Liquid chromatograph

Patent metadata

Field	Value
Publication number	US-10969368-B2
Application number	US-201716328302-A
Country	US
Kind code	B2
Filing date	Jun 30, 2017
Priority date	Sep 16, 2016
Publication date	Apr 6, 2021
Grant date	Apr 6, 2021

Abstract

The liquid chromatograph is provided with: a first dimension analysis unit; a diluent determination unit configured to determine the composition and flow rate of a diluent for diluting an eluent flowing out of the first dimension analysis unit based on the composition of the eluent flowing from the first dimension analysis unit; and a diluent liquid delivery unit configured to deliver the diluent of the composition determined by the diluent determination unit at the flow rate determined by the diluent determination unit so as to be delivered to the trap column while diluting the eluent flowing from the first dimension analysis unit.

First claim

The invention claimed is:

1. A liquid chromatograph comprising:
a first dimension analysis unit including a mobile phase liquid delivery unit configured to deliver a liquid mixture of plural kinds of solvents as a mobile phase while changing its composition and an analytical column configured to separate a sample injected into a flow path through which the mobile phase flows into components;
a controller comprising a diluent determination unit configured to determine a composition and a flow rate of a diluent for diluting an eluent flowing out of the first dimension analysis unit based on a composition of the eluent;
a trap column configured to trap sample components in the eluent flowing out of the first dimension analysis unit; and
a diluent liquid delivery unit configured to deliver the diluent of a composition determined by the diluent determination unit at a flow rate determined by the diluent determination unit so as to deliver the eluent flowing out of the first dimension analysis unit to the trap column while diluting the eluent;
wherein the first dimension analysis unit includes a detector for detecting separated components; and
wherein the diluent determination unit is configured to specify a component of the eluent based on a gradient program of the mobile phase liquid delivery unit of the first dimension analysis unit and a retention time of a peak of a detection signal of the detector and determine the composition and flow rate of the diluent according to the composition of the eluent.

2. The liquid chromatograph as recited in claim 1 ,
wherein the diluent determination unit is configured to specify the composition of the eluent flowing out of the first dimension analysis unit based on information on a liquid delivery flow rate of each solvent acquired from the mobile phase liquid delivery unit.

3. The liquid chromatograph as recited in claim 1 , wherein:
the controller further comprises a diluent data holding unit configured to hold, as diluent data, a preset correspondence relationship between the composition of the eluent flowing out of the first dimension analysis unit and the composition and flow rate of the diluent corresponding to the composition of the eluent,
wherein the diluent determination unit determines the composition and flow rate of the diluent corresponding to the composition of the eluent flowing out of the first dimension analysis unit based on the diluent data.

4. The liquid chromatograph as recited in claim 3 , wherein in the diluent data holding unit diluent data is prepared so that when the composition of the eluent is specified, the diluent composition and dilution ratio optimal for diluting the eluent are automatically determined.

5. The liquid chromatograph as recited in 4 , wherein the diluent having an appropriate composition and flow rate is automatically delivered from the diluent liquid delivery unit making it unnecessary for a user to perform an analysis to determine the composition and flow rate of the diluent.

6. The liquid chromatograph as recited in claim 1 , further comprising an eluent holding unit that holds eluent flowed out of the first dimension analysis unit and prior to reaching the trap column, which eluent corresponds to a desired peak appearing in a detection signal of the detector of the first dimension analysis unit.

7. The liquid chromatograph as recited in claim 6 , wherein the controller controls operations of the first dimension analysis unit, the eluent holding unit and the diluent liquid delivery unit.

8. The liquid chromatograph as recited in claim 7 , wherein the controller is configured to receive a signal from the detector of the first dimension analysis unit and controls the operation of the eluent holding unit so that desired sample components are held in the eluent holding unit based on the detection signal from the detector.

9. The liquid chromatograph as recited in claim 6 , wherein the diluent determination unit is configured to specify the composition of the eluent when the eluent is held in the eluent holding unit based on data about the liquid mixture of solvents of the mobile phase.

10. The liquid chromatograph as recited in claim 9 , wherein the diluent determination unit is configured to determine the composition and flow rate of the diluent based on the diluent data held in the diluent data holding unit.

11. The liquid chromatograph as recited in claim 10 , wherein the diluent data held in the diluent data holding unit denotes data showing the correspondence relation between the composition of the eluent including the sample components held in the eluent holding unit and the composition and flow rate of the diluent to be provided suitable for the composition.

12. The liquid chromatograph as recited in claim 10 , wherein the diluent data holding unit comprises a look-up table.

13. The liquid chromatograph as recited in claim 6 , wherein the eluent holding unit comprises a plurality of fraction loops for holding a plurality of eluents corresponding to a plurality of detected peaks in a detection signal by the detector.

14. The liquid chromatograph as recited in claim 1 , wherein the controller is a computer.

15. The liquid chromatograph as recited in claim 14 , wherein the diluent determination unit is a function obtained by a CPU executing a program stored in a storage device within the computer, and the diluent data holding unit is a function realized by one area of the storage device.

16. The liquid chromatograph as recited in claim 1 , wherein the diluent liquid delivery unit comprises liquid delivery pumps controlled by the controller so that a desired composition of diluents is mixed, which desired composition is determined by the diluent determination unit according to the composition of the eluent from the first dimension analysis unit.

17. The liquid chromatograph as recited in claim 1 , further comprising a second dimension analysis unit positioned downstream from the trap column.

18. A liquid chromatography method comprising:
in a first dimension analysis unit including a mobile phase liquid delivery unit, delivering a liquid mixture of plural kinds of solvents as a mobile phase while changing its composition and an analytical column configured to separate a sample injected into a flow path through which the mobile phase flows into components;
within a controller comprising a diluent determination unit, determining a composition and a flow rate of a diluent for diluting an eluent flowing out of the first dimension analysis unit based on a composition of the eluent;
trapping sample components in a trap column from the eluent flowing out of the first dimension analysis unit; and
in a diluent liquid delivery unit, delivering the diluent of a determined by the diluent determination unit at a flow rate determined by the diluent determination unit so as to deliver the eluent flowing out of the first dimension analysis unit to the trap column while diluting the eluent;
detecting separated components with a detector that is part of the first dimension analysis unit; and
in the diluent determination unit specifying a component of the eluent based on a gradient program of the mobile phase liquid delivery unit of the first dimension analysis unit and a retention time of a peak of a detection signal of the detector and determining the composition and flow rate of the diluent according to the composition of the eluent.

Assignees

• Shimadzu Corp

Inventors

• YOSHINO Saki

Classifications

• G01N30/32

  of pressure or speed (G01N30/36 takes precedence) · CPC title

• G01N30/34 Primary

  of fluid composition, e.g. gradient (G01N30/36 takes precedence) · CPC title

• G01N30/08 Primary

  using an enricher · CPC title

• G01N30/463

  for multidimensional chromatography · CPC title

• G01N30/84

  Preparation of the fraction to be distributed · CPC title