WO2020100233A1 - Low-pressure gradient liquid delivery system and liquid chromatograph - Google Patents

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

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WO2020100233A1
WO2020100233A1 PCT/JP2018/042145 JP2018042145W WO2020100233A1 WO 2020100233 A1 WO2020100233 A1 WO 2020100233A1 JP 2018042145 W JP2018042145 W JP 2018042145W WO 2020100233 A1 WO2020100233 A1 WO 2020100233A1
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liquid
mixing ratio
liquids
solvent
pressure gradient
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PCT/JP2018/042145
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French (fr)
Japanese (ja)
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伊織 大友
覚 渡辺
知広 舎川
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株式会社島津製作所
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Priority to CN201880097859.5A priority Critical patent/CN112740029B/en
Priority to JP2020556509A priority patent/JP6992912B2/en
Priority to PCT/JP2018/042145 priority patent/WO2020100233A1/en
Publication of WO2020100233A1 publication Critical patent/WO2020100233A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/50—Conditioning of the sorbent material or stationary liquid

Definitions

  • the present invention relates to a low pressure gradient liquid delivery system and a liquid chromatograph.
  • liquid chromatographic analysis a mixture of multiple liquids is often used as the mobile phase, and gradient analysis is often performed while changing the mixing ratio of the liquids that make up the mobile phase for each time period.
  • the system automatically calculates the mixing ratio of each liquid to make the characteristics (eg, pH) of the mobile phase in each time period set by the user.
  • characteristics eg, pH
  • the high-pressure gradient method is a method in which a plurality of liquid feed pumps are used to feed a plurality of liquids at the same time.
  • the low-pressure gradient method is a method 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 liquid can be fed at the same time.
  • an object of the present invention is to provide a novel low-pressure gradient system capable of realizing gradient analysis using three or more liquids.
  • the first aspect of the present invention is for pumping liquid from the container through three or more liquid supply channels for respectively pumping the liquid from the container containing the liquid, and for feeding the liquid.
  • One liquid feed pump, and one liquid feed passage interposed between the three or more liquid feed passages and the liquid feed pump and communicating with the liquid feed pump, the three or more liquid feeds A switching mechanism for selectively switching among the flow paths, a mixer for mixing the liquids pumped by the liquid feed pump, and three or more liquids to be mixed in the mixer based on user input.
  • a composition setting unit configured to set a mixing ratio for each time zone, and a mixing ratio set by the composition setting unit for the mixing ratio for each time zone of the three or more liquids mixed in the mixer.
  • a low-pressure gradient liquid delivery system comprising: a control unit configured to control the switching operation of the switching mechanism.
  • a second aspect of the present invention uses the above-mentioned low pressure gradient liquid feeding system and a liquid mixture of the liquid fed by the low pressure gradient liquid feeding system as a mobile phase, and separates and analyzes a sample on a flow path through which the mobile phase flows. It is a liquid chromatograph provided with the analysis part which performs.
  • a composition setting unit configured to set a mixing ratio of three or more liquids mixed in the mixer for each time period based on a user input.
  • a control configured to control the switching operation of the switching mechanism so that the mixing ratio of the three or more liquids mixed in the mixer for each time period becomes the mixing ratio set by the composition setting unit. Since it is provided with a section, a novel low-pressure gradient liquid transfer system capable of realizing a gradient analysis using three or more liquids is provided.
  • liquid chromatograph since the mobile phase is delivered using the above-mentioned low pressure gradient delivery system, a novel low pressure gradient capable of realizing a gradient analysis using three or more solutions.
  • a method of analytical system is provided.
  • the liquid chromatograph 1 of this embodiment mainly includes a low pressure gradient liquid sending system 2 and an analysis unit 4.
  • the low-pressure gradient liquid sending system 2 has a gradient function of sending a mixed liquid of three or more liquids as a mobile phase in the analysis channel 6 and changing the composition of the mobile phase with time.
  • 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 supply system 2 includes four liquid supply flow paths 8, 10, 12, and 14, a switching valve 16, a liquid supply pump 18, a mixer 20, and a control device 22.
  • the liquid supply flow paths 8, 10, 12, and 14 are flow paths for pumping the liquid from the containers containing the liquids 1 to 4, respectively.
  • the liquid supply flow paths 8, 10, 12, 14 are connected to different selection ports of the switching valve 16.
  • the suction side of the liquid feed pump 18 is connected to the common port of the switching valve 16. That is, the switching valve 16 is interposed between the liquid feed pump 18 and the four liquid supply passages 8, 10, 12, and 14, and selectively switches the liquid feed passages that communicate with the liquid feed pump 18. It constitutes a switching mechanism.
  • the switching mechanism is not limited to the switching valve 16.
  • a stop valve is provided on each of the liquid supply flow paths 8, 10, 12, and 14, and any one stop valve is opened to open the liquid feed pump 18 and any one liquid supply flow. It can also be configured to be in fluid communication with the passage.
  • the stop valve provided on each liquid supply flow path 8, 10, 12, 14 constitutes a switching mechanism for selectively switching the liquid supply flow path communicating with the liquid supply pump 18. ..
  • the switching mechanism may have any configuration as long as it can selectively switch the liquid supply flow path fluidly communicating with the liquid feed pump 18.
  • the mixer 20 is provided downstream of the liquid feed pump 18, and the liquid fed by the liquid feed pump 18 is mixed in the mixer 20.
  • the mixer 20 may be provided upstream of the liquid feed pump 18.
  • the operation of the switching valve 16 and the liquid feed pump 18 is controlled by the control device 22.
  • the control device 22 is realized by an electronic circuit having a central processing unit (CPU) and a storage 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 switches 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, in accordance with a preset gradient program. It is configured to control the switching operation of the valve 16.
  • the gradient program indicates how the composition of the mobile phase is changed with the passage of time from the start of the analysis.
  • the gradient setting program is set by the composition setting unit 26 based on user input.
  • the gradient program set by the composition setting unit 26 four liquids, liquid 1 to liquid 4, are divided into two groups, a first group and a second group, and a first solvent and a first solvent which are liquids belonging to the first group
  • An example is one in which the mixing ratio with the second solvent composed of the liquids belonging to the two groups is changed with time.
  • the composition setting unit 26 causes the composition of the first solvent and the composition of the second solvent to be input as illustrated in FIG. 2, and the input compositions are used as the first solvent composition and the second solvent composition, respectively.
  • the composition setting unit 26 inputs, as a user input, how to temporally change the mixing ratio of the first solvent and the second solvent, that is, the mixing ratio of the first solvent and the second solvent for each time period. Based on the determination, the gradient program as illustrated in FIG. 3 is set.
  • the mixing ratio calculating unit 28 calculates the mixing ratio of the liquids 1 to 4 in the mobile phase in each time zone from the first solvent composition, the second solvent composition, and the gradient program set by the composition setting unit 26. It is configured.
  • the calculation of the mixing ratio by the mixing ratio calculation unit 28 will be described by using the numerical values illustrated in FIGS. 2 and 3 as an example of the time period when the second solvent concentration is 60% on the gradient program of FIG. To do.
  • the ratio here is a volume ratio.
  • the control unit 24 controls the switching valve so that the composition in the mixed liquid mixed in the mixer 20 in each time zone becomes the mixing ratio of the liquids 1 to 4 in each time period calculated by the mixing ratio calculating unit 28. 16 switching operations are controlled.
  • the user when setting the gradient program, as illustrated in FIG. 3, the user uses a procedure similar in complexity to setting a program for low pressure gradient analysis using two liquids.
  • a gradient program for low pressure gradient analysis using 4 solutions can be set. This makes it possible to realize low-pressure gradient analysis using a large number of liquids without forcing the user to perform a complicated setting procedure.
  • 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.
  • the separation column 32 is for separating the sample injected into the analysis flow path 6 by the sample injection unit 30 into each component.
  • the detector 34 is for detecting the sample components separated by the separation column 32.
  • the low pressure gradient analysis can be performed using the four liquids of liquid 1 to liquid 4, but the present invention is not limited to this, and the low pressure gradient is not limited thereto. Any number of liquids may be used in the analysis as long as they are three or more.
  • the first group includes two liquids, liquid 1 and liquid 2
  • the second group includes two liquids, liquid 3 and liquid 4, but the present invention is not limited to this.
  • the total of the liquids belonging to the first group and the second group is 3 or more, the number of liquids included in each group may be any number.
  • the embodiment of the present invention is as follows.
  • three or more liquid supply channels (8; 10; 12; 14) for respectively pumping the liquid from the container containing the liquid and the liquid supply channels (8; 10). 12; 14), one liquid delivery pump (18) for pumping and delivering the liquid from the container, the three or more liquid supply flow paths (8; 10; 12; 14) and the One of the three or more liquid supply flow paths (8; 10; 12; 14) is provided between the liquid supply pump (18) and communicates with the liquid supply pump (18).
  • a switching mechanism (16) for selectively switching from the above, a mixer (20) for mixing the liquid pumped up by the liquid feed pump (18), and a mixer (20) in the mixer (20) based on user input.
  • a composition setting unit (26) configured to set a mixing ratio of three or more liquids to be mixed for each time period, and a mixing ratio of the three or more liquids to be mixed in the mixer for each time period.
  • Low pressure gradient liquid delivery comprising a control unit (24) configured to control the switching operation of the switching mechanism (16) so that the mixing ratio is set to the mixing ratio set by the composition setting unit (26).
  • a composition setting unit (26) configured to set a mixing ratio of three or more liquids mixed in the mixer for each time period based on user input, and a mixer.
  • the switching operation of the switching mechanism (16) is controlled in order to set the mixing ratio of the three or more liquids mixed in each time zone to the mixing ratio set by the composition setting unit (26). Since the control section (24) is provided, a novel low-pressure gradient type liquid delivery system capable of realizing a gradient analysis using three or more liquids is provided.
  • the composition setting part (26) divides the three or more liquids into two groups, a first group and a second group, and a first liquid consisting of the liquids belonging to the first group.
  • the composition of the solvent and the composition of the second solvent composed of the liquid belonging to the second group are set, and the mixing ratio of the first solvent and the second solvent for each time zone is set.
  • the low-pressure gradient liquid delivery system (2) includes the composition of the first solvent, the composition of the second solvent, the composition of the second solvent, and the composition of the first solvent and the second solvent, which are set by the composition setting unit (26).
  • a mixing ratio calculation unit (28) configured to calculate the mixing ratio of the three or more liquids for each time period using the mixing ratio for each time period, the control unit (24) comprising:
  • 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) becomes the mixing ratio calculated by the mixing ratio calculation unit (28).
  • It may be configured as follows. According to such a configuration, the user sets the gradient program for low-pressure gradient analysis using three or more liquids by a procedure having the same degree of complexity as the gradient program for low-pressure gradient analysis using two liquids. be able to. As a result, it is possible to easily realize a gradient analysis using three or more liquids in the system for low pressure gradient.
  • the low pressure gradient liquid feeding system (2) and a liquid mixture of the liquid fed by the low pressure gradient liquid feeding system (2) are used as a mobile phase, and the mobile phase flows.
  • It is a liquid chromatograph (1) provided with an analysis unit (4) for separating and analyzing a sample on a channel (6).
  • the mobile phase is delivered using the low pressure gradient delivery system (2) described above, a novel low pressure gradient method capable of realizing a gradient analysis using three or more fluids. Analysis system is provided.
  • Liquid Chromatograph 2 Low Pressure Gradient Liquid Delivery System 4 Analyzing Section 6 Analytical Flow Paths 8, 10, 12, 14 Liquid Supply Flow Path 16 Switching Valve (Switching Mechanism) 18 Liquid-sending pump 20 Mixer 22 Control device 24 Control unit 26 Composition setting unit 28 Mixing ratio calculation unit 30 Sample injection unit 32 Separation column 34 Detector

Abstract

A low-pressure gradient liquid delivery system 2 is provided with: three or more liquid supply channels (8, 10, 12, 14) for drawing a liquid from each of containers accommodating the liquid; a single liquid delivery pump (18) for drawing the liquid from the containers via the liquid supply channels (8, 10, 12, 14); a switching mechanism (16) for selectively switching a single liquid supply channel to be communicated with the liquid delivery pump (18) from among the three or more liquid supply channels (8, 10, 12, 14), the switching mechanism (16) being interposed between the three or more liquid supply channels (8, 10, 12, 14) and the liquid delivery pump (18); a mixer (20) for mixing the liquid drawn by the liquid delivery pump (18); a composition setting unit (26) configured so as to set a mixture ratio for each time period of the three or more liquids mixed in the mixer (20), on the basis of a user input; and a control unit (24) configured so as to control the switching operation of the switching mechanism (16) to make the mixture ratio for each time period of the three or more liquids mixed in the mixer the mixture ratio set by the composition setting unit (26).

Description

低圧グラジエント送液システム及び液体クロマトグラフLow pressure gradient liquid delivery system and liquid chromatograph
　本発明は、低圧グラジエント送液システム及び液体クロマトグラフに関するものである。 The present invention relates to a low pressure gradient liquid delivery system and a liquid chromatograph.
　液体クロマトグラフィー分析では、複数の液の混合液を移動相として用いられることが多く、移動相を組成する液の混合比率を時間帯ごとに変化させながら行なうグラジエント分析もよく実施される。 In liquid chromatographic analysis, a mixture of multiple liquids is often used as the mobile phase, and gradient analysis is often performed while changing the mixing ratio of the liquids that make up the mobile phase for each time period.
　グラジエント分析を行なうには、移動相の組成をどのように時間変化させていくかについて規定するグラジエントプログラムを予めシステムに設定しておく必要がある。しかしながら、グラジエント分析に用いる液の数が多くなると、各液の混合比率をどのように変化させていくのかについての計算が複雑になり、グラジエントプログラムの設定が煩雑になる。 In order to perform a gradient analysis, it is necessary to set a gradient program in the system in advance that defines how the composition of the mobile phase is changed over time. However, when the number of liquids used in the gradient analysis increases, the calculation about how to change the mixing ratio of each liquid becomes complicated, and the setting of the gradient program becomes complicated.
　プログラムの設定の煩雑さを軽減するために、各時間帯における移動相の特性（例えば、ｐＨ）をユーザの設定したものとするための各液の混合比率をシステム側で自動的に計算させるようにすることが提案されている（特許文献１）。 In order to reduce the complexity of program settings, the system automatically calculates the mixing ratio of each liquid to make the characteristics (eg, pH) of the mobile phase in each time period set by the user. Has been proposed (Patent Document 1).
ＷＯ２０１５／１７２０１１Ａ１WO2015 / 172011A1
　グラジエント分析の方式として、高圧グラジエント方式と低圧グラジエント方式がある。高圧グラジエント方式は、複数台の送液ポンプを用いて複数の液を同時に送液する方式である。一方で、低圧グラジエント方式は、１台の送液ポンプを用い、送液ポンプによって送液される液を切替バルブで切り替える方式であり、同時に送液できる液は１種類だけである。 ▽ As a method of gradient analysis, there are a high pressure gradient method and a low pressure gradient method. The high-pressure gradient method is a method in which a plurality of liquid feed pumps are used to feed a plurality of liquids at the same time. On the other hand, the low-pressure gradient method is a method 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 liquid can be fed at the same time.
　これまでの低圧グラジエント方式のシステムでは、２液を用いたグラジエント分析用のグラジエントプログラムしか設定できないようになっていた。そのため、例えば、水系溶媒と有機溶媒のほかに緩衝液などの液を使用したい場合、予め溶媒に緩衝液などの液を混合してｐＨ等を調整しておく必要があった。 In the conventional low-pressure gradient system, only the gradient program for gradient analysis using two liquids can be set. Therefore, for example, when it is desired to use a solution such as a buffer solution in addition to the aqueous solvent and the organic solvent, it is necessary to previously mix the solvent with a solution such as the buffer solution to adjust the pH and the like.
　そこで、本発明は、３つ以上の液を用いたグラジエント分析を実現できる新規な低圧グラジエント方式のシステムを提供することを目的とするものである。 Therefore, an object of the present invention is to provide a novel low-pressure gradient system capable of realizing gradient analysis using three or more liquids.
　本発明の第１の態様は、液を収容した容器からそれぞれ液を汲み上げるための３つ以上の液供給流路と、前記液供給流路を介して前記容器から液を汲み上げて送液するための１つの送液ポンプと、前記３つ以上の液供給流路と前記送液ポンプとの間に介在し、前記送液ポンプと連通させる１つの液供給流路を前記３つ以上の液供給流路のうちから選択的に切り替えるための切替機構と、前記送液ポンプによって汲み上げられた液の混合を行なうためのミキサと、ユーザ入力に基づいて、前記ミキサにおいて混合される３つ以上の液の時間帯ごとの混合比率を設定するように構成された組成設定部と、前記ミキサにおいて混合される前記３つ以上の液の時間帯ごとの混合比率を前記組成設定部により設定された混合比率とするために、前記切替機構の切替え動作を制御するように構成された制御部と、を備えた低圧グラジエント送液システムである。 The first aspect of the present invention is for pumping liquid from the container through three or more liquid supply channels for respectively pumping the liquid from the container containing the liquid, and for feeding the liquid. One liquid feed pump, and one liquid feed passage interposed between the three or more liquid feed passages and the liquid feed pump and communicating with the liquid feed pump, the three or more liquid feeds A switching mechanism for selectively switching among the flow paths, a mixer for mixing the liquids pumped by the liquid feed pump, and three or more liquids to be mixed in the mixer based on user input. A composition setting unit configured to set a mixing ratio for each time zone, and a mixing ratio set by the composition setting unit for the mixing ratio for each time zone of the three or more liquids mixed in the mixer. In order to achieve this, a low-pressure gradient liquid delivery system comprising: a control unit configured to control the switching operation of the switching mechanism.
　本発明の第２の態様は、上記低圧グラジエント送液システムと、前記低圧グラジエント送液システムにより送液される液の混合液を移動相として用い、前記移動相の流れる流路上で試料の分離分析を行なう分析部と、を備えた液体クロマトグラフである。 A second aspect of the present invention uses the above-mentioned low pressure gradient liquid feeding system and a liquid mixture of the liquid fed by the low pressure gradient liquid feeding system as a mobile phase, and separates and analyzes a sample on a flow path through which the mobile phase flows. It is a liquid chromatograph provided with the analysis part which performs.
　本発明の第１の態様に係る低圧グラジエント送液システムでは、ユーザ入力に基づいて、ミキサにおいて混合される３つ以上の液の時間帯ごとの混合比率を設定するように構成された組成設定部と、ミキサにおいて混合される前記３つ以上の液の時間帯ごとの混合比率を前記組成設定部により設定された混合比率とするために、切替機構の切替え動作を制御するように構成された制御部と、を備えているので、３つ以上の液を用いたグラジエント分析を実現できる新規な低圧グラジエント方式の送液システムが提供される。 In the low-pressure gradient liquid delivery system according to the first aspect of the present invention, a composition setting unit configured to set a mixing ratio of three or more liquids mixed in the mixer for each time period based on a user input. And a control configured to control the switching operation of the switching mechanism so that the mixing ratio of the three or more liquids mixed in the mixer for each time period becomes the mixing ratio set by the composition setting unit. Since it is provided with a section, a novel low-pressure gradient liquid transfer system capable of realizing a gradient analysis using three or more liquids is provided.
　本発明の第２の態様に係る液体クロマトグラフでは、上述の低圧グラジエント送液システムを用いて移動相の送液を行なうので、３つ以上の液を用いたグラジエント分析を実現できる新規な低圧グラジエント方式の分析システムが提供される。 In the liquid chromatograph according to the second aspect of the present invention, since the mobile phase is delivered using the above-mentioned low pressure gradient delivery system, a novel low pressure gradient capable of realizing a gradient analysis using three or more solutions. A method of analytical system is provided.
低圧グラジエント送液システム及び液体クロマトグラフの一実施例を示す概略構成図である。It is a schematic structure figure showing one example of a low-pressure gradient liquid sending system and a liquid chromatograph. 同実施例における第１溶媒の組成及び第２溶媒の組成の設定の一例を示す図である。It is a figure which shows an example of setting of the composition of a 1st solvent and the composition of a 2nd solvent in the Example. 同実施例における移動相の組成の設定の一例を示す図である。It is a figure which shows an example of setting of the composition of the mobile phase in the same Example.
　以下、低圧グラジエント送液システム及び液体クロマトグラフの一実施例について、図面を用いて説明する。 An example of a low pressure gradient liquid delivery system and a liquid chromatograph will be described below with reference to the drawings.
　図１に示されているように、この実施例の液体クロマトグラフ１は、主として、低圧グラジエント送液システム２と分析部４を備えている。 As shown in FIG. 1, the liquid chromatograph 1 of this embodiment mainly includes a low pressure gradient liquid sending system 2 and an analysis unit 4.
　低圧グラジエント送液システム２は、３つ以上の液からなる混合液を移動相として分析流路６中で送液するとともに、移動相の組成を時間的に変化させるグラジエント機能を有するものである。この実施例においては、低圧グラジエント送液システム２は、４つの液（液１～液４）を用いたグラジエント送液を行なうことができる。 The low-pressure gradient liquid sending system 2 has a gradient function of sending a mixed liquid of three or more liquids as a mobile phase in the analysis channel 6 and changing the composition of the mobile phase with time. In this embodiment, the low pressure gradient liquid feeding system 2 can perform gradient liquid feeding using four liquids (Liquid 1 to Liquid 4).
　低圧グラジエント送液システム２は、４つの液供給流路８，１０，１２，１４と、切替バルブ１６と、送液ポンプ１８と、ミキサ２０と、制御装置２２と、を備えている。液供給流路８，１０，１２，１４は、液１～液４を収容する容器からそれぞれ液を汲み上げるための流路である。液供給流路８，１０，１２，１４は切替バルブ１６の互いに異なる選択ポートに接続されている。送液ポンプ１８の吸入側は切替バルブ１６の共通ポートに接続されている。すなわち、切替バルブ１６は、送液ポンプ１８と４つの液供給流路８，１０，１２，１４との間に介在し、送液ポンプ１８と連通させる液供給流路を選択的に切り替えるための切替機構を構成する。 The low pressure gradient liquid supply system 2 includes four liquid supply flow paths 8, 10, 12, and 14, a switching valve 16, a liquid supply pump 18, a mixer 20, and a control device 22. The liquid supply flow paths 8, 10, 12, and 14 are flow paths for pumping the liquid from the containers containing the liquids 1 to 4, respectively. The liquid supply flow paths 8, 10, 12, 14 are connected to different selection ports of the switching valve 16. The suction side of the liquid feed pump 18 is connected to the common port of the switching valve 16. That is, the switching valve 16 is interposed between the liquid feed pump 18 and the four liquid supply passages 8, 10, 12, and 14, and selectively switches the liquid feed passages that communicate with the liquid feed pump 18. It constitutes a switching mechanism.
　なお、切替機構は切替バルブ１６に限定されるものではない。例えば、切替バルブ１６に代えて、各液供給流路８，１０，１２，１４上にストップバルブを設け、いずれか１つのストップバルブを開くことによって送液ポンプ１８といずれか１つの液供給流路とを流体的に連通させるように構成することもできる。そのような場合は、各液供給流路８，１０，１２，１４上に設けられたストップバルブが、送液ポンプ１８と連通させる液供給流路を選択的に切り替えるための切替機構を構成する。このほか、切替機構は、送液ポンプ１８と流体的に連通させる液供給流路を選択的に切り替えることができるものであれば、どのような構成を有していてもよい。 Note that the switching mechanism is not limited to the switching valve 16. For example, instead of the switching valve 16, a stop valve is provided on each of the liquid supply flow paths 8, 10, 12, and 14, and any one stop valve is opened to open the liquid feed pump 18 and any one liquid supply flow. It can also be configured to be in fluid communication with the passage. In such a case, the stop valve provided on each liquid supply flow path 8, 10, 12, 14 constitutes a switching mechanism for selectively switching the liquid supply flow path communicating with the liquid supply pump 18. .. In addition, the switching mechanism may have any configuration as long as it can selectively switch the liquid supply flow path fluidly communicating with the liquid feed pump 18.
　ミキサ２０は送液ポンプ１８の下流に設けられており、送液ポンプ１８によって送液されてきた液がミキサ２０において混合される。なお、ミキサ２０は送液ポンプ１８の上流に設けられていてもよい。 The mixer 20 is provided downstream of the liquid feed pump 18, and the liquid fed by the liquid feed pump 18 is mixed in the mixer 20. The mixer 20 may be provided upstream of the liquid feed pump 18.
　切替バルブ１６及び送液ポンプ１８の動作は制御装置２２によって制御される。制御装置２２は、中央演算装置（ＣＰＵ）や記憶装置を有する電子回路によって実現されるものである。制御装置２２は、その機能として、制御部２４、組成設定部２６及び混合比率計算部２８を備えている。制御部２４、組成設定部２６及び混合比率計算部２８は、ＣＰＵが特定のプログラムを実行することによって得られる機能である。 The operation of the switching valve 16 and the liquid feed pump 18 is controlled by the control device 22. The control device 22 is realized by an electronic circuit having a central processing unit (CPU) and a storage 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.
　制御部２４は、分析流路６を流れる移動相の組成、すなわち、ミキサ２０において混合される液１～液４の混合比率を、予め設定されたグラジエントプログラムに沿ったものとするために、切替バルブ１６の切替え動作を制御するように構成されている。ここで、グラジエントプログラムとは、分析を開始してから時間を経るごとにどのように移動相の組成を変化させていくかを示すものである。 The control unit 24 switches 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, in accordance with a preset gradient program. It is configured to control the switching operation of the valve 16. Here, the gradient program indicates how the composition of the mobile phase is changed with the passage of time from the start of the analysis.
　グラジエントプログラムは組成設定部２６がユーザ入力に基づいて設定する。組成設定部２６によって設定されるグラジエントプログラムとしては、液１～液４の４つの液を第１グループと第２グループの２つのグループに分け、第１グループに属する液からなる第１溶媒と第２グループに属する液からなる第２溶媒との混合比率を時間的に変化させていくものが挙げられる。 The gradient setting program is set by the composition setting unit 26 based on user input. As the gradient program set by the composition setting unit 26, four liquids, liquid 1 to liquid 4, are divided into two groups, a first group and a second group, and a first solvent and a first solvent which are liquids belonging to the first group An example is one in which the mixing ratio with the second solvent composed of the liquids belonging to the two groups is changed with time.
　上記の場合、組成設定部２６は、第１溶媒の組成と第２溶媒の組成を図２に例示されているように入力させ、入力された組成をそれぞれ第１溶媒組成、第２溶媒組成として設定する。さらに、組成設定部２６は、第１溶媒と第２溶媒の混合比率をどのように時間的に変化させるか、すなわち、第１溶媒と第２溶媒の時間帯ごとの混合比率を、ユーザ入力に基づいて決定することにより、図３に例示されているようなグラジエントプログラムを設定する。 In the above case, the composition setting unit 26 causes the composition of the first solvent and the composition of the second solvent to be input as illustrated in FIG. 2, and the input compositions are used as the first solvent composition and the second solvent composition, respectively. Set. Further, the composition setting unit 26 inputs, as a user input, how to temporally change the mixing ratio of the first solvent and the second solvent, that is, the mixing ratio of the first solvent and the second solvent for each time period. Based on the determination, the gradient program as illustrated in FIG. 3 is set.
　混合比率計算部２８は、組成設定部２６により設定された第１溶媒組成、第２溶媒組成及びグラジエントプログラムから、各時間帯における移動相中の液１～液４の混合比率を計算するように構成されている。 The mixing ratio calculating unit 28 calculates the mixing ratio of the liquids 1 to 4 in the mobile phase in each time zone from the first solvent composition, the second solvent composition, and the gradient program set by the composition setting unit 26. It is configured.
　混合比率計算部２８による混合比率の計算を、図２及び図３に例示された数値を用いて、図３のグラジエントプログラム上で第２溶媒濃度が６０％である時間帯を例に挙げて説明する。この時間帯の移動相中の第１溶媒（液１：液２＝９：１）の混合比率は４０％、第２溶媒（液３：液４＝１：１）の混合比率は６０％である。したがって、移動相中における液１～液４の混合比率は以下のように計算される。なお、ここでの比率は体積比率である。
　液１：４０％×９０％＝３６％
　液２：４０％×１０％＝４％
　液３：６０％×５０％＝３０％
　液４：６０％×５０％＝３０％
　したがって、上記時間帯における移動相の組成は、液１：液２：液３：液４＝３６：４：３０：３０となる。 The calculation of the mixing ratio by the mixing ratio calculation unit 28 will be described by using the numerical values illustrated in FIGS. 2 and 3 as an example of the time period when the second solvent concentration is 60% on the gradient program of FIG. To do. The mixing ratio of the first solvent (liquid 1: liquid 2 = 9: 1) in the mobile phase in this period was 40%, and the mixing ratio of the second solvent (liquid 3: liquid 4 = 1: 1) was 60%. is there. Therefore, the mixing ratio of liquid 1 to liquid 4 in the mobile phase is calculated as follows. The ratio here is a volume ratio.
Liquid 1: 40% x 90% = 36%
Liquid 2: 40% x 10% = 4%
Liquid 3: 60% x 50% = 30%
Liquid 4: 60% x 50% = 30%
Therefore, the composition of the mobile phase in the above time zone is liquid 1: liquid 2: liquid 3: liquid 4 = 36: 4: 30: 30.
　制御部２４は、各時間帯におけるミキサ２０で混合される混合液中の組成が、混合比率計算部２８により計算された各時間帯の液１～液４の混合比率となるように、切替バルブ１６の切替え動作を制御する。 The control unit 24 controls the switching valve so that the composition in the mixed liquid mixed in the mixer 20 in each time zone becomes the mixing ratio of the liquids 1 to 4 in each time period calculated by the mixing ratio calculating unit 28. 16 switching operations are controlled.
　上記のように、グラジエントプログラムの設定の際、図３に例示されているように、ユーザは、２液を用いた低圧グラジエント分析用のプログラムを設定するのと同程度の複雑さの手順で、４液を用いた低圧グラジエント分析用のグラジエントプログラムを設定することができる。これにより、ユーザに煩雑な設定手順を強いることなく、多数の液を用いた低圧グラジエント分析を実現することができる。 As described above, when setting the gradient program, as illustrated in FIG. 3, the user uses a procedure similar in complexity to setting a program for low pressure gradient analysis using two liquids. A gradient program for low pressure gradient analysis using 4 solutions can be set. This makes it possible to realize low-pressure gradient analysis using a large number of liquids without forcing the user to perform a complicated setting procedure.
　図１に戻って液体クロマトグラフの一実施例の説明を続けると、分析部４は、試料注入部３０、分離カラム３２及び検出器３４を備えている。試料注入部３０は、分析流路６中に試料を注入する機能を備えたものであり、例えばオートサンプラである。分離カラム３２は、試料注入部３０により分析流路６中に注入された試料を成分ごとに分離するためのものである。検出器３４は、分離カラム３２で分離された試料成分を検出するためのものである。 Returning to FIG. 1 and continuing the description of one embodiment of the liquid chromatograph, 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. The separation column 32 is for separating the sample injected into the analysis flow path 6 by the sample injection unit 30 into each component. The detector 34 is for detecting the sample components separated by the separation column 32.
　以上において説明した実施例では、液１～液４の４つの液を用いて低圧グラジエント分析を行なうことができるように構成されているが、本発明はこれに限定されるものではなく、低圧グラジエント分析に用いる液は３つ以上であればいくつであってもよい。 In the embodiment described above, the low pressure gradient analysis can be performed using the four liquids of liquid 1 to liquid 4, but the present invention is not limited to this, and the low pressure gradient is not limited thereto. Any number of liquids may be used in the analysis as long as they are three or more.
　また、上記実施例では、第１グループを液１及び液２の２液を含むものとし、第２グループを液３及び液４の２液を含むものとしているが、本発明はこれに限定されるものではなく、第１グループ及び第２グループに属する液の合計が３液以上であれば、各グループに含まれる液の数はいくらであってもよい。 Further, in the above embodiment, the first group includes two liquids, liquid 1 and liquid 2, and the second group includes two liquids, liquid 3 and liquid 4, but the present invention is not limited to this. However, if the total of the liquids belonging to the first group and the second group is 3 or more, the number of liquids included in each group may be any number.
　すなわち、本発明の実施態様は以下のとおりである。 That is, the embodiment of the present invention is as follows.
　本発明の第１の実施態様は、液を収容した容器からそれぞれ液を汲み上げるための３つ以上の液供給流路（８；１０；１２；１４）と、前記液供給流路（８；１０；１２；１４）を介して前記容器から液を汲み上げて送液するための１つの送液ポンプ（１８）と、前記３つ以上の液供給流路（８；１０；１２；１４）と前記送液ポンプ（１８）との間に介在し、前記送液ポンプ（１８）と連通させる１つの液供給流路を前記３つ以上の液供給流路（８；１０；１２；１４）のうちから選択的に切り替えるための切替機構（１６）と、前記送液ポンプ（１８）によって汲み上げられた液の混合を行なうためのミキサ（２０）と、ユーザ入力に基づいて、前記ミキサ（２０）において混合される３つ以上の液の時間帯ごとの混合比率を設定するように構成された組成設定部（２６）と、前記ミキサにおいて混合される前記３つ以上の液の時間帯ごとの混合比率を前記組成設定部（２６）により設定された混合比率とするために、前記切替機構（１６）の切替え動作を制御するように構成された制御部（２４）と、を備えた低圧グラジエント送液システム（２）である。 In the first embodiment of the present invention, three or more liquid supply channels (8; 10; 12; 14) for respectively pumping the liquid from the container containing the liquid and the liquid supply channels (8; 10). 12; 14), one liquid delivery pump (18) for pumping and delivering the liquid from the container, the three or more liquid supply flow paths (8; 10; 12; 14) and the One of the three or more liquid supply flow paths (8; 10; 12; 14) is provided between the liquid supply pump (18) and communicates with the liquid supply pump (18). A switching mechanism (16) for selectively switching from the above, a mixer (20) for mixing the liquid pumped up by the liquid feed pump (18), and a mixer (20) in the mixer (20) based on user input. A composition setting unit (26) configured to set a mixing ratio of three or more liquids to be mixed for each time period, and a mixing ratio of the three or more liquids to be mixed in the mixer for each time period. Low pressure gradient liquid delivery, comprising a control unit (24) configured to control the switching operation of the switching mechanism (16) so that the mixing ratio is set to the mixing ratio set by the composition setting unit (26). The system (2).
　上記第１の実施態様によれば、ユーザ入力に基づいて、ミキサにおいて混合される３つ以上の液の時間帯ごとの混合比率を設定するように構成された組成設定部（２６）と、ミキサにおいて混合される前記３つ以上の液の時間帯ごとの混合比率を前記組成設定部（２６）により設定された混合比率とするために、切替機構（１６）の切替え動作を制御するように構成された制御部（２４）と、を備えているので、３つ以上の液を用いたグラジエント分析を実現できる新規な低圧グラジエント方式の送液システムが提供される。 According to the first embodiment, a composition setting unit (26) configured to set a mixing ratio of three or more liquids mixed in the mixer for each time period based on user input, and a mixer. The switching operation of the switching mechanism (16) is controlled in order to set the mixing ratio of the three or more liquids mixed in each time zone to the mixing ratio set by the composition setting unit (26). Since the control section (24) is provided, a novel low-pressure gradient type liquid delivery system capable of realizing a gradient analysis using three or more liquids is provided.
　上記第１の実施態様において、前記組成設定部（２６）は、前記３つ以上の液を第１グループ及び第２グループからなる２つのグループに分け、前記第１グループに属する液からなる第１溶媒の組成、及び前記第２グループに属する液からなる第２溶媒の組成を設定するとともに、前記第１溶媒と前記第２溶媒との時間帯ごとの混合比率を設定するように構成されていてもよい。その場合、前記低圧グラジエント送液システム（２）は、前記組成設定部（２６）により設定された前記第１溶媒の組成、前記第２溶媒の組成、前記第１溶媒と前記第２溶媒との時間帯ごとの混合比率を用いて、前記時間帯ごとの前記３つ以上の液の混合比率を計算するように構成された混合比率計算部（２８）を備え、前記制御部（２４）は、前記ミキサ（２０）において混合される前記３つ以上の液の混合比率を前記混合比率計算部（２８）によって計算された混合比率とするために、前記切替機構（１６）の切替え動作を制御するように構成されていてもよい。このような構成によれば、ユーザは、２液を用いた低圧グラジエント分析用のグラジエントプログラムと同程度の複雑さの手順によって３つ以上の液を用いた低圧グラジエント分析用のグラジエントプログラムを設定することができる。その結果、低圧グラジエント用のシステムにおいて、３つ以上の液を用いたグラジエント分析を容易に実現することができる。 In the first embodiment, the composition setting part (26) divides the three or more liquids into two groups, a first group and a second group, and a first liquid consisting of the liquids belonging to the first group. The composition of the solvent and the composition of the second solvent composed of the liquid belonging to the second group are set, and the mixing ratio of the first solvent and the second solvent for each time zone is set. Good. In that case, the low-pressure gradient liquid delivery system (2) includes the composition of the first solvent, the composition of the second solvent, the composition of the second solvent, and the composition of the first solvent and the second solvent, which are set by the composition setting unit (26). A mixing ratio calculation unit (28) configured to calculate the mixing ratio of the three or more liquids for each time period using the mixing ratio for each time period, the control unit (24) comprising: 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) becomes the mixing ratio calculated by the mixing ratio calculation unit (28). It may be configured as follows. According to such a configuration, the user sets the gradient program for low-pressure gradient analysis using three or more liquids by a procedure having the same degree of complexity as the gradient program for low-pressure gradient analysis using two liquids. be able to. As a result, it is possible to easily realize a gradient analysis using three or more liquids in the system for low pressure gradient.
　本発明の第２の実施態様は、上記低圧グラジエント送液システム（２）と、前記低圧グラジエント送液システム（２）により送液される液の混合液を移動相として用い、前記移動相の流れる流路（６）上で試料の分離分析を行なう分析部（４）と、を備えた液体クロマトグラフ（１）である。 In the second embodiment of the present invention, the low pressure gradient liquid feeding system (2) and a liquid mixture of the liquid fed by the low pressure gradient liquid feeding system (2) are used as a mobile phase, and the mobile phase flows. It is a liquid chromatograph (1) provided with an analysis unit (4) for separating and analyzing a sample on a channel (6).
　上記第２の実施態様によれば、上述の低圧グラジエント送液システム（２）を用いて移動相の送液を行なうので、３つ以上の液を用いたグラジエント分析を実現できる新規な低圧グラジエント方式の分析システムが提供される。 According to the second embodiment, since the mobile phase is delivered using the low pressure gradient delivery system (2) described above, a novel low pressure gradient method capable of realizing a gradient analysis using three or more fluids. Analysis system is provided.
　　　１　　　液体クロマトグラフ
　　　２　　　低圧グラジエント送液システム
　　　４　　　分析部
　　　６　　　分析流路
　　　８，１０，１２，１４　　　液供給流路
　　　１６　　　切替バルブ（切替機構）
　　　１８　　　送液ポンプ
　　　２０　　　ミキサ
　　　２２　　　制御装置
　　　２４　　　制御部
　　　２６　　　組成設定部
　　　２８　　　混合比率計算部
　　　３０　　　試料注入部
　　　３２　　　分離カラム
　　　３４　　　検出器 1 Liquid Chromatograph 2 Low Pressure Gradient Liquid Delivery System 4 Analyzing Section 6 Analytical Flow Paths 8, 10, 12, 14 Liquid Supply Flow Path 16 Switching Valve (Switching Mechanism)
18 Liquid-sending pump 20 Mixer 22 Control device 24 Control unit 26 Composition setting unit 28 Mixing ratio calculation unit 30 Sample injection unit 32 Separation column 34 Detector

Claims (3)

  1. 　液を収容した容器からそれぞれ液を汲み上げるための３つ以上の液供給流路と、
    　前記液供給流路を介して前記容器から液を汲み上げて送液するための１つの送液ポンプと、
    　前記３つ以上の液供給流路と前記送液ポンプとの間に介在し、前記送液ポンプと連通させる１つの液供給流路を前記３つ以上の液供給流路のうちから選択的に切り替えるための切替機構と、
    　前記送液ポンプによって汲み上げられた液の混合を行なうためのミキサと、
    　ユーザ入力に基づいて、前記ミキサにおいて混合される３つ以上の液の時間帯ごとの混合比率を設定するように構成された組成設定部と、
    　前記ミキサにおいて混合される前記３つ以上の液の時間帯ごとの混合比率を前記組成設定部により設定された混合比率とするために、前記切替機構の切替え動作を制御するように構成された制御部と、を備えた低圧グラジエント送液システム。     Three or more liquid supply channels for respectively pumping the liquid from the container containing the liquid,
    One liquid-sending pump for pumping and sending the liquid from the container via the liquid-supplying channel;
    One liquid supply passage interposed between the three or more liquid supply passages and the liquid supply pump and communicating with the liquid supply pump is selectively selected from the three or more liquid supply passages. A switching mechanism for switching,
    A mixer for mixing the liquids pumped by the liquid feed pump,
    A composition setting unit configured to set a mixing ratio of three or more liquids mixed in the mixer for each time period based on a user input;
    A control configured to control the switching operation of the switching mechanism so that the mixing ratio of the three or more liquids mixed in the mixer for each time period becomes the mixing ratio set by the composition setting unit. Part, and a low-pressure gradient liquid delivery system comprising.
  2. 　前記組成設定部は、前記３つ以上の液を第１グループ及び第２グループからなる２つのグループに分け、前記第１グループに属する液からなる第１溶媒の組成、及び前記第２グループに属する液からなる第２溶媒の組成を設定するとともに、前記第１溶媒と前記第２溶媒との時間帯ごとの混合比率を設定するように構成されており、
    　前記低圧グラジエント送液システムは、前記組成設定部により設定された前記第１溶媒の組成、前記第２溶媒の組成、前記第１溶媒と前記第２溶媒との時間帯ごとの混合比率を用いて、前記時間帯ごとの前記３つ以上の液の混合比率を計算するように構成された混合比率計算部を備え、
    　前記制御部は、前記ミキサにおいて混合される前記３つ以上の液の混合比率を前記混合比率計算部によって計算された混合比率とするために、前記切替機構の切替え動作を制御するように構成されている、請求項１に記載の低圧グラジエント送液システム。     The composition setting unit divides the three or more liquids into two groups of a first group and a second group, and a composition of a first solvent composed of the liquids belonging to the first group and a second group. It is configured to set the composition of the second solvent composed of a liquid and set the mixing ratio of the first solvent and the second solvent for each time zone,
    The low-pressure gradient liquid delivery system uses the composition of the first solvent, the composition of the second solvent, and the mixing ratio for each time zone of the first solvent and the second solvent set by the composition setting unit. A mixing ratio calculator configured to calculate a mixing ratio of the three or more liquids for each of the time periods,
    The control unit is configured to control the switching operation of the switching mechanism so that the mixing ratio of the three or more liquids mixed in the mixer is the mixing ratio calculated by the mixing ratio calculation unit. The low pressure gradient liquid delivery system according to claim 1.
  3. 　請求項１又は２に記載の低圧グラジエント送液システムと、
    　前記低圧グラジエント送液システムにより送液される液の混合液を移動相として用い、前記移動相の流れる流路上で試料の分離分析を行なう分析部と、を備えた液体クロマトグラフ。     A low pressure gradient liquid delivery system according to claim 1 or 2,
    A liquid chromatograph comprising: an analysis unit that uses a mixed liquid of liquids delivered by the low-pressure gradient liquid delivery system as a mobile phase and performs a separation analysis of a sample on a flow path of the mobile phase.
PCT/JP2018/042145 2018-11-14 2018-11-14 Low-pressure gradient liquid delivery system and liquid chromatograph WO2020100233A1 (en)

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