CN112740029A - Low-pressure gradient liquid feeding system and liquid chromatograph - Google Patents

Low-pressure gradient liquid feeding system and liquid chromatograph Download PDF

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Publication number
CN112740029A
CN112740029A CN201880097859.5A CN201880097859A CN112740029A CN 112740029 A CN112740029 A CN 112740029A CN 201880097859 A CN201880097859 A CN 201880097859A CN 112740029 A CN112740029 A CN 112740029A
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liquid
mixing ratio
liquids
solvent
pressure gradient
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CN112740029B (en
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大友伊织
渡辺覚
舎川知広
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Shimadzu Corp
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Shimadzu Corp
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/32Control of physical parameters of the fluid carrier of pressure or speed
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/26Conditioning of the fluid carrier; Flow patterns
    • G01N30/28Control of physical parameters of the fluid carrier
    • G01N30/34Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/50Conditioning of the sorbent material or stationary liquid

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The low-pressure gradient liquid feeding system 2 of the present invention includes: three or more liquid supply channels (8, 10, 12, 14) for drawing liquids from containers containing the liquids, respectively; a liquid feeding pump (18) for sucking the liquid from the container through the liquid supply channels (8, 10, 12, 14) and feeding the liquid; a switching mechanism (16) which is interposed between the three or more liquid supply channels (8, 10, 12, 14) and the liquid sending pump (18) and selectively switches one liquid supply channel, which communicates with the liquid sending pump (18), from among the three or more liquid supply channels (8, 10, 12, 14); a mixer (20) for mixing the liquid pumped by the liquid-feeding pump (18); a composition setting unit (26) configured to set a mixing ratio per time period of three or more liquids mixed in the mixer (20) based on a user input; and a control unit (24) configured to control a switching operation of the switching mechanism (16) so that a mixing ratio per time period of the three or more liquids mixed in the mixer is set to the mixing ratio set by the composition setting unit (26).

Description

Low-pressure gradient liquid feeding system and liquid chromatograph
Technical Field
The invention relates to a low-pressure gradient liquid feeding system and a liquid chromatograph.
Background
In liquid chromatography, a mixed liquid of a plurality of liquids is often used as a mobile phase, and gradient analysis is often performed while changing the mixing ratio of the liquids constituting the mobile phase for each period of time.
In order to perform gradient analysis, a gradient program that specifies how the composition of the mobile phase changes with time needs to be set in the system in advance. However, if the number of liquids used for gradient analysis is large, the calculation of how to change the mixing ratio of the liquids becomes complicated, and the setting of the gradient program becomes complicated.
In order to reduce the complexity of the program setting, it has been proposed that the system side automatically calculates the mixing ratio of each liquid for setting the characteristics (for example, the pH value) of the mobile phase in each time zone to the characteristics set by the user (patent document 1).
[ Prior art documents ]
[ patent document ]
Patent document 1: WO2015/172011A1
Disclosure of Invention
[ problems to be solved by the invention ]
As the gradient analysis method, there are a high-pressure gradient method and a low-pressure gradient method. The high-pressure gradient system is a system that uses a plurality of liquid-feeding pumps to feed a plurality of liquids at the same time. On the other hand, the low-pressure gradient system is a system in which one liquid feed pump is used and the liquid fed by the liquid feed pump is switched by a switching valve, and only one type of liquid can be fed at the same time.
In the conventional low-pressure gradient system, only a gradient program for gradient analysis using two liquids can be set. Therefore, for example, when a liquid such as a buffer is used in addition to the water-based solvent and the organic solvent, it is necessary to mix the liquid such as the buffer in the solvent in advance to adjust the pH.
Accordingly, an object of the present invention is to provide a novel low-pressure gradient system that can perform gradient analysis using three or more liquids.
[ means for solving problems ]
A first aspect of the present invention is a low-pressure gradient liquid feeding system including: three or more liquid supply channels for drawing liquids from containers containing the liquids, respectively; a liquid feeding pump for sucking the liquid from the container through the liquid supply passage and feeding the liquid; a switching mechanism that is interposed between the three or more liquid supply flow paths and the liquid sending pump, and that selectively switches one liquid supply flow path that communicates with the liquid sending pump from among the three or more liquid supply flow paths; a mixer for mixing the liquid drawn by the liquid-sending pump; a composition setting unit configured to set a mixing ratio per time period of three or more liquids mixed in the mixer based on a user input; and a control unit configured to control a switching operation of the switching mechanism so that a mixing ratio per time period of the three or more liquids mixed in the mixer is set to the mixing ratio set by the composition setting unit.
A second aspect of the present invention is a liquid chromatograph including: the low-pressure gradient liquid feeding system; and an analysis unit that performs separation and analysis of a sample on a channel through which the mobile phase flows, using the liquid mixture of the liquids sent by the low-pressure gradient liquid sending system as the mobile phase.
[ Effect of the invention ]
A low-pressure gradient liquid feeding system according to a first aspect of the present invention includes: a composition setting unit configured to set a mixing ratio per time period of three or more liquids mixed in the mixer based on a user input; and a control unit configured to control a switching operation of the switching mechanism so that a mixing ratio per time period of the three or more liquids mixed in the mixer is set to the mixing ratio set by the composition setting unit, whereby a novel low-pressure gradient liquid feeding system capable of realizing gradient analysis using the three or more liquids can be provided.
In the liquid chromatograph according to the second aspect of the present invention, since the mobile phase is transported by using the low-pressure gradient liquid feeding system, a novel analysis system of a low-pressure gradient method that can perform gradient analysis using three or more liquids can be provided.
Drawings
Fig. 1 is a schematic configuration diagram showing an embodiment of a low-pressure gradient liquid feeding system and a liquid chromatograph.
Fig. 2 is a diagram showing an example of setting of the composition of the first solvent and the composition of the second solvent in the above example.
Fig. 3 is a diagram showing an example of the composition setting of the mobile phase in the above embodiment.
Detailed Description
Hereinafter, an embodiment of the low-pressure gradient liquid feeding system and the liquid chromatograph will be described with reference to the drawings.
As shown in fig. 1, the liquid chromatograph 1 of the embodiment mainly includes a low-pressure gradient liquid feeding system 2 and an analysis unit 4.
The low-pressure gradient liquid feeding system 2 has a gradient function of feeding a mixed liquid including three or more liquids as a mobile phase to the analysis channel 6 and changing the composition of the mobile phase with time. In the embodiment, the low-pressure gradient liquid feeding system 2 can perform gradient liquid feeding using four liquids (liquid 1 to liquid 4).
The low-pressure gradient liquid feeding system 2 comprises: four liquid supply flow paths 8, 10, 12, 14; a switching valve 16; a liquid-feeding pump 18; a mixer 20; and a control device 22. The liquid supply channel 8, the liquid supply channel 10, the liquid supply channel 12, and the liquid supply channel 14 are channels for drawing liquid from containers that store the liquids 1 to 4, respectively. The liquid supply channel 8, the liquid supply channel 10, the liquid supply channel 12, and the liquid supply channel 14 are connected to different selection ports of the switching valve 16. The suction side of the liquid sending pump 18 is connected to the common port of the switching valve 16. That is, the switching valve 16 constitutes a switching mechanism that is present between the liquid-sending pump 18 and the four liquid- supply flow paths 8, 10, 12, and 14 in an isolated manner and that selectively switches the liquid-supply flow paths that communicate with the liquid-sending pump 18.
The switching mechanism is not limited to the switching valve 16. For example, the switching mechanism may be configured to: in place of the switching valve 16, shut-off valves are provided in each of the liquid supply channel 8, the liquid supply channel 10, the liquid supply channel 12, and the liquid supply channel 14, and the liquid sending pump 18 is brought into fluid communication with any one of the liquid supply channels by opening any one of the shut-off valves. In this case, the shutoff valves provided in the liquid supply flow paths 8, 10, 12, and 14 constitute a switching mechanism for selectively switching the liquid supply flow paths communicating with the liquid sending pump 18. The switching mechanism may have any configuration as long as it can selectively switch the liquid supply flow path that is in fluid communication with the liquid sending pump 18.
The mixer 20 is provided downstream of the liquid-feeding pump 18, and the liquid fed by the liquid-feeding pump 18 is mixed in the mixer 20. The mixer 20 may be provided upstream of the liquid-feeding pump 18.
The operations of the switching valve 16 and the liquid-feeding pump 18 are controlled by a control device 22. The control device 22 is implemented by an electronic circuit having a Central Processing Unit (CPU) or a memory device. The control device 22 includes a control unit 24, a composition setting unit 26, and a mixing ratio calculation unit 28 as its functions. The control unit 24, the composition setting unit 26, and the mixing ratio calculation unit 28 are functions obtained by the CPU executing a specific program.
The control unit 24 is configured to: the switching operation of the switching valve 16 is controlled so that the composition of the mobile phase flowing through the analysis flow path 6, that is, the mixing ratio of the liquids 1 to 4 mixed in the mixer 20 is a ratio following a preset gradient program. Here, the gradient program is a program showing how the composition of the mobile phase changes with time from the start of analysis.
The composition setting unit 26 sets a gradient program based on a user input. As the gradient program set by the composition setting unit 26, the following programs can be cited: the four liquids of the liquids 1 to 4 are divided into two groups of a first group and a second group, and the mixing ratio of the first solvent including the liquid belonging to the first group and the second solvent including the liquid belonging to the second group is changed with time.
In this case, the composition setting unit 26 receives the composition of the first solvent and the composition of the second solvent as illustrated in fig. 2, and sets the received compositions as the first solvent composition and the second solvent composition, respectively. Further, the composition setting unit 26 determines how the mixture ratio of the first solvent and the second solvent is changed over time, that is, determines the mixture ratio of the first solvent and the second solvent per time period based on the user input, thereby setting the gradient program as illustrated in fig. 3.
The mixing ratio calculation unit 28 is configured to: the mixing ratio of the liquids 1 to 4 in the mobile phase for each time period is calculated from the first solvent composition, the second solvent composition, and the gradient program set by the composition setting unit 26.
The calculation of the mixing ratio by the mixing ratio calculation section 28 will be described by taking an example of a time period in which the second solvent concentration is 60% in the gradient program of fig. 3, using the numerical values illustrated in fig. 2 and 3. The mixing ratio of the first solvent (liquid 1: liquid 2: 9: 1) and the mixing ratio of the second solvent (liquid 3: liquid 4: 1) in the mobile phase of the period were 40% and 60%. Therefore, the mixing ratio of the liquid 1 to the liquid 4 in the mobile phase is calculated as follows. In addition, the ratio here is a volume ratio.
Liquid 1: 40%. times.90%. 36%
Liquid 2: 40%. times.10%. 4%
Liquid 3: 60%. times.50%. 30%
Liquid 4: 60%. times.50%. 30%
Thus, the composition of the mobile phase in the time period becomes liquid 1: liquid 2: liquid 3: liquid 4-36: 4: 30: 30.
the control unit 24 controls the switching operation of the switching device 16 so that the composition of the mixed liquid mixed by the mixer 20 in each time zone becomes the mixing ratio of the liquids 1 to 4 in each time zone calculated by the mixing ratio calculation unit 28.
As described above, in setting the gradient program, as illustrated in fig. 3, the user can set the gradient program for low-pressure gradient analysis using four liquids in accordance with a procedure which is as complicated as the procedure for low-pressure gradient analysis using two liquids. Thereby, a low pressure gradient analysis using a plurality of liquids can be realized without imposing a cumbersome setting procedure on the user.
Returning to fig. 1, the explanation of an embodiment of the liquid chromatograph is continued, and the analysis unit 4 includes a sample injection unit 30, a separation column 32, and a detector 34. The sample injection unit 30 has a function of injecting a sample into the analysis channel 6, and is, for example, an autosampler (autosampler). The separation column 32 is used to separate the sample injected into the analysis channel 6 by the sample injection unit 30 into components. The detector 34 is used to detect the sample component separated by the separation column 32.
In the embodiment described above, the low-pressure gradient analysis is performed using four liquids, i.e., the liquid 1 to the liquid 4, but the present invention is not limited thereto, and any number of liquids may be used for the low-pressure gradient analysis as long as three or more liquids are used.
In the above-described embodiment, the first group is made to contain two liquids, i.e., the liquid 1 and the liquid 2, and the second group is made to contain two liquids, i.e., the liquid 3 and the liquid 4.
That is, the embodiments of the present invention are described below.
A first embodiment of the present invention is a low-pressure gradient liquid feeding system (2) including: three or more liquid supply channels (8; 10; 12; 14) for drawing liquids from containers containing the liquids, respectively; a liquid feeding pump (18) for sucking the liquid from the container through the liquid supply passage (8; 10; 12; 14) and feeding the liquid; a switching mechanism (16) which is interposed between the three or more liquid supply flow paths (8; 10; 12; 14) and the liquid sending pump (18) and selectively switches one liquid supply flow path communicating with the liquid sending pump (18) from among the three or more liquid supply flow paths (8; 10; 12; 14); a mixer (20) for mixing the liquid pumped by the liquid-feeding pump (18); a composition setting unit (26) configured to set a mixing ratio per time period of three or more liquids mixed in the mixer (20) based on a user input; and a control unit (24) configured to control a switching operation of the switching mechanism (16) so that a mixing ratio per time period of the three or more liquids mixed in the mixer is set to the mixing ratio set by the composition setting unit (26).
According to the first embodiment, it comprises: a composition setting unit (26) configured to set a mixing ratio per time period of three or more liquids to be mixed in the mixer, based on a user input; and a control unit (24) configured to control the switching operation of the switching mechanism (16) so as to set the mixing ratio per time period of the three or more liquids mixed in the mixer to the mixing ratio set by the composition setting unit (26), whereby a novel low-pressure gradient liquid feeding system capable of realizing gradient analysis using three or more liquids can be provided.
In the first embodiment, the composition setting unit (26) may be configured to: the three or more liquids are divided into two groups including a first group and a second group, a composition of a first solvent including a liquid belonging to the first group and a composition of a second solvent including a liquid belonging to the second group are set, and a mixing ratio per period of time of the first solvent and the second solvent is set. In this case, the low-pressure gradient liquid feeding system (2) includes a mixing ratio calculation unit (28), and the mixing ratio calculation unit (28) is configured to: the control unit (24) may be configured to calculate a mixing ratio of the three or more liquids per time period using the composition of the first solvent, the composition of the second solvent, and the mixing ratio of the first solvent and the second solvent per time period, which are set by the composition setting unit (26), and to: the switching operation of the switching mechanism (16) is controlled so that the mixing ratio of the three or more liquids mixed in the mixer (20) is the mixing ratio calculated by the mixing ratio calculation unit (28). With the above-described configuration, the user can set a gradient program for low-pressure gradient analysis using three or more liquids according to a procedure which is as complicated as a gradient program for low-pressure gradient analysis using two liquids. As a result, in the system for low-pressure gradient, gradient analysis using three or more liquids can be easily realized.
A second embodiment of the present invention is a liquid chromatograph (1) including: the low-pressure gradient liquid feeding system (2); and an analysis unit (4) that performs separation and analysis of a sample on a flow path (6) through which the mobile phase flows, using the liquid mixture delivered by the low-pressure gradient delivery system (2) as the mobile phase.
According to the second embodiment, since the mobile phase is transported by using the low-pressure gradient liquid feeding system (2), a novel analysis system of a low-pressure gradient system that can perform gradient analysis using three or more liquids can be provided.
[ description of symbols ]
1: liquid chromatograph
2: low-pressure gradient liquid feeding system
4: analysis section
6: analytical flow path
8. 10, 12, 14: liquid supply flow path
16: switching valve (switching mechanism)
18: liquid feeding pump
20: mixing device
22: control device
24: control unit
26: composition setting part
28: mixing ratio calculation unit
30: sample injection part
32: separation column
34: a detector.

Claims (3)

1. A low pressure gradient fluid delivery system comprising: three or more liquid supply channels for drawing liquids from containers containing the liquids, respectively;
a liquid feeding pump for sucking the liquid from the container through the liquid supply passage and feeding the liquid;
a switching mechanism that is interposed between the three or more liquid supply flow paths and the liquid sending pump, and that selectively switches one liquid supply flow path that communicates with the liquid sending pump from among the three or more liquid supply flow paths;
a mixer for mixing the liquid drawn by the liquid-sending pump;
a composition setting unit configured to set a mixing ratio per time period of three or more liquids mixed in the mixer based on a user input; and
and a control unit configured to control a switching operation of the switching mechanism so that a mixing ratio per time period of the three or more liquids mixed in the mixer is set to the mixing ratio set by the composition setting unit.
2. The low pressure gradient feed system of claim 1, wherein
The composition setting unit is configured to: dividing the three or more liquids into two groups including a first group and a second group, setting a composition of a first solvent including a liquid belonging to the first group and a composition of a second solvent including a liquid belonging to the second group, and setting a mixing ratio per period of time of the first solvent and the second solvent,
the low-pressure gradient liquid feeding system includes a mixing ratio calculation unit configured to: calculating a mixing ratio of the three or more liquids per time period using the composition of the first solvent, the composition of the second solvent, and the mixing ratio of the first solvent and the second solvent per time period set by the composition setting unit,
the control unit is configured to: the switching operation of the switching mechanism is controlled so that the mixing ratio of the three or more liquids mixed in the mixer is the mixing ratio calculated by the mixing ratio calculating unit.
3. A liquid chromatograph comprising: the low pressure gradient feed system of claim 1 or 2; and
and an analysis unit that performs separation and analysis of the sample on a flow path through which the mobile phase flows, using the liquid mixture of the liquids sent by the low-pressure gradient liquid sending system as the mobile phase.
CN201880097859.5A 2018-11-14 2018-11-14 Low-pressure gradient liquid feeding system and liquid chromatograph Active CN112740029B (en)

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PCT/JP2018/042145 WO2020100233A1 (en) 2018-11-14 2018-11-14 Low-pressure gradient liquid delivery system and liquid chromatograph

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JP5268445B2 (en) * 2008-06-25 2013-08-21 株式会社日立ハイテクノロジーズ Flow injection analyzer
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US20020116989A1 (en) * 2001-02-27 2002-08-29 Isco, Inc. Liquid chromatographic method and system
JP2004093251A (en) * 2002-08-30 2004-03-25 Yamazen Corp Liquid chromatograph
JP2004138413A (en) * 2002-10-16 2004-05-13 Shimadzu Corp Liquid chromatograph apparatus and its liquid supplying apparatus
JP2007327846A (en) * 2006-06-07 2007-12-20 Gl Sciences Inc Gradient liquid feeding method and device
JP2010502960A (en) * 2006-08-29 2010-01-28 クライオバイオフィジカ,インコーポレイテッド Multi-component, simultaneous, independent multi-gradient system for liquid chromatography
JP2010085146A (en) * 2008-09-30 2010-04-15 Hitachi High-Technologies Corp Gradient liquid feeding apparatus, gradient liquid feeding system, and liquid chromatograph
CN105116080A (en) * 2010-06-16 2015-12-02 株式会社日立高新技术 Liquid mixing device and liquid chromatograph
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JP6992912B2 (en) 2022-01-13
WO2020100233A1 (en) 2020-05-22
CN112740029B (en) 2023-08-04
JPWO2020100233A1 (en) 2021-09-02

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