WO2012172382A1 - Procédé et appareil destinés à améliorer la performance de procédés de séparation chromatographique sur colonne - Google Patents

Procédé et appareil destinés à améliorer la performance de procédés de séparation chromatographique sur colonne Download PDF

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Publication number
WO2012172382A1
WO2012172382A1 PCT/HU2012/000049 HU2012000049W WO2012172382A1 WO 2012172382 A1 WO2012172382 A1 WO 2012172382A1 HU 2012000049 W HU2012000049 W HU 2012000049W WO 2012172382 A1 WO2012172382 A1 WO 2012172382A1
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WIPO (PCT)
Prior art keywords
column
chromatographic
mobile phase
outlet
stationary phase
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Ceased
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PCT/HU2012/000049
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English (en)
Inventor
Emil Mincsovics
Tibor BARTOK
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Morovjan Gyorgy
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Morovjan Gyorgy
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Application filed by Morovjan Gyorgy filed Critical Morovjan Gyorgy
Publication of WO2012172382A1 publication Critical patent/WO2012172382A1/fr
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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/24—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the treatment of the fractions to be distributed
    • 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
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces
    • G01N30/6017—Fluid distributors
    • 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
    • G01N30/60—Construction of the column
    • G01N30/6004—Construction of the column end pieces
    • G01N30/603—Construction of the column end pieces retaining the stationary phase, e.g. Frits
    • 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
    • G01N30/60—Construction of the column
    • G01N30/6052—Construction of the column body
    • G01N30/606—Construction of the column body with fluid access or exit ports

Definitions

  • the present invention is related to a method and corresponding apparatus for improving the performance of column chromatographic separation processes and systems used in such processes.
  • the invention can be generally used during column chromatographic separations regardless of the scale or purpose of the separation, i.e. during analytical tests of preparative chromatographic processes.
  • Column liquid chromatography is a separation method wherein the solute mixture to be separated dissolved in the liquid mobile phase is contacted with a fixed, non-miscible stationary phase arranged geometrically in the form of a column.
  • components of the solute mixture to be separated interact with the fixed stationary phase and according to the differences in the equilibrium constants (distribution coefficients) of the interaction, spend different time intervals associated with the stationary phase. Due to the differential distribution between the stationary and the mobile phase, components of the solute mixture to be separated leave the stationary phase separated in time.
  • column liquid chromatography is suitable for determining the composition of solute mixtures as well as separating and isolating the constituents of such mixtures.
  • Performance of a chromatographic separation method depends on several factors, including but not limited to the quality of the stationary and mobile phase, physical structure of the stationary phase.
  • the composition, shape and size of said particles, qualitative and quantitative composition of the mixture to be separated and qualities of the sorbent bed are determining factors regarding the separation.
  • Stationary phases are of high-porosity, highly adsorptive solid particles or liquids immiscible with the mobile phase and coated on the surface of a solid support are generally applied.
  • the size of particles comprising the bed of the stationary phase is usually in the range of a few micrometers to a few hundred micrometers.
  • Shape of the particles is usually spherical or an almost symmetrical spheroid although in some cases, particles of irregular shape are also applied. Pore size distribution, shape and character of the pores and interconnections thereof determine the adsorption processes occurring on the stationary phase as well as the kinetics of the separation significantly.
  • stationary phases have become available which comprise a porous adsorptive layer mecanicsheU" produced on the surface of an essentially non-porous particle mecaniccore").
  • Chemically stationary phases are usually particles of chemically modified inorganic or organic polymers, e.g.
  • silica hydrated silicic acid
  • alumina aluminium oxide
  • zirconia styrene- divinylbenzene copolymers
  • chemically modified derivatives thereof e.g. alkyl-modified silica
  • stationary phases disclosed in the state of the art which comprise one single porous organic or inorganic block- polymerized adsorbent block (a monolithic phase) rather than individual particles.
  • Analytical as well as preparative column chromatographic separations including process chromatography are characterized by the sample amount (weight) separated on the column (sample capacity), separation speed (number of samples separated in a time unit) and resolution characteristic to the separation of subsequently eluted analytes.
  • resolution is a function of the distribution coefficients of the target component and the component having its distribution coefficient closest to that of the target component as well as the band (elution zone) broadening occuring in the separation process.
  • Band broadening during the elution from a chromatographic column can be characterized by efficiency (number of theoretical plates, height equivalent to a theoretical plate, HETP).
  • performance of a chromatographic system or a chromatographic column can be characterized by band broadening and comparison is possible by using a set of test analytes or by having test conditions fixed, between analytes as well.
  • the distribution coefficient (or retention factor) between the stationary and mobile phase and the selectivity between the critical pair of the compounds can be influenced by varying the quality of the stationary phase, the composition of the mobile phase or the temperature.
  • the retention factor is determined by the quality of the stationary phase and the composition of the eluent for a given compound.
  • US Patent No. 3966609 discloses a column chromatographic apparatus comprising a piston at least one end of the chromatographic column rather than a fixed column end piece (outlet element), said piston being moveable in the direction of the longitudinal axis (i.e. axially) of the chromatographic column in order to decrease band broadening originating from the volume change of the stationary phase. Ports or connectors are provided for mobile phase and sample introduction to and withdrawal from the cross-section of a piston.
  • the disadvantage of the method resides in the fact that no moveable piston can be used at the relatively high pressure used during high- performance column chromatographic separations.
  • US Patent No. 4250035 discloses a method and apparatus for compensating for dead volume occurring near the column wall as well as for the inhomogeneous arrangement of the sorbent bed at the column wall to a certain degree.
  • the tubular part of the chromatographic column comprising the column wall is manufactured from a deformable material and a radial pressure is exerted from outside to said cylindrical column wall.
  • the radial pressure has to be kept strictly constant, since changes of the pressure can significantly alter the performance of the chromatographic system.
  • an auxiliary flow of the mobile phase is applied for reducing the loss of efficiency due to dead volume and inhomogeneity of sorbent bed occurring in the proximity of the column wall.
  • Said auxiliary mobile phase flow is introduced into the chromatographic column near the column wall at the sample introduction side independently from the means of sample introduction in order to prevent solute diffusion to the vicinity of the inhomogeneous sorbent bed volume close to the column wall, thus approximating the so-called whilte diameter column" effect.
  • Mobile phase containing analytes eluting from the central cross section of the column close to the longitudinal axis is directed to the detector.
  • the objective of our research-development activity was to develop a method and an apparatus which provides for preventing or decreasing the loss of performance in column chromatographic separations resulting from radial inhomogeneity and wall-effect of the chromatographic column. Said loss of performance is primarily manifested in the decrease of efficiency and resolution.
  • the aim of our work was to provide an arrangement of a chromatographic column which can be easily and robustly applied in existing column chromatographic separation systems known from the state of the art.
  • the separated components can be obtained in greater purity than by using methods according to the state of the art.
  • Figure 1 demonstrates the parts of the column chromatographic system pertinent to the present invention.
  • Figure 2 demonstrates an embodiment of the apparatus according to the present invention wherein the means for directing the mobile phase eluting in the proximity of the column wall and diverting such stream from the central column outlet port are comprised in the outlet fitting element 3 of the chromatographic column.
  • Figure 3 demonstrates an embodiment of the apparatus according to the present invention wherein the means for directing the mobile phase eluting in the proximity of the column wall and diverting said stream are comprised in an insert 14.
  • Figure 4 demonstrates an embodiment of the apparatus according to the present invention wherein the means for directing the mobile phase eluting in the proximity of the column wall are comprised in a filter 9 retaining the stationary phase.
  • a method for improving the performance of column chromatographic separations which comprises transferring a sample into a chromatographic mobile phase and separating sample components in known manner and subsequent to separation, separating and removing the part of the mobile phase eluting from the chromatographic stationary phase in the proximity of the wall of the chromatographic column and detecting, isolating and/or further separating sample components eluted in the portion of the mobile phase eluting from the central part of the radial cross-section of the stationary phase perpendicular to the longitudinal axis thereof. Separation of the mobile phase stream into a part eluted from the proximity of the column wall and a second part eluted from the central axial section of the sorbent is preferably carried out at the exit cross section of said stationary phase.
  • the part of the mobile phase exiting near the column wall or in the central section of the exit cross-section of the stationary phase is diverted at the end of the stationary phase, conducted out separately and discarded or recycled.
  • the outlet port located in the central (axial) part of the column end cross section provides for delivering the mobile phase containing analytes eluted from the more orderly structured central part of the stationary phase into a detector or for further separation or isolation.
  • the central exit outlet of the chromatographic column prepared according to the present invention can be formed in a manner essentially known from the prior art.
  • the outlet comprising means for conducting the portion of the mobile phase exiting in the proximity of the column wall can be arranged in the form of one or more grommets, annular channels, recesses or grooves which are interconnected to an exit connecting port.
  • the position of the outlet means can be determined according to the column diameter, method of column filling or column preparation and the field of application (i. e. analytical or preparative separation).
  • the position and actual arrangement of the outlet port intended for conducting the portion of the mobile phase eluting near the column wall can be modified according to the application area of the chromatographic column as well.
  • the central outlet and the outlet intended for diverting the portion of the mobile phase eluted near the column wall are arranged in the proximity of the contact surface of the stationary phase and the outlet fitting element for collecting the mobile phase exiting from the stationary phase. Accordingly, the location of the central outlet port is in the axis of the chromatographic column (i. e. the central part of the stationary phase), while grommets, annular channels, grooves or recesses collecting the part of the mobile phase exiting from the stationary phase bed near the column wall are connected to a port arranged off-axis, near the column wall.
  • the means intended for conducting the mobile phase can contain additional channels to the annular or concentric liquid collecting channels in order to collect and conduct mobile phase exiting from different radial positions of the stationary phase cross-section perpendicular to the axis of the stationary phase. It is important, however, that the means intended for diverting the portion of the mobile phase, should not cause any flow disturbance, i. e. change of linear velocity profile near the column wall region. Such changes are not desired since they usually result in distortion of band shape and loss of performance.
  • the ratio of the flow rate of the eluent stream entering into the detector and that of the eluent stream entering into the chromatographic column is kept precisely constant.
  • the ratio of the flow rate of the eluent stream entering into the detector and that of the eluent stream entering into the chromatographic column is kept precisely constant.
  • linearity of detection as well as efficacy/resolution of the separation may suffer.
  • the above objective can be achieved by maintaining the flow rate of the diverted eluent stream exiting from the chromatographic column in the proximity of the column wall strictly constant. It has been found that in case of analytical separations, it is sufficient to install a section of tubing (i.e. capillary tube) providing a constant pressure resistance (pressure drop). Pressure drop in chromatographic tubing (i.e. capillaries) depends on the material of said tubing, composition and temperature of the mobile phase, the inner diameter and the length of the tubing which is available from the state of the art, i.e. from commercial vendors or can be determined experimentally using techniques known from the prior art.
  • the advantage of the method according to the present invention resides in the fact that said method does not require an auxiliary mobile phase stream, thus there is no need for modifying the mobile phase delivery system and usually no excess mobile phase consumption occurs.
  • the modification of the chromatographic column is minor and involves the outlet (exit) fitting element or some related smaller parts only ( Figure 1).
  • the modified outlet element, filter or insert can be machined in a simple way according to methods known from the state of the art, e.g. using computer-controlled (CNC) machining.
  • CNC computer-controlled
  • a further advantage of the solution according to the present invention resides in the fact that the flow rate of the mobile phase stream diverted from the outlet fitting element 3 can be simply controlled by changing the pressure drop of the exit tubing (i.e. installing a section of tubing having known pressure drop) or by choking.
  • the method according to the present invention results in improved performance of the chromatographic system.
  • performance the separating ability of the system is meant, which is inversely proportional with the degree band broadening.
  • any methods known for the assessment of resolution or efficacy of a chromatographic system can be used.
  • the efficacy or the height equivalent to a theoretical plate (HETP) can be calculated for each peak (i. e. each sample component).
  • the resolution can also be calculated. Methods for such calculations are known from the state of the art.
  • an apparatus for carrying out the method according to the invention is provided.
  • the scheme of the apparatus is demonstrated by Figure 1, which is principally a chromatographic column containing a stationary phase with modified outlet fitting element 3 according to the present invention.
  • Chromatographic mobile phase is delivered at a constant flow rate by a high-pressure pump according to methods known from the state of the art.
  • the method according to the present invention can be used during isocratic as well as gradient elution.
  • the sample to be separated can be injected into the stream of the mobile phase using any manual or automatic sample injector known from the prior art.
  • the mobile phase stream exiting the sample injector enters the chromatographic column through connection tubing 4 and inlet fitting element 2.
  • the mobile phase stream exits the chromatographic column through outlet fitting element 3.
  • the inlet of the chromatographic column 1 comprises the inlet fitting element 2, whereby the connection tubing 4 and the chromatographic column 1 are attached without dead volume by a pressure-tight seal and by means suitable for retaining the stationary phase.
  • Any inlet fitting element 2 and fitting chromatographic column 1 known from the state of the art are suitable for use in the method according to the present invention after slight modification.
  • Inlet and outlet fitting elements (2,3) are usually attached to the chromatographic column by threads and compression fittings.
  • any other method for pressure-tight connection known from the state of the art e.g. flanged fittings can be used provided that pressure-tight and low or zero dead-volume connections can be established.
  • Connections referred to as ports in the present specification are apertures by which the mobile phase enters or leaves the apparatus. Ports are usually provided with means for establishing pressure-tight and low or zero dead volume connection between the parts of the apparatus, such as a chromatographic column according to the present invention and the interconnecting tubing.
  • such connections can be established by compression screws and conical sealing rings (ferrules).
  • the method according to the present invention can be carried out using a chromatographic column equipped with an outlet fitting element 3 known from the prior art with slight modifications.
  • an outlet element 3 known from the state of the art having a central outlet exit port is provided with means suitable for collecting and conducting the portion of the mobile phase exiting from the chromatographic column 1 in the proximity of the column wall and attached to a second outlet port 6 by a suitable connector.
  • Means for collecting and conducting the portion of the mobile phase exiting from the chromatographic column 1 in the proximity of the column wall can be shaped as one or more grommets, annular or concentric grooves, recesses or channels, which are interconnected by suitable means, e.g.
  • the mobile phase stream exiting the chromatographic column 1 centrally i.e. collaterally to the axis of the column is directed through the connection tubing 5 into a detector or alternatively, for subsequent separation of fractionation.
  • the mobile phase stream exiting the chromatographic column in the proximity of the column wall exits the outlet fitting element 3 through port and connection tubing 6, whereto optionally a flow or pressure controller can be attached.
  • Preferable forms of the means for collecting and conducting the portion of the mobile phase exiting from the chromatographic column 1 in the proximity of the column wall are annular grooves or channels interconnected to one or more outlet ports 6.
  • the preferable cross-section profile is half-circular.
  • Other suitable cross- sectional profiles advantageous from the point of the view of easy and convenient manufacturing are rectangular, triangular or oval (half-elliptical).
  • the width of the annular grooves or channels for collecting and conduction the mobile phase portion leaving the chromatographic column near the column wall is chosen to 0.5 to 40 percent of the inner diameter of the chromatographic column.
  • a particularly preferably range for this width is 5 to 8 percent of the column inner diameter.
  • the depth of the channel is 10 to 500 percent of the width thereof.
  • FIG 2 the most advantageous embodiment of an outlet fitting element 3 is depicted.
  • central port and connection tubing 5 as well as port and connection tubing for conducting the mobile phase exiting near the column wall 6 are attached to outlet element 3 by compression ferrule and screw.
  • Outlet element 3 is attached to a chromatographic column 1 comprising the chromatographic tube 7 and the stationary phase 8 containing therein e.g. in the form of a sorbent bed, are connected with a threaded connection (not shown).
  • a retaining filter 9 is arranged, which is, upon closure of the threaded connection, fringed upon the surface of the stationary phase 8 and the outlet element 3 without any side or circumferential dead volume or clearance.
  • annular groove 10 suitable for collecting the mobile phase is located at a distance smaller than the inner diameter of the chromatographic tube 7 measured from the bore 11 connected to the central outlet port 5, said annular groove 10 communicating to the port 6 through the channel 12.
  • the cross-sectional view of the annular groove 10 at the contacting plane of the filter 9 and outlet element 3 is shown on the right hand side cross-sectional view diagramitA" of Figure 2, wherein the annular groove 10, outlet port 6 and communicating channel 12 are demonstrated together with a compression screw and sealing ring.
  • the embodiment of the present invention demonstrated in Figure 2 can be advantageously used in case of chromatographic columns filled with a bed of granular stationary phase, especially on an analytical scale.
  • a bed of granular stationary phase especially on an analytical scale.
  • a granular or porous block polymer stationary phase of any desirable chemistry can be equally well used.
  • the stationary phase 8 is secured with an insert 13 located inside the outlet fitting element 3 said insert 13 having at least one annular groove 14 on the surface facing towards the stationary phase 8 or towards an optional retaining filter element 9 placed onto the surface of the stationary phase 8.
  • Said annular groove 14 communicates through a channel 12 with a port 15 in order to divert the mobile phase stream exiting from the chromatographic column in the proximity of the column wall.
  • the mobile phase stream exiting from the central port 16 of the outlet element 3 and the bore 11 attached thereto flows through a connection tubing into the detector.
  • the mobile phase collecting annular groove or channel 17 for collecting the mobile phase stream exiting from the chromatographic stationary phase in the proximity of the column wall is formed on the surface of a filter element 9 retaining and sealing the chromatographic stationary phase.
  • a porous block polymer stationary phase is used and the annular groove or channel is formed directly on the exit surface of said whilmonolithic" block polymer stationary phase provided that the outlet element 3 possesses adequately arranged ports.
  • This embodiment is demonstrated in principle in Figure 4 with the modification that the annular collecting groove or channel 17 is formed directly on the surface of the block polymer stationary phase (dotted area) instead of the filter element 9.
  • the embodiments shown in Figures 2 and 3 can be used as well with the modification that no retaining filter 9 is necessary.
  • the method and apparatus according to the present invention can be used for any column chromatographic separation system or stationary phase (e.g. normal, reversed phase; ion exchange, size exclusion chromatography; affinity chromatography, hydrophobic interaction chromatography etc.). It has been found that the method and apparatus according to the present invention can be applied for improving the performance of the chromatographic system not only during analytical but in preparative separations as well even in the case of traditional column when the stationary phase has relative greater particle size (e.g. 63-200 ⁇ ).
  • the use of the method and apparatus is not restricted to the field of elution chromatography; it can be equally well used in displacement and frontal chromatographic separations for improving separation performance as well. The effects of the method and apparatus are demonstrated by the following example.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

L'invention concerne un procédé et un appareil destinés à améliorer la performance des séparation chromatographique sur colonne, qui comprend l'introduction d'un échantillon à séparer dans un courant de phase mobile d'une manière connue et, suite à la séparation chromatographique, la partie de la phase mobile sortant de la colonne chromatographique près de la paroi de colonne est séparée près de coupe transversale terminale de ladite colonne chromatographique perpendiculaire à l'axe de ladite colonne, pendant qu'au même moment, la partie de la phase mobile sortant de la partie centrale de ladite colonne chromatographique près de ladite coupe transversale terminale perpendiculaire et d'un courant constitué par la phase mobile sortant par le centre et soumise à la détection, au fractionnement ou à une nouvelle séparation d'analyte.
PCT/HU2012/000049 2011-06-14 2012-06-14 Procédé et appareil destinés à améliorer la performance de procédés de séparation chromatographique sur colonne Ceased WO2012172382A1 (fr)

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HU1100312A HUP1100312A2 (en) 2011-06-14 2011-06-14 Procedure and equipment for improving of performance characteristics of column chromatography separation processes
HUP1100312 2011-06-14

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WO2012172382A1 true WO2012172382A1 (fr) 2012-12-20

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018508793A (ja) * 2015-02-09 2018-03-29 マックス−プランク−ゲゼルシャフト・ツア・フェルデルング・デア・ヴィッセンシャフテン・エー・ファオ クロマトグラフィー適用におけるスウェプトボリュームおよびデッドボリュームを最小限にするための手段および方法
CN108333283A (zh) * 2017-01-20 2018-07-27 中国科学院上海微系统与信息技术研究所 一种含有流线型椭圆微柱阵列的微色谱柱及其制备方法
CN114858957A (zh) * 2016-10-25 2022-08-05 里珍纳龙药品有限公司 用于色谱数据分析的方法和系统

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JPS62240857A (ja) * 1986-04-14 1987-10-21 Kurita Water Ind Ltd クロマトグラフイ装置
EP0257582A2 (fr) * 1986-08-21 1988-03-02 Ceskoslovenska akademie ved Colonne pour la chromatographie préparative en phase liquide
JP2000088829A (ja) * 1998-09-11 2000-03-31 Shimadzu Corp カラム
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WO2011159232A1 (fr) * 2010-06-15 2011-12-22 Ge Healthcare Bio-Sciences Ab Unité de distribution de fluide

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