WO2020100233A1 - Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide - Google Patents

Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide Download PDF

Info

Publication number
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
Authority
WO
WIPO (PCT)
Prior art keywords
liquid
mixing ratio
liquids
solvent
pressure gradient
Prior art date
Application number
PCT/JP2018/042145
Other languages
English (en)
Japanese (ja)
Inventor
伊織 大友
覚 渡辺
知広 舎川
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to JP2020556509A priority Critical patent/JP6992912B2/ja
Priority to PCT/JP2018/042145 priority patent/WO2020100233A1/fr
Priority to CN201880097859.5A priority patent/CN112740029B/zh
Publication of WO2020100233A1 publication Critical patent/WO2020100233A1/fr

Links

Images

Classifications

    • 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

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

La présente invention concerne un système de distribution de liquide à gradient basse pression qui comprend : au moins trois canaux d'alimentation en liquide (8, 10, 12, 14) pour aspirer un liquide à partir de chacun des récipients recevant le liquide; une seule pompe de distribution de liquide (18) pour aspirer le liquide à partir des récipients par le biais des canaux d'alimentation en liquide (8, 10, 12, 14); un mécanisme de commutation (16) pour commuter de manière sélective un seul canal d'alimentation en liquide à mettre en communication avec la pompe de distribution de liquide (18) parmi les trois, ou plus, canaux d'alimentation en liquide (8, 10, 12, 14), le mécanisme de commutation (16) étant intercalé entre les trois, ou plus, canaux d'alimentation en liquide (8, 10, 12, 14) et la pompe de distribution de liquide (18); un mélangeur (20) pour mélanger le liquide aspiré par la pompe de distribution de liquide (18); une unité de réglage de composition (26) configurée de sorte à régler un rapport de mélange pour chaque période de temps des trois, ou plus, liquides mélangés dans le mélangeur (20), sur la base d'une entrée d'utilisateur; et une unité de commande (24) configurée de sorte à commander l'opération de commutation du mécanisme de commutation (16) pour rendre le rapport de mélange pour chaque période de temps des trois, ou plus, liquides mélangés dans le mélangeur, le rapport de mélange étant réglé par l'unité de réglage de composition (26).
PCT/JP2018/042145 2018-11-14 2018-11-14 Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide WO2020100233A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2020556509A JP6992912B2 (ja) 2018-11-14 2018-11-14 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
PCT/JP2018/042145 WO2020100233A1 (fr) 2018-11-14 2018-11-14 Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide
CN201880097859.5A CN112740029B (zh) 2018-11-14 2018-11-14 低压梯度送液系统以及液相色谱仪

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/JP2018/042145 WO2020100233A1 (fr) 2018-11-14 2018-11-14 Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide

Publications (1)

Publication Number Publication Date
WO2020100233A1 true WO2020100233A1 (fr) 2020-05-22

Family

ID=70731146

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2018/042145 WO2020100233A1 (fr) 2018-11-14 2018-11-14 Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide

Country Status (3)

Country Link
JP (1) JP6992912B2 (fr)
CN (1) CN112740029B (fr)
WO (1) WO2020100233A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040151594A1 (en) * 2003-01-10 2004-08-05 Allington Robert W. High pressure reciprocating pump and control of the same
JP2010008113A (ja) * 2008-06-25 2010-01-14 Hitachi High-Technologies Corp フローインジェクション分析装置
JP2010502960A (ja) * 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 液体クロマトグラフィー用の多成分、同時、独立多勾配システム
JP2015180884A (ja) * 2010-06-16 2015-10-15 株式会社日立ハイテクノロジーズ 液体混合装置、および液体クロマトグラフ
WO2015172011A1 (fr) * 2014-05-09 2015-11-12 Waters Technologies Corporation Procédés de préparation de mélanges liquides

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6755074B2 (en) * 2001-02-27 2004-06-29 Isco, Inc. Liquid chromatographic method and system
JP3756860B2 (ja) * 2002-08-30 2006-03-15 山善株式会社 液体クロマトグラフ
JP2004138413A (ja) * 2002-10-16 2004-05-13 Shimadzu Corp 液体クロマトグラフ装置及びその送液装置
JP4732960B2 (ja) * 2006-06-07 2011-07-27 ジーエルサイエンス株式会社 グラジェント送液方法及び装置
JP2010085146A (ja) * 2008-09-30 2010-04-15 Hitachi High-Technologies Corp グラジエント送液装置，グラジエント送液システム、および液体クロマトグラフ
CN102309933B (zh) * 2010-07-08 2013-09-04 江苏天瑞仪器股份有限公司 液相梯度混合器
JP5838866B2 (ja) * 2012-03-08 2016-01-06 株式会社島津製作所 送液機構及び液体クロマトグラフ

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040151594A1 (en) * 2003-01-10 2004-08-05 Allington Robert W. High pressure reciprocating pump and control of the same
JP2009162234A (ja) * 2003-01-10 2009-07-23 Teledyne Isco Inc ポンプシリンダ内の減圧体積を決定する方法およびその装置
JP2010502960A (ja) * 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 液体クロマトグラフィー用の多成分、同時、独立多勾配システム
JP2010008113A (ja) * 2008-06-25 2010-01-14 Hitachi High-Technologies Corp フローインジェクション分析装置
JP2015180884A (ja) * 2010-06-16 2015-10-15 株式会社日立ハイテクノロジーズ 液体混合装置、および液体クロマトグラフ
WO2015172011A1 (fr) * 2014-05-09 2015-11-12 Waters Technologies Corporation Procédés de préparation de mélanges liquides

Also Published As

Publication number Publication date
JPWO2020100233A1 (ja) 2021-09-02
JP6992912B2 (ja) 2022-01-13
CN112740029A (zh) 2021-04-30
CN112740029B (zh) 2023-08-04

Similar Documents

Publication Publication Date Title
US11130074B2 (en) Hybrid gradient delivery system and operation
US11573212B2 (en) Flow channel mechanism and liquid chromatograph including the same
JP6696578B2 (ja) 切替バルブ、バイナリポンプ及びそのバイナリポンプを備えた液体クロマトグラフ
US20180272250A1 (en) Method for adjusting a gradient delay volume
WO2018105076A1 (fr) Chromatographe en phase liquide
US10473632B2 (en) Metering device with defined enabled flow direction
EP3642613B1 (fr) Dilution en ligne pour un système de chromatographie en phase liquide utilisant une pompe de dosage d'échantillon
JP2007171034A (ja) グラジエント送液装置
JP2015052592A (ja) 液体クロマトグラフィ装置、液体クロマトグラフィ分析方法、及び液体クロマトグラフィ分析プログラム
US20130340508A1 (en) Mobile phase delivery device and liquid chromatograph
US11879877B2 (en) Binary pump and liquid chromatograph provided with same
US20240060939A1 (en) Sample metering and injection for liquid chromatography
WO2020100233A1 (fr) Système de distribution de liquide à gradient basse pression et chromatographe en phase liquide
JP3172222U (ja) 試料注入ユニット及び液体クロマトグラフ
US10969368B2 (en) Liquid chromatograph
US20210156826A1 (en) Sample injection for liquid chromatography using split solvent flow
JP6672781B2 (ja) 流路機構及びこれを備えた液体クロマトグラフ
US11413555B2 (en) Liquid delivery device and liquid chromatograph equipped with liquid delivery device
JP2004138413A (ja) 液体クロマトグラフ装置及びその送液装置
JP6485300B2 (ja) 送液装置及び液体クロマトグラフ
JP7120335B2 (ja) 液体クロマトグラフおよび液体クロマトグラフを用いた分析方法
US11953474B2 (en) Preparative chromatograph
US11340197B2 (en) Mechanisms and methods for liquid sample introduction into a chromatography system
JP2006118374A (ja) 送液システム
JPS60143760A (ja) 液体クロマトグラフ用グラジエント装置

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 18939967

Country of ref document: EP

Kind code of ref document: A1

ENP Entry into the national phase

Ref document number: 2020556509

Country of ref document: JP

Kind code of ref document: A

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 18939967

Country of ref document: EP

Kind code of ref document: A1