WO2004017064A1 - Dispositif de separation de constituants d'echantillons par chromatographie liquide sous pression - Google Patents
Dispositif de separation de constituants d'echantillons par chromatographie liquide sous pression Download PDFInfo
- Publication number
- WO2004017064A1 WO2004017064A1 PCT/FR2003/001663 FR0301663W WO2004017064A1 WO 2004017064 A1 WO2004017064 A1 WO 2004017064A1 FR 0301663 W FR0301663 W FR 0301663W WO 2004017064 A1 WO2004017064 A1 WO 2004017064A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- mobile phase
- sample
- stationary phase
- phase
- injection
- Prior art date
Links
- ICXOGAOKYGLFHU-UHFFFAOYSA-N CCC(CC)CCN Chemical compound CCC(CC)CCN ICXOGAOKYGLFHU-UHFFFAOYSA-N 0.000 description 1
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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/91—Application of the sample
-
- 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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N2030/906—Plate chromatography, e.g. thin layer or paper chromatography pressurised fluid phase
Definitions
- the invention relates to a device for separating the constituents of a sample by liquid chromatography under pressure, of the type known under the name OPLC (Over Pressured Layer Chromatography or Optimum Performance Layer Chromatography).
- OPLC Over Pressured Layer Chromatography or Optimum Performance Layer Chromatography
- This technique consists of depositing a sample at one end of a stationary phase layer formed of a suitable material such as powder or particles of silicate gel, alumina, magnesium silicate, cellulose, polyamide. , etc., which is sealed between two walls to be subjected to an external pressure applied to these walls.
- the components of the sample are separated by entrainment in the stationary phase by means of a mobile phase formed by a pressurized fluid.
- the walls delimiting the stationary phase are equipped with means for injecting the sample into the stationary phase and for supplying the latter in the mobile phase, at a first end of the stationary phase, and include means for collecting sample and mobile phase at the other end of the stationary phase.
- This can include a single sample processing channel, the supply and collection means being formed by transverse grooves in the walls which open onto the ends of the stationary phase.
- several parallel and juxtaposed treatment paths can be defined in the stationary phase between transverse grooves of the ends of the walls, which form the supply and collection means, the different treatment paths being separated from each other by longitudinal partitions.
- the stationary phase can be placed in a separation chamber of an apparatus comprising means mobile phase supply and mobile phase and sample output means, or it can be housed beforehand in a cassette which is then placed in the aforementioned device.
- the flow of mobile phase injected into the stationary phase moves therein in a substantially uniform manner except in the areas of contact with side walls which extend from one end to the other of the stationary phase and which delimit laterally the route of treatment.
- the object of the invention is in particular to remedy this drawback in a simple and effective manner.
- It relates to a device for separating the constituents of a sample by OPLC type chromatography, in which the fronts of the sample constituents are substantially linear over their entire extent and in particular at their ends.
- a device of the aforementioned type comprising a stationary phase formed by an appropriate medium placed between two walls, means for injecting a sample at a first end of the stationary phase, means for supplying in the mobile phase from this end of the stationary phase and from the mobile phase and sample collection means at the opposite end from the stationary phase, at least one sample processing channel being defined in the stationary phase between the means supply and collection means, characterized in that it also comprises means for injecting mobile phase on the longitudinal sides of said treatment channel, at the first end of the stationary phase.
- the invention thus makes it possible to eliminate the edge effects at the ends of the fronts of sample constituents in the stationary phase, since the ends of these fronts are separated from the fixed side walls by mobile phase flows which are devoid of sample, so that a difference in the flow velocity along the side walls no longer affects the separation of the components of the samples.
- the aforementioned means for injecting the mobile phase on either side of the treatment channel are formed at the ends of the means for supplying the stationary phase in the mobile phase.
- Transverse grooves or the like formed at the ends of the stationary phase for supplying the mobile phase can be extended to form the injection means located on either side of the treatment path, so that the phase mobile is also progressing along the sides of the treatment path on either side of it.
- said mobile phase injection means can be independent of a transverse groove forming the means for supplying the treatment path in mobile phase.
- the invention applies both to the case where the stationary phase comprises a single sample processing channel, and to the case where it comprises several parallel juxtaposed sample processing channels, separated longitudinally from one another by channels mobile phase flow, which then have a multiple function of suppression of edge effects, protection of the sample constituents against the external environment and separation of the different processing paths.
- the device according to the invention can be miniaturized on surfaces having a thickness of a few microns and an area of between a few mm 2 and a few hundred cm 2 .
- the invention is also applicable to the case where the stationary phase forms a cylindrical column, mobile phase injection means being provided at one end of this column to form a flow of mobile phase around each sample processing channel in the stationary phase and to remove side effects on the surrounding wall.
- FIG. 1 is a schematic top view of a device according to the invention.
- FIG. 1 is a schematic side view of the device of Figure 1;
- Figures 3 and 4 are schematic views from below of two plastic sheets forming a wall of the device of Figures 1 and 2;
- FIGS. 5 and 6 are partial schematic views on a larger scale and in section along the lines V-V of Figure 3 and VI-VI of Figure 4;
- FIG. 7 is a schematic top view of an alternative embodiment of this device, comprising several parallel and juxtaposed processing paths;
- FIG. 8 is a schematic top view of an alternative embodiment of the device of Figures 1 to 6;
- FIG. 9 is a schematic top view of an alternative embodiment of the device of Figure 7;
- FIG. 10 is a partial schematic view in axial section of another variant of the invention in which the stationary phase forms a cylindrical column;
- FIG. 11 is a schematic top view of the upper disc of the column;
- - Figure 12 is a schematic top view of this disc in section along the line XII - XII of Figure 11;
- FIG. 13 is a schematic bottom of the lower disc of the column
- FIG. 14 is a schematic view of this filter in section along the line XIV - XIV of FIG. 13.
- the reference 10 designates a stationary phase, which is formed of a layer of material enclosed between two walls 12, 14 in a plastic material such as for example poly (tetrafluoroethylene), the stationary phase being formed of monoliths of powder or particles of alumina, silicate gel, magnesium silicate, cellulose, polyamide, etc.
- the stationary phase 10 and the walls 12, 14 are in the form of a sealed cassette, which is placed in a suitable device allowing to exert an external pressure P on the walls 12 and 14 , as indicated by the arrows in FIG. 2.
- the stationary phase layer 10 can be placed inside an apparatus which has the walls 12, 14.
- Mobile phase supply, sample injection and mobile phase and sample collection means are associated with the opposite longitudinal ends of the stationary phase 10, as described in more detail below.
- the mobile phase supply means include a pump 16 or other similar means for pressurizing, the inlet 18 of which is connected to a mobile phase reservoir (here an appropriate liquid) and the outlet of which is connected to a groove transverse 22 which is formed by example in the upper wall 12 and which opens in the vicinity of the side walls delimiting the stationary phase 10, for a flow of mobile phase along the side walls of the stationary phase 10.
- a pump 16 or other similar means for pressurizing the inlet 18 of which is connected to a mobile phase reservoir (here an appropriate liquid) and the outlet of which is connected to a groove transverse 22 which is formed by example in the upper wall 12 and which opens in the vicinity of the side walls delimiting the stationary phase 10, for a flow of mobile phase along the side walls of the stationary phase 10.
- the outlet 26 of the injection means 24 opens into another transverse groove 28 of the upper wall 12, which uniformly distributes the flow rate of the mobile and sample phase over almost the entire width of the stationary phase 10, the groove 28 ending a short distance from the side walls 36.
- another transverse groove 30 is formed in the upper wall 12 and opens to the outside of the latter by an orifice to be connected to means 32 for outputting the liquid phase and possibly sample constituents.
- This groove 30 extends over substantially the entire width of the stationary phase 10.
- the transverse feed groove 22 is extended beyond the ends of the mobile phase distribution groove 28 and of sample, and its ends 40 extend in the immediate vicinity and along the side walls 36, substantially up to the level of the transverse groove 28 for dispensing sample, and form mobile phase injection means oriented in parallel to the side walls 36 in the direction of the transverse collection groove 30, for a mobile phase flow on the side walls 36.
- This flow does not participate in the separation of the constituents of the sample in the stationary phase and does not contain any sample, and moves faster or slower than the mobile phase in the rest of the stationary phase, but eliminates the abovementioned edge effects and protects the treatment path against the external environment.
- one of the walls for example the upper wall 12 is formed from two superimposed sheets 42, 44 of plastic material such as TEFLON (poly (tetrafluoroethylene)) in which the grooves 22, 28 and the corresponding injection orifices are formed.
- plastic material such as TEFLON (poly (tetrafluoroethylene)
- FIG. 3 The lower face or underside of the upper sheet 42 is shown in FIG. 3 and that of the lower sheet 44 is shown in FIG. 4.
- the groove 22 is formed in the lower face of the upper sheet 42 along a transverse edge, and is fed in its middle by a through orifice 46 of the sheet 42, as shown.
- the ends 48 of the groove 22 extend perpendicular to this groove in the direction of the other transverse edge of the sheet 42.
- a through orifice 50 is formed in the sheet 42, a short distance from the orifice 46, and is intended to be connected to the aforementioned outlet 26.
- This orifice 50 opens into a small longitudinal groove 52 of the underside of the sheet 42.
- the groove 52 itself opens onto a through hole 54 of the bottom sheet 44, the underside of which is in contact with the phase stationary 10, has the transverse distribution groove 28.
- the “staircase” supply of the groove 28 makes it possible to limit the impact of the mobile phase flow rate on the stationary phase.
- the ends 48 of the groove 22 formed in the sheet 42 open onto the stationary phase via through orifices 40 in the sheet 44, which can have any desired section or shape and which form the injection means mobile phase along the side walls 36.
- the transverse collection groove 30 is formed in the plate
- outlet means 32 comprising two through orifices formed in the plates 42 and 44.
- Beads of porous sintered material can be arranged in the grooves 28, 30, as well as at the ends 40, to protect the stationary phase and to regulate the flow of mobile phase.
- the stationary phase 10 no longer comprises a single sample processing channel, but several parallel channels 58 which are juxtaposed transversely and which are separated longitudinally from each other by channels 60 d mobile phase flow.
- the device shown in a simplified manner in FIG. 7 comprises a pump 16 for supplying the mobile phase, the outlet 20 of which is connected to a transverse groove 62 for distributing the mobile phase, this groove
- sample injection means 24 which are each associated with a processing channel 58 and whose outputs 26 are connected to transverse distribution grooves 64 provided at the ends of the processing channels 58.
- the feed groove 62 is also connected to small grooves or to injection orifices 66 provided on either side of the distribution grooves 64 and dimensioned to create longitudinal flow paths 60 of the desired width on both sides. and other of each treatment route 58.
- transverse collection grooves 68 receive the mobile phase delivered by the distribution grooves 64 and that injected by the orifices 66. These transverse collection grooves 68 are connected to detection means 70 of a known type.
- the device shown in FIG. 8 differs from that of FIG. 1 in that it comprises orifices 72 formed in the upper wall 12 of the device at the ends of the mobile phase flow paths along the side walls 36, these orifices 72 being in the extension of the transverse collection groove 30.
- the mobile phase flows along the side walls 36, which do not participate in the separation of the components of the sample in the stationary phase, exit the device through the orifices 72 and are not mixed with the sample constituents collected in the groove 30.
- the device shown in FIG. 9 differs from that of FIG. 7 in that the ends of the mobile phase flow paths 60 have orifices of outlet 74 which are independent of the transverse collection grooves 68 formed at the ends of the treatment channels 58.
- FIG. 9 is t identical to that of FIG. 7.
- the invention also applies when the stationary phase forms a cylindrical column of any cross section which is contained in a tube.
- the mobile phase is injected at one end of the stationary phase column, in an annular channel which surrounds the sample injection surface. This removes edge effects between the front of sample constituents and the inner wall of the tube and separates the processing lines from each other.
- An exemplary embodiment of such a device is shown in Figures 10 to 14. It essentially comprises a cylindrical tube 76 of suitable rigid material, in particular steel or of a suitable plastic material such as PEEK (polyetheretherketone), the ends of which threaded receive screwed covers 78 intended to pressurize the stationary phase 80 which fills the tube 76.
- PEEK polyetheretherketone
- the upper cover 78 is supported on an upper disc 82 engaged in the upper end of the tube 76 and comprising supply conduits 84 in sample and in mobile phase and at least one feed pipe 86 in mobile phase.
- the disc 82 is supported on a disc 88 of porous material surrounded by a sealing ring 90 interposed between the disc 82 and the tube 76.
- Chambers 92 are delimited in the disc 88 and separated from each other by partitions watertight 94 transverse and longitudinal.
- Each chamber 92 is supplied with a sample and in mobile phase by a conduit 84 which passes through a transverse partition 94.
- the or each conduit 86 for supplying in mobile phase opens out above the disc 88 between the chambers 92.
- the lower end of the tube 76 likewise comprises a porous lower disk 96 surrounded by a sealing ring 98 interposed between the disk 96 and the tube 76, the stationary phase being supported by the disk 96 and the ring 98.
- the disc 96 is divided into four independent sectors 99 by watertight bulkheads 100 longitudinal.
- the disc 96 and the ring 98 rest on a lower disc 102 engaged in the lower end of the tube 76 and coming to bear on the lower cover 78.
- Conduits 104 carried by the lower disc 102 each connect a sector 99 to means detection exteriors not shown.
- the chambers 92 of the porous upper disc 88 and the sectors 99 of the porous lower disc 96 define in the stationary phase column 80 four sample processing channels, which are parallel and separated from each other and from the tube 76 by mobile phase flows supplied by the above-mentioned conduit (s) 86.
- the mobile phase flows are collected at the output with the sample constituents and the mobile phase coming from the sample processing channels.
- conduits for collecting the aforementioned mobile phase flows which have served to separate the treatment paths from one another and from the tube 76.
- the invention consists in injecting a flow of mobile phase to separate different processing paths from one another and to eliminate edge effects between a fixed wall and the mobile phase which flows in the stationary phase.
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03787832A EP1535057A1 (fr) | 2002-08-02 | 2003-06-03 | Dispositif de separation de constituants d'echantillons par chromatographie liquide sous pression |
AU2003264669A AU2003264669A1 (en) | 2002-08-02 | 2003-06-03 | Device for separating sample components by liquid chromatography under pressure |
JP2004528546A JP2005534937A (ja) | 2002-08-02 | 2003-06-03 | 圧力下の液体クロマトグラフィによって試料成分を分離するための機器 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0209899A FR2843198B1 (fr) | 2002-08-02 | 2002-08-02 | Dispositif de separation de constituants d'echantillons par chromatograhie liquide sous pression |
FR02/09899 | 2002-08-02 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004017064A1 true WO2004017064A1 (fr) | 2004-02-26 |
Family
ID=30129670
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FR2003/001663 WO2004017064A1 (fr) | 2002-08-02 | 2003-06-03 | Dispositif de separation de constituants d'echantillons par chromatographie liquide sous pression |
Country Status (7)
Country | Link |
---|---|
US (1) | US20040020834A1 (fr) |
EP (1) | EP1535057A1 (fr) |
JP (1) | JP2005534937A (fr) |
CN (1) | CN100350245C (fr) |
AU (1) | AU2003264669A1 (fr) |
FR (1) | FR2843198B1 (fr) |
WO (1) | WO2004017064A1 (fr) |
Families Citing this family (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20020187557A1 (en) * | 2001-06-07 | 2002-12-12 | Hobbs Steven E. | Systems and methods for introducing samples into microfluidic devices |
US7261812B1 (en) | 2002-02-13 | 2007-08-28 | Nanostream, Inc. | Multi-column separation devices and methods |
CN100528363C (zh) * | 2002-02-13 | 2009-08-19 | 安捷伦科技有限公司 | 微流体分离柱装置及其制备方法 |
US6936167B2 (en) | 2002-10-31 | 2005-08-30 | Nanostream, Inc. | System and method for performing multiple parallel chromatographic separations |
EP1648582A4 (fr) * | 2003-06-19 | 2010-02-17 | Univ Indiana Res & Tech Corp | Methode et appareil de mise en oeuvre d electrochromatograph ie planaire a pression elevee |
US7028536B2 (en) * | 2004-06-29 | 2006-04-18 | Nanostream, Inc. | Sealing interface for microfluidic device |
US20050032238A1 (en) * | 2003-08-07 | 2005-02-10 | Nanostream, Inc. | Vented microfluidic separation devices and methods |
US8007742B2 (en) | 2005-09-20 | 2011-08-30 | United States Of America As Represented By The Secretary Of Commerce | IRIS digester-evaporator interface |
US7940249B2 (en) | 2005-11-01 | 2011-05-10 | Authentec, Inc. | Devices using a metal layer with an array of vias to reduce degradation |
JP2007163459A (ja) * | 2005-11-18 | 2007-06-28 | Sharp Corp | 分析用マイクロチップ |
US9164111B2 (en) * | 2007-03-12 | 2015-10-20 | Resolved Technologies, Inc. | Device for multiple tests from a single sample |
CN102680638B (zh) * | 2011-03-15 | 2014-04-23 | 上海高佳仪器科技有限公司 | 一种加压薄层色谱预制板的制造方法 |
CN105473021B (zh) * | 2013-03-15 | 2018-01-19 | 智能专利有限责任公司 | 可穿戴设备及相关系统 |
CN107271602B (zh) * | 2017-06-05 | 2019-02-15 | 山东省中医药研究院 | 一种消除薄层色谱边缘效应的装置 |
CN111366674A (zh) * | 2020-04-13 | 2020-07-03 | 杭州旭昱科技有限公司 | 一种oplc加压薄层色谱仪多油缸加压装置 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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DE2800464A1 (de) * | 1978-01-05 | 1979-07-12 | Bayer Ag | Verfahren zur erzeugung hochbelegter substanzzonen im sorbens von duennschichtchromatographieplatten |
GB2078127A (en) * | 1980-06-03 | 1982-01-06 | Mueszeripari Muevek Lab | Linear overpressured thin-layer chromatographic apparatus |
Family Cites Families (12)
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US3915856A (en) * | 1974-12-20 | 1975-10-28 | Holger Meyer | Method of carrying out preparative thin-layer chromatography and apparatus for use in the method |
HU184065B (en) * | 1979-12-06 | 1984-06-28 | Mueszeripari Muevek Lab | Cromatographic layer sheet for a pressurized layer chromatographic equipment |
US4469601A (en) * | 1981-03-17 | 1984-09-04 | Varex Corporation | System and apparatus for multi-dimensional real-time chromatography |
US4346001A (en) * | 1981-06-12 | 1982-08-24 | Labor Muszeripari Muvek | Linear overpressured thin-layer chromatographic apparatus |
US4348286A (en) * | 1981-07-17 | 1982-09-07 | Analtech, Incorporated | Large sample thin layer chromatography |
HU189133B (en) * | 1982-04-28 | 1986-06-30 | Labor Mueszeripari Muevek,Hu | Special layer plate and/or layer plate system for overpressure multi-layer chromatography |
HU190910B (en) * | 1983-08-16 | 1986-12-28 | Reanal Finomvegyszergyar,Hu | Method for producing glue suitable for fixing sorbent layer of pressurized one and multiple layer chromatography |
JPS6042653A (ja) * | 1983-08-17 | 1985-03-06 | Shionogi & Co Ltd | クロマトグラフィ−・プレ−ト |
GB2173125B (en) * | 1985-04-04 | 1989-04-19 | Mueszeripari Muevek Lab | Apparatus for overpressured thin-layer chromatographic technique |
US5116495A (en) * | 1987-09-11 | 1992-05-26 | Ottosensors Corporation | Capillary chromatography device |
FR2803220B1 (fr) * | 2000-01-04 | 2002-07-05 | Bionisis | Dispositif et procede de traitement d'un echantillon par separation sur une phase stationnaire, sous flux force controle |
CN2488066Y (zh) * | 2001-07-16 | 2002-04-24 | 常州市新祥天然产物分离设备有限公司 | 天然产物分离纯化用层析柱 |
-
2002
- 2002-08-02 FR FR0209899A patent/FR2843198B1/fr not_active Expired - Fee Related
-
2003
- 2003-01-17 US US10/346,224 patent/US20040020834A1/en not_active Abandoned
- 2003-06-03 AU AU2003264669A patent/AU2003264669A1/en not_active Abandoned
- 2003-06-03 CN CNB038210800A patent/CN100350245C/zh not_active Expired - Fee Related
- 2003-06-03 WO PCT/FR2003/001663 patent/WO2004017064A1/fr not_active Application Discontinuation
- 2003-06-03 JP JP2004528546A patent/JP2005534937A/ja active Pending
- 2003-06-03 EP EP03787832A patent/EP1535057A1/fr not_active Withdrawn
Patent Citations (2)
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DE2800464A1 (de) * | 1978-01-05 | 1979-07-12 | Bayer Ag | Verfahren zur erzeugung hochbelegter substanzzonen im sorbens von duennschichtchromatographieplatten |
GB2078127A (en) * | 1980-06-03 | 1982-01-06 | Mueszeripari Muevek Lab | Linear overpressured thin-layer chromatographic apparatus |
Non-Patent Citations (1)
Title |
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NYIREDY S: "The bridge between TLC and HPLC: overpressured layer chromatography (OPLC)", TRAC, TRENDS IN ANALYTICAL CHEMISTRY, ANALYTICAL CHEMISTRY. CAMBRIDGE, GB, vol. 20, no. 2, February 2001 (2001-02-01), pages 91 - 101, XP004249002, ISSN: 0165-9936 * |
Also Published As
Publication number | Publication date |
---|---|
JP2005534937A (ja) | 2005-11-17 |
CN1678905A (zh) | 2005-10-05 |
CN100350245C (zh) | 2007-11-21 |
AU2003264669A1 (en) | 2004-03-03 |
US20040020834A1 (en) | 2004-02-05 |
FR2843198A1 (fr) | 2004-02-06 |
FR2843198B1 (fr) | 2004-10-15 |
EP1535057A1 (fr) | 2005-06-01 |
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