preparative chromatograph according to claim 1, configured to switch between a liquid chromatograph mode in which the sample is sent together with a liquid to the separation column and a supercritical fluid chromatograph mode in which the sample is sent together with carbon dioxide in a supercritical state to the separation column; and
configured to supply the carbon dioxide to the flow path between the separation column and the fractionator in the liquid chromatograph mode.

### Claim 3 (depends on 2)

The preparative chromatograph according to claim 2, further comprising:
a first pump configured to supply the carbon dioxide to a flow path;
a back pressure regulator provided between the detector provided downstream of the separation column and the gas-liquid separator, the back pressure regulator being configured to adjust a pressure in a flow path on the detector side; and
a flow path switching valve configured to switch a supply destination of the carbon dioxide supplied from the first pump between a flow path between the back pressure regulator and the fractionator and a flow path upstream of the separation column.

### Claim 4 (depends on 3)

The preparative chromatograph according to claim 3, further comprising:
a second pump configured to supply a liquid to a flow path; wherein
the flow path switching valve is configured to switch a supply destination of the liquid supplied from the second pump between the flow path upstream of the separation column and the flow path between the back pressure regulator and the fractionator.

### Claim 5 (depends on 4)

The preparative chromatograph according to claim 4, further comprising:
a controller configured or programmed to control driving of the first pump; wherein
the controller is configured or programmed to control switching of the supply destination of the carbon dioxide supplied from the first pump by the flow path switching valve based on a switching operation of a user.

### Claim 6 (depends on 5)

The preparative chromatograph according to claim 5, wherein
the controller is configured or programmed to control the switching of the supply destination of the carbon dioxide supplied from the first pump by the flow path switching valve based on the switching operation of the user to supply the carbon dioxide supplied from the first pump to the flow path between the back pressure regulator and the fractionator in the liquid chromatograph mode and supply the carbon dioxide in the supercritical state supplied from the first pump to the flow path upstream of the separation column in the supercritical fluid chromatograph mode.

### Claim 7 (depends on 6)

The preparative chromatograph according to claim 6, further comprising:
a third pump configured to supply a liquid to the flow path upstream of the separation column; wherein
the controller is configured or programmed to control switching of the supply destination of the liquid supplied from the second pump by the flow path switching valve based on a switching operation of the user to mix the liquid supplied from the second pump and the liquid supplied from the third pump in the flow path upstream of the separation column in the liquid chromatograph mode and supply the liquid supplied from the second pump to the flow path between the back pressure regulator and the fractionator in the supercritical fluid chromatograph mode.

### Claim 8

A preparative method using a preparative chromatograph, the preparative method comprising:
separating components of a sample by a separation column;
detecting the components of the sample separated by the separation column;
fractionating the components of the sample separated by the separation column based on a detection result obtained by the detecting;
separating a fluid containing the components of the sample fractionated in the fractionating into a gas and a liquid; and
supplying carbon dioxide to the fluid containing the components of the sample before the fractionating of the components of the sample separated by the separation column.

### Claim 9 (depends on 8)

The preparative method according to claim 8, further comprising:
switching a supply destination of the carbon dioxide between a flow path upstream of the separation column and a flow path downstream of the separation column to switch between a liquid chromatograph mode in which the sample is sent together with a liquid to the separation column and a supercritical fluid chromatograph mode in which the sample is sent together with carbon dioxide in a supercritical state to the separation column.