JP2011149919A - Column for intermediate pressure liquid chromatography, and pre-pack column - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a column for intermediate pressure liquid chromatography used repeatedly. <P>SOLUTION: This column for intermediate pressure liquid chromatography includes a transparent or translucent straight body section 1 made of resin forming a cylindrical chamber, a tip 2 having a passage that is connected to one end of the straight body section 1, connects one end of the chamber to the outside, and has a diameter smaller than the chamber, a pair of filters 3 and 4 that have liquid permeability, are arranged at one end and the other end of a charged layer when a filler is filled into the chamber, and prevent leakage of the filler, and a plug 5 for removably blocking the other end of the chamber. The straight body section 1 is made of fluororesin, and a member for regulating the moving of the filter 4 toward the other end of the chamber is provided. <P>COPYRIGHT: (C)2011,JPO&INPIT

Description

  The present invention relates to a medium pressure liquid chromatography column, and more particularly to a medium pressure liquid chromatography column suitable for repeated use.

  Separation and purification of the compound in the laboratory is performed by liquid chromatography using a column in which a column tube is packed with a particulate filler. This liquid chromatography may be performed under medium pressure conditions in which the eluent is pumped. As a column used for such medium pressure liquid chromatography, for example, a transparent or translucent column body formed of polypropylene, high-density polyethylene, polysulfone, or polyvinyl chloride, and a packing material are confined in the column body. There is known a column having a pair of filters for this purpose and a resin head having a through hole inside and in close contact with the open end of the column main body (see, for example, Patent Document 1).

  In the experimental stage, examination of separation conditions and sample adjustment may not be sufficient, so it is desirable to be able to confirm the state during separation and to be easy to handle. In these respects, the column is excellent.

  However, the column is not sufficiently resistant to chemicals in the column body, and in particular when used in normal phase liquid chromatography where the concentration of the organic solvent in the eluent is high, it must be discarded after one use. Sometimes.

  On the other hand, in chemical experiments, methods and instruments that further reduce the environmental burden have been studied. In addition, in the medium pressure liquid chromatography column, since the packing material is selected according to the substance to be separated, an expensive packing material such as a packing material for optical resolution may be used. The filler can generally be used repeatedly. Expensive fillers are desirably used repeatedly from an economical viewpoint in addition to reducing environmental burdens. From these viewpoints, a reusable column for medium pressure liquid chromatography has been particularly desired in recent years, and in this respect, the above-mentioned column still has room for study.

Japanese Patent Laid-Open No. 7-198701

  The present invention provides a medium pressure liquid chromatography column that can be used repeatedly.

  The inventors of the present invention have intensively studied a column for medium pressure liquid chromatography that has high resistance to chemicals and is advantageous for washing a packing material for reuse, and has completed the present invention.

  That is, the column for medium pressure liquid chromatography of the present invention is a column for medium pressure liquid chromatography made of a fluororesin for filling a particulate filler.

Further, the present invention provides a fluororesin-made straight body part that forms a cylindrical chamber and a diameter smaller than that of the chamber that is connected to one end of the straight body part and connects one end of the chamber to the outside. A front end portion having a passage and a liquid permeability, and disposed at one end and the other end of a filling layer formed when the chamber is filled with a filler, for preventing leakage of the filler The medium pressure liquid chromatography column having a pair of filters is provided.

  In the present invention, the tip portion is connected to one end of the chamber, and a tapered portion that gradually decreases from the diameter of the chamber, and a passage that connects the tip portion of the taper portion and communicates the taper portion with the outside. An intermediate pressure liquid chromatography column is provided.

  The present invention also provides the medium pressure liquid chromatography column, wherein a ratio of an axial length of the chamber to a diameter of the chamber is 2 or more.

  The present invention also provides the medium pressure liquid chromatography column further comprising a plug that detachably closes the other end of the chamber.

  The present invention also provides the medium pressure liquid chromatography column, wherein the stopper further includes a passage communicating between the chamber and the outside when the stopper closes the other end of the chamber with the stopper.

  The plug may further include a recess that forms a recess with respect to the chamber when the other end of the chamber is closed with the plug, and the passage communicates the recess with the outside. A pressure liquid chromatography column is provided.

  The present invention also provides the medium pressure liquid chromatography column further comprising a regulating portion that regulates movement of the filter arranged at the other end of the packed bed in the direction of the other end of the chamber.

  Further, according to the present invention, when the restricting portion closes the other end of the chamber with the plug, the contact protrudes from the plug into the chamber and contacts the filter disposed at the other end of the packed bed. The medium pressure liquid chromatography column is provided.

  The present invention also provides the medium pressure liquid chromatography column, wherein the stopper is a movable stopper capable of adjusting a position of closing the chamber in an axial direction of the straight body portion.

  The present invention also provides a medium pressure liquid chromatography column in which a particulate packing material is packed in a medium pressure liquid chromatography column having the straight body portion, the tip portion, the filter, the stopper, and the restriction portion. The filter is disposed on one end and the other end of a packed bed made of a filler contained in the chamber, and the movement of the filter on the other end side toward the other end of the chamber is A pre-packed column regulated by a regulation unit is provided.

  The present invention also provides the prepacked column, wherein the filler has a particle size of 10 μm or more.

  The present invention also provides the prepacked column, wherein an organic solvent is further accommodated in the chamber.

  Moreover, this invention provides the said prepack column in which the said filler has the separating agent for optical isomers as a separating agent.

  The present invention also provides the prepack column having a movable stopper capable of adjusting a position of closing the chamber in an axial direction of the straight body portion as the stopper and the restricting portion.

  Hereinafter, in the present specification, the medium pressure liquid chromatography column of the present invention or the prepacked column of the present invention is also simply referred to as “the column of the present invention”.

  The medium pressure liquid chromatography column of the present invention is a fluororesin column for filling a particulate filler. The column of the present invention is a column that can be filled with a particulate filler and has a strength and a structure that can be used for medium pressure liquid chromatography, and is a fluororesin molded product or a fluororesin component. Can be configured by assembly.

  The column of the present invention is smaller than the chamber, which is connected to one end of the straight body portion and a straight body portion made of a fluororesin that forms a cylindrical chamber, and connects one end of the chamber to the outside. In order to prevent leakage of the filler by being disposed at one end and the other end of the filling layer formed when the inside of the chamber is filled with a filler, having a tip portion having a passage having a diameter and liquid permeability It is preferable to have a pair of filters from the viewpoint of repeated use.

  The straight body portion forms a cylindrical chamber. The straight body portion is preferably formed in a cylindrical shape, but the outer shape is not particularly limited. It is preferable from the viewpoint of observing the state of the room that the straight body part has a light transmittance that allows the state of the inside to be confirmed when visible light or ultraviolet light is irradiated. The light transmittance of the straight body portion can be expressed by the transmittance of visible light (wavelength 400 to 780 nm) or haze (cloudiness). The visible light transmittance of the straight body portion is preferably 0.5% or more and more preferably 1% or more in a plate-shaped test piece having a thickness of 3 mm formed of the material of the straight body portion. Preferably, it is more preferably 2% or more. The haze of the straight body part is preferably less than 50% in the test piece. More specifically, the straight body portion preferably has a visible light transmittance of 0.5% or more in the test piece, more preferably 1% or more, and further preferably 2% or more. More preferably, the visible light transmittance of the test piece is 2% or more, and the haze of the test piece is less than 50%. The light transmittance of the straight body portion can be measured using a normal apparatus capable of measuring the transmittance with visible light.

  The straight body portion is formed of a fluorine resin. Examples of the fluororesin include vinylidene fluoride (PVDF), polychlorotrifluoroethylene (PCTFE), polytetrafluoroethylene (PTFE), ethylene-tetrafluoroethylene copolymer (ETFE), and perfluoroethylene propylene copolymer (FEP). And perfluoroalkoxyalkanes (PFA). The fluororesin is preferably PVDF, PCTFE, PFA, or PTFE from the viewpoint of ease of molding, mechanical strength, and transparency.

The wall thickness of the straight body portion can be determined according to the use conditions (pressure) of the column of the present invention. For example, the use pressure of the column of the present invention is 10 kgf / cm ² (9.8 × 10 ⁵ Pa) or less. In this case, from the viewpoint of pressure resistance and mechanical strength, it is preferably 0.7 to 50.0 mm, more preferably 0.9 to 20.0 mm, and 0.9 to 10.0 mm. More preferably, it is 1.0 to 5.0 mm.

  As for the size of the chamber, the ratio of the axial length of the chamber to the diameter of the chamber is preferably 2 or more from the viewpoint of obtaining sufficient separation performance under the use conditions of the column of the present invention. It is more preferably 5 or more, and further preferably 3.5 or more. On the other hand, from the viewpoint of convenience of use of the column of the present invention, the ratio is preferably 25 or less, more preferably 20 or less, and even more preferably 18 or less.

The distal end portion has a passage having a diameter smaller than that of the chamber, which is connected to one end of the straight body portion and connects one end of the chamber and the outside. The tip portion can be formed detachably with the straight body portion, or can be formed integrally with the straight body portion. The tip portion can be formed of the same material as that of the straight body portion, or can be formed of a material different from that of the straight body portion. As the tip portion, for example, a so-called tapered portion that is connected to one end of the chamber and gradually decreases from the diameter of the chamber, and a passage that is connected to the tip of the tapered portion and communicates the tapered portion with the outside, is so-called. A syringe-type configuration may be mentioned.

  The taper portion is formed by cutting the eluent easily from the chamber, preventing air accumulation at the tip portion when the column of the present invention is used, and cutting the tip portion integrally with the straight body portion. It is preferable to have a taper angle of 120 to 150 degrees with respect to the axis of the chamber from the viewpoint of easily discharging the shavings when forming. The interior of the passage may be formed with a detachable connecting portion such as a screw or luer lock structure on the outer periphery or inner periphery of the tip of the passage so that the tip can be connected directly to the pipe or via a joint. This is preferable from the viewpoint of easy cleaning for repeated use of the packed bed.

  The filter has liquid permeability. Further, the filter is disposed at one end and the other end of the filling layer formed when the filler is filled in the chamber in order to prevent the filler from leaking from the chamber. At least one pair (two or more) of the filters is used. Each filter may be the same or different. The filter may be flexible or stretchable, or may be rigid. Further, in each filter, a plurality of filters may be overlapped and used as one filter.

  As the filter, a circular, disk-shaped, or cylindrical filter having substantially the same diameter as the chamber can be used. In addition, as the filter, a member having sufficient fineness to collect the filler is used. Examples of such a filter include a disk-shaped or cylindrical glass filter, a disk-shaped or cylindrical resin filter, a disk-shaped or circular filter paper, glass wool, and a sponge.

  The column of the present invention may further have a configuration other than the configuration described above. Examples of such other configurations include a plug that detachably plugs the other end of the chamber, and a regulating portion that regulates movement of the filter disposed at the other end of the packed layer in the other end direction of the chamber. And the flange part provided in the other end of the outer peripheral surface of the said straight body part is mentioned.

  The stopper plugs the other end of the chamber in a detachable manner. It is preferable to further include a stopper from the viewpoint of storage stability in the room. The plug is preferably a plug that seals the other end of the chamber from the viewpoint of preventing evaporation of the solvent in the chamber. It is preferable from the viewpoint of facilitating washing for repeated use of the column of the present invention that the stopper further has a passage communicating the interior and the exterior when the other end of the chamber is closed with the stopper. . This passage may be freely opened and closed, or may be opened during use.

  Further, the stopper may be a movable stopper capable of adjusting the position for closing the chamber in the axial direction of the column, or may be a fixed stopper whose position for closing the chamber is unchanged in the axial direction of the column. The movable stopper is preferable from the viewpoint of maintaining the filling state of the filler by moving the position closing the chamber toward one end or the other end of the filling layer to further press the filling layer. In addition, when the movable plug is a movable plug that can close the chamber in close contact with the end of the packed bed and does not allow the filler to pass through, the use of the filter can be omitted.

The plug further includes a recess that forms a recess in the chamber when the other end of the chamber is closed with the plug, and the passage is a plug that connects the recess and the outside. It is preferable from the viewpoint of easily forming the passage during use. In addition, the plug having the concave portion is preferable from the viewpoint of using a convex portion formed around the concave portion as a contact portion in a regulating portion described later. Further, the stopper having the recess can insert a filter medium such as a filter, a net, and a fiber lump into the recess, and stains due to washing for repeated use of the column of the present invention using such a filter medium. From the viewpoint of collecting

  The restricting part restricts movement of the filter disposed at the other end of the packed bed in the other end direction of the chamber. It is preferable to further have a regulating part from the viewpoint of performing washing of the packed bed for repeated use by backwashing the solvent in the direction opposite to the liquid flow direction during separation and purification. The restricting portion may be formed by a protrusion on the inner peripheral wall of the chamber, a protruding edge provided around the inner peripheral wall of the chamber, or an annular member inserted into the chamber, which is formed integrally with the straight body portion. it can.

  The restricting portion preferably has an annular shape or a radial shape in a transverse direction of the chamber and a shape lacking a part thereof from the viewpoint of uniformly contacting the filter. Moreover, it is preferable from a viewpoint of the ease of handling that the said control part is a member inserted from the other end of a chamber and being fixed in the specific position in a room | chamber interior. As such a restricting portion, for example, when the other end of the chamber is closed with a stopper, which will be described later, the protrusion protrudes from the stopper into the chamber and comes into contact with the filter disposed at the other end of the packed bed. A contact part.

  The contact portion preferably has elasticity from the viewpoint of preventing movement of the filter and filler on the other end side.

The prepacked column of the present invention is used for medium pressure liquid chromatography. Here, the medium pressure liquid chromatography refers to column chromatography in which an eluent is supplied by a pump at a pressure of 1 to 10 kgf / cm ² or less.

  The prepack column of the present invention is formed by filling the column of the present invention with a particulate filler. The prepack column of the present invention can be configured by, for example, filling the column of the present invention having the straight body portion, the tip portion, the filter, the plug, and the regulating portion with a filler. In such a prepacked column of the present invention, the filter is disposed at one end and the other end of the packed bed made of the filler accommodated in the chamber, and the filter on the other end side toward the other end of the chamber. The movement is regulated by the regulation unit. The prepack column of the present invention is formed by placing one of the filters in the chamber, filling a predetermined amount of particulate filler, placing the other filter in the chamber, and mounting the stopper. Can do. Filling with the filler can be performed by a dry filling method in which the chamber is filled with the filler as it is, or by a wet filling method in which the chamber is filled with the filler together with the solvent.

  The particle size of the filler is preferably 10 μm or more and more preferably 10 to 200 μm from the viewpoint of obtaining sufficient separation performance and suppressing pressure loss when using the prepacked column of the present invention. More preferably, it is 20-100 micrometers. As the particle size of the filler, an average particle size measured with a normal particle size measuring device can be adopted, but it may be a catalog value.

  Examples of the filler include a supported filler composed of a carrier such as silica gel and a separating agent supported on the carrier, and a separating agent filler composed of particles of the separating agent. The carrier-type filler may be a filler in which the carrier directly carries the separation agent, or the carrier physically or chemically carries the separation agent via other components such as a surface treatment agent. It may be a filler.

Examples of the carrier include inorganic carriers such as silica, alumina, magnesia, glass, kaolin, titanium oxide, silicate, and hydroxyapatite, and organic carriers such as polystyrene, polyacrylamide, and polyacrylate. The carrier is preferably porous from the viewpoint of increasing the optical resolution for the target. As the inorganic carrier, a carrier that is surface-treated with an organosilicon compound having an amino group or a glycidyl group is known, and such a carrier can also be used as a carrier in the present invention.

  As the separating agent, either a low molecular separating agent or a high molecular separating agent can be used. Examples of the low molecular separation agent include a ligand exchange type separation agent, a charge transfer (π-π) type separation agent, a hydrogen bond type separation agent, an inclusion type separation agent, and an ion bond type separation agent. Examples include a separating agent, an intercalating type separating agent, a crown ether or a derivative thereof, and a cyclodextrin or a derivative thereof. Examples of the polymer separating agent include polysaccharide derivatives, polyamides, polymethacrylic acid esters, polyacrylamides, proteins, and tartaric acid derivatives. Examples of the polysaccharide derivatives include cellulose phenyl carbamate derivatives, cellulose phenyl ester derivatives, amylose phenyl carbamate derivatives, and amylose phenyl ester derivatives. The phenyl group in these derivatives may have one or more substituents selected from the group consisting of hydrocarbons having 1 to 20 carbon atoms and halogen.

  The filler is preferably a filler excellent in stability of separation performance that can be used repeatedly or an expensive filler that is preferably used repeatedly. Examples of the filler include a filler having a separating agent for optical isomers having an optical resolution ability as a separating agent. Examples of such a filler include a ligand exchange type separating agent and a crown. Examples of the filler include ethers or derivatives thereof, cyclodextrins or derivatives thereof, polysaccharide derivatives, polymethacrylic acid esters, or proteins.

  In the prepack column of the present invention, the organic solvent is further accommodated in the chamber, so that the use conditions of the prepack column of the present invention can be stabilized early, the packing state of the filler can be stabilized, and air bubbles can be mixed into the packed bed. It is preferable from the viewpoint of prevention. The organic solvent may be one kind or a mixed solvent of two or more kinds.

  The prepack column of the present invention can be used for separation of substances by supplying an eluent from the other end of the straight body part at a predetermined pressure, and analyzing and collecting the liquid discharged from the passage at the tip part. . The prepack column of the present invention can be washed by passing a washing solvent through the packed bed in the same direction as the eluent supply direction or in the opposite direction. From the viewpoint of enhancing the cleaning effect, it is preferable that the column is cleaned by passing a cleaning solvent through the packed bed in a direction opposite to the eluent supply direction. For washing the column, for example, the stopper is attached to the other end of the straight body portion, a passage for the stopper is formed, and a cleaning solvent is supplied at a predetermined pressure from the passage of the tip portion. The liquid can be discharged from the passage of the stopper. The eluent and the washing solvent may be the same or different. Further, the pressure for supplying the eluent and the pressure for supplying the cleaning solvent may be the same or different.

Since the prepack column of the present invention is excellent in chemical resistance of the straight body portion, a liquid having high solubility (polarity) can be used as an eluent or a cleaning solvent. Both the eluent and the solvent for washing may be one kind or a mixture of two or more kinds of solvents. Examples of the eluent include alcohols such as methanol, ethanol, and 2-propanol, esters such as methyl acetate and ethyl acetate, tetrahydrofuran (THF), ethyl ether, tert-butyl methyl ether (MTBE), and 1,4. -Ethers such as dioxane, alkanes such as n-hexane, iso-hexane, n-heptane and cyclohexane, halogen solvents such as chlorobutane, chloroform, dichloromethane (methylene chloride) and trichloroethylene, acetamide and N, N- Acetamides such as dimethylacetamide (DMAc); aromatic hydrocarbons such as benzene, toluene and xylene; nitriles such as acetonitrile; aprotic polar solvents such as dimethylsulfoxide and dimethylformamide; Emissions such as water, diethylamine, amines such as monoethanolamine and triethylamine, and can be used an acid such as acetic acid and propionic acid. Among the solvents, acids and bases can be added in a small amount to the eluent from the viewpoint of stabilizing the separation object. As the solvent for cleaning, for example, alcohols such as ethanol can be used. The eluent and the cleaning solvent may contain an acid or an alkali as long as the separation performance of the filler is expressed.

  Since the prepack column of the present invention can be used repeatedly, it can be suitably used for optical resolution and purification of the product from the crude product. Moreover, since the prepack column of the present invention is excellent in chemical stability of the straight body portion, it can be suitably used for normal phase liquid chromatography in which the eluent is generally composed of an organic solvent.

  Since the column of the present invention is made of a fluororesin, it can provide a medium pressure liquid chromatography column that can be used repeatedly.

  In the present invention, it is more effective from the viewpoint of repeated use to have the straight body part, the tip part, and the filter.

  In the present invention, it is more effective from the viewpoint of storage stability in the room to further include a plug that detachably closes the other end of the room.

  Further, in the present invention, it is more preferable from the viewpoint of sufficient cleaning of the column of the present invention that the filter further includes a restricting portion that restricts movement of the filter arranged at the other end of the packed bed in the direction of the other end of the chamber. More effective.

  Further, in the present invention, the distal end portion is connected to one end of the chamber, and has a tapered portion that gradually decreases from the diameter of the chamber, and a passage that is connected to the distal end of the tapered portion and communicates the tapered portion with the outside. This is even more effective from the viewpoints of easy manufacture of the column of the present invention, ease of liquid discharge, and prevention of air accumulation.

  In the present invention, it is more effective that the ratio of the axial length of the chamber to the diameter of the chamber is 2 or more from the viewpoint of sufficient separation performance and suppression of pressure loss.

  In the present invention, when the other end of the chamber is blocked with the stopper, the restricting portion protrudes into the chamber from the stopper and contacts the filter disposed at the other end of the packed bed. It is even more effective from the viewpoint of easily regulating the installation of the filter on the other end side and the movement of the filter on the other end side.

  In the present invention, the stopper further includes a passage that communicates the chamber with the outside when the other end of the chamber is closed with the stopper, so that the column can be easily washed for repeated use. Is even more effective.

  In the present invention, the stopper further includes a recess that forms a recess with respect to the chamber when the other end of the chamber is closed with the stopper, and the passage communicates between the recess and the outside. It is more effective from the viewpoint of purifying the column by washing for repeated use of the column.

Further, the prepack column of the present invention is a column of the present invention having the straight body portion, the tip portion, the filter, the stopper, and the restriction portion, and is filled with a particulate filler, and one end and the other end of the packed bed. And the movement of the filter on the other end side in the direction of the other end of the chamber is restricted by the restricting portion. Therefore, it is used for a medium pressure liquid chromatography column that can be used repeatedly. be able to.

  In the present invention, it is more effective that the particle size of the filler is 10 μm or more from the viewpoint of sufficient separation performance and suppression of pressure loss.

  In the present invention, the organic solvent is further contained in the chamber, so that the prepack column of the present invention can be stabilized early, the packing state of the filler can be stabilized, and bubbles can be prevented from being mixed into the packed bed. More effective from the viewpoint.

  Moreover, in this invention, it is much more effective from the viewpoint of the economic effect by repeated use of an expensive filler that the said filler has the separating agent for optical isomers as a separating agent.

It is a figure which shows one Embodiment of the column of this invention. It is a figure which shows the straight body part 1 and the front-end | tip part 2 of the column of FIG. It is a figure which shows the cross section at the time of detachment | desorption of the stopper 5 of the column of FIG. It is a figure which shows the other form of the straight body part 1 and the front-end | tip part 2. FIG. It is a figure which shows the 1st form of the connection of the channel | path 18 and the further channel | path. It is a figure which shows the 2nd form of the connection of the channel | path 18 and the further channel | path. It is a figure which shows the 3rd form of the connection of the channel | path 18 and the further channel | path. It is a figure which shows the 4th form of the connection of the channel | path 18 and the further channel | path. It is a figure which shows the cross section of the other form of the straight body part. It is a figure which shows the cross section of the further another form of the straight body part. It is a figure which shows the other form of the stopper. It is a figure which shows the further another form of the stopper. It is a figure which shows another form of the stopper. It is a figure which shows other embodiment of the column of this invention. It is a figure which shows the cross section of the stopper 45 of the column of FIG. It is a figure which shows the form at the time of isolation | separation of the column of FIG. 14, and refinement | purification. It is a figure which shows the form at the time of washing | cleaning of the column of FIG. It is a figure which shows the form at the time of the preservation | save of the column of FIG. It is a figure which shows the cross section of further another embodiment of the column of this invention. It is a figure which decomposes | disassembles and shows the movable stopper 75 of the column of FIG. It is sectional drawing which shows the mounting state of the movable stopper in the case of the packing length longer than the packing length of the column of FIG. It is sectional drawing which shows the mounting state of the movable stopper in the case of the packing length shorter than the packing length of the column of FIG. It is a figure which decomposes | disassembles and shows the other form of the movable stopper 75. FIG. It is a figure which shows the other form of the inner stopper 79 of the movable stopper 75. FIG. It is a figure which shows the further another form of the inner stopper 79 of the movable stopper 75. FIG. It is a figure which shows the further another form of the inner stopper 79 of the movable stopper 75. FIG. FIG. 20 is a cross-sectional view showing the column of FIG. 19 having a movable stopper 95. It is a figure which disassembles and shows the movable stopper 95. FIG. 6 is a cross-sectional view showing an example of a state in which the movable plug 95 is mounted. FIG. It is sectional drawing which shows the other form of the movable stopper 95. FIG. It is a figure which shows the cross section of further another embodiment of the column of this invention. It is a figure which shows the modification of the column of FIG. 1 is a diagram showing a chromatogram obtained in Example 1. FIG. 6 is a diagram showing a chromatogram obtained in Example 2. FIG.

The column of the present invention is shown, for example, in FIG.
The column in FIG. 1 is connected to one end of a straight body portion 1 made of a fluororesin made of a fluororesin, which is a fluororesin, and connects one end of the chamber to the outside. A tip 2 having a passage having a diameter smaller than that of the chamber, and a liquid-permeable and disposed at one end and the other end of a filling layer formed when the chamber is filled with a filler. It has a pair of filters 3 and 4 for preventing the leakage of the agent, and a plug 5 that detachably closes the other end of the chamber.

  The straight body 1 is a cylindrical body made of vinylidene fluoride (PVDF). The straight body 1 is formed such that the ratio of the length of the chamber in the axial direction to the diameter of the chamber is 4. The straight body portion 1 has a uniform thickness of 3 mm. As shown in FIG. 2, an annular flange portion 6 that protrudes from the outer peripheral surface is formed at the other end of the outer peripheral surface of the straight body portion 1.

  The distal end portion 2 is formed integrally with the straight body portion 1, is connected to one end of the chamber, and is connected to the tapered portion 7 that gradually decreases from the diameter of the chamber, the distal end of the tapered portion 7, and the tapered portion. 7 and a passage 8 communicating with the outside. The taper angle in the taper portion 7 is 146 °.

  The filters 3 and 4 are porous disks made of polytetrafluoroethylene (PTFE). The diameter of the disk is approximately the same as the diameter of the chamber. The filter 3 is a filter disposed on one end side, and the filter 4 is a filter disposed on the other end side. The filter 3 is disposed at one end of the straight body portion by the taper portion 7. In addition to the porous PTFE disk described above, a SUS mesh filter or a sintered metal filter can be used for the filters 3 and 4.

  The stopper 5 is made of silicon rubber. As shown in FIG. 3, the stopper 5 includes a disk portion 9, a first cylindrical portion 10 connected to one surface of the disk portion 9, and a second surface connected to the other surface of the disk portion 9. And a cylindrical portion 11. The outer diameter of the first cylindrical portion 10 is equal to or smaller than the diameter of the chamber, and gradually decreases as the distance from the one surface of the disk portion 9 increases. As described above, the outer peripheral surface of the first cylindrical portion 10 forms a taper that decreases toward the tip. The outer diameter of the second cylindrical part 11 is substantially the same as the diameter of the disk part 9. The diameter of the disk portion 9 is the same as or slightly larger than the outer diameter of the flange portion 6.

  On the other hand, the front chamber is filled with a filler formed by supporting an amylose derivative on silica gel as a particulate filler. The average particle diameter of this filler is 20 μm. The filler is filled by placing the filter 3 in the chamber and then filling a predetermined amount of filler. Thereafter, the filter 4 is arranged.

  The plug 5 inserts the first cylindrical portion 10 from the other end of the straight barrel portion 1 and closes the other end of the quality by folding back the second cylindrical portion 11 toward the straight barrel portion 1 (FIG. 1). ). The tip of the first cylindrical portion 10 is in contact with the filter 4 and presses the filter 4 toward one end. Thus, the 1st cylindrical part 10 is a control part which controls the movement of the filter 4 to the other end direction of the said chamber. The tip of the first cylindrical portion 10 is annular, and the inside of the first cylindrical portion 10 forms a concave portion that is recessed with respect to the filter 4.

In the column of FIG. 1, the stopper 5 is removed, the sample is supplied from the other end of the straight barrel portion 1, and the other end of the straight barrel portion 1 is connected to a pump for supplying an eluent (for example, methanol). By supplying the liquid at an intermediate pressure (for example, 2 kgf / cm ² ) and collecting the liquid discharged from the passage 8 of the tip 2, it is used for separation and purification of specific components from the mixture.

The column shown in FIG. 1 used for separation and purification is connected to a pump 8 for supplying a cleaning solvent (for example, ethanol) and a passage 8, and a fiber lump such as cotton or a filter inside the first cylindrical portion 10 of the stopper 5 A stopper 5 is attached to the other end of the straight body 1, and a hole is formed in the center of the disk portion 9 to communicate the inside of the first cylindrical portion 10 and the inside of the second cylindrical portion 11. Cleaning can be performed by supplying a cleaning solvent from the passage 8 and discharging it from the hole of the plug 5. It is also possible to form the hole in a female screw hole and separately connect a connector to the female screw hole. In this case, the eluent is supplied at an intermediate pressure (for example, 2 kgf / cm ² ) by connecting to a pump that supplies the eluent with the stopper 5 mounted on the column, and is discharged from the passage 8 of the tip 2 in FIG. It is also possible to separate and purify specific components from the mixture by collecting the liquid.

  The washed column of FIG. 1 may be dried and stored as it is, or the solvent for washing in the column may be replaced with an appropriate liquid such as an eluent, and an appropriate cap is attached to the end of the passage 8. It may be stored in a state filled with liquid by mounting and closing the hole of the stopper 5 with a sealing member such as a sealing film. The column of FIG. 1 after washing can be used again for separation and purification of substances.

  The column shown in FIG. 1 is excellent in chemical resistance because the straight body portion 1 and the tip portion 2 are made of PVDF, and always contains an eluent composed of an organic solvent and a cleaning solvent having a high dissolution power. However, sufficient transparency and mechanical strength can be obtained. In addition, the plasticizer may ooze out from polypropylene, but oozing out from such a resin is also prevented. Furthermore, since the friction on the surface is smaller than that of polypropylene, the stopper 5 is easy to adhere to the inner wall of the chamber and has excellent sealing properties. Furthermore, since the straight body part 1 and the front end part 2 have transparency, it is possible to observe the inside of the room, find an air reservoir in the packed bed, and appropriately deal with it.

  Since the column of FIG. 1 has the taper portion 7, the liquid that has passed through the filter 3 fills the taper portion 7 and is easily discharged during use, so that air accumulation in the taper portion 7 can be prevented. Moreover, since it has the taper part 7, the movement to the taper part 7 side of the filter 3 is controlled, and collapse of a packed bed is prevented.

  In the column of FIG. 1, since the average particle diameter of the filler is 20 μm or more, the pressure loss during liquid passage can be reduced, and the axial direction of the chamber with respect to the diameter of the chamber in the straight body portion 1 Since the ratio of the lengths is 2 or more, it is easy to obtain a sufficient degree of separation of the substance to be separated.

  The column of FIG. 1 can seal the chamber because the stopper 5 is made of silicon rubber having elasticity and being chemically stable. Moreover, since the 1st cylindrical part 10 in the stopper 5 becomes a control part with respect to the filter 4, it can prevent collapse of a filling layer, and since the 1st cylindrical part 10 presses the filter 4 to one end side, This is effective from the viewpoint of preventing leakage of the packed bed. Further, since the first cylindrical portion 10 forms a recess with respect to the filter 4, when cleaning the column of FIG. 1, a member for collecting dirt discharged by the cleaning can be packed in the recess, which is suitable for cleaning the column. It is.

  Since the column of FIG. 1 has the flange portion 6, the second cylindrical portion 11 in the plug 5 can be easily locked to the flange portion 6, which is effective from the viewpoint of preventing the plug 5 from falling off.

The form shown in FIG. 4 may be sufficient as the straight body part 1 and the front-end | tip part 2. FIG. The form of FIG. 4 has the straight body part 1 and the front-end | tip part 12 connected to the end. The distal end portion 12 has a tapered portion 7 that continues from the chamber, and a passage 18 that communicates with the tapered portion 7 and the outside. The distal end portion 12 is a cylindrical body whose outer peripheral surface is continuous with the outer peripheral surface of the straight body portion 1. The passage 18 has a female screw hole with an enlarged diameter at the tip, and a connector can be separately connected to the tip. In these respects, the distal end portion 12 and the passage 18 in FIG. 4 are different from the distal end portion 2 and the passage 8 in FIG.

  The female screw hole of the passage 18 can be connected to a connector or an adapter that is used under medium pressure conditions such as a syringe barrel, whereby a further passage can be connected to the passage 18. For example, as shown in FIGS. 5 and 6, a further passage can be connected to the passage 18 by connecting a tube connector having a male thread that is screwed into the female screw hole. Alternatively, as shown in FIG. 7, a first luer adapter having a male screw and a male luer that are screwed into a female screw hole, a second luer adapter having a female luer and a female screw connected to the male luer, and A further passage can be connected to the passage 18 by means of a tube connector threaded into the female thread. Alternatively, as shown in FIG. 8, a third luer adapter having a male screw and a female luer that are screwed into a female screw hole, a fourth luer adapter having a male luer and a female screw connected to the female luer, and A further passage can be connected to the passage 18 using a tube connector.

  The embodiment shown in FIG. 4 can be easily manufactured as compared with the embodiment shown in FIG. 1 when a cylindrical fluorine-based resin is formed by cutting. Further, since the connector of FIG. 4 can be connected to the female screw hole of the passage 18, a supply pipe for supplying the cleaning solvent when the cleaning solvent is supplied at an intermediate pressure when cleaning the column. It is effective from the viewpoint of preventing the deviation.

  In the form of FIG. 1, the restricting portion is formed in the stopper 5, but the restricting portion may be provided in the straight body portion 1. Examples of such a restricting portion include the forms shown in FIGS. 9 and 10. The form of FIG. 9 has the straight body part 21 and the convex part 22 currently provided in the inner peripheral wall of the said chamber. The straight body portion 21 is different from the straight body portion 1 of FIG. The convex part 22 is provided in the position where the filter 4 arrange | positioned at the other end of a packed bed should be arrange | positioned. In the straight body portion 21 having the convex portion 22, a filter having flexibility such as a filter paper or a resin filter having a circular shape or a disk shape having substantially the same diameter as the chamber is used for the filters 3 and 4.

  The form of FIG. 9 can form a control part integrally with a straight body part. Regardless of the attachment of the plug 5, the movement of the filter 4 in the direction of the other end of the chamber can be restricted.

  The form of FIG. 10 has the straight body part 31 and the recessed part 32 currently provided in the inner peripheral wall of the said chamber. The straight body portion 31 is different from the straight body portion 1 of FIG. The recess 32 is also provided at a position where the filter 4 disposed at the other end of the packed bed is to be disposed. In the straight body portion 31 having the concave portion 32, the filter 4 has a circular or disk shape having a diameter larger than the diameter of the chamber, smaller than the diameter of the concave portion 32, and smaller in thickness than the width of the concave portion 32. A flexible filter such as a filter paper or a resin filter is used.

  The form of FIG. 10 can also form a control part integrally with a straight body part similarly to the form of FIG. In the form of FIG. 10, the movement of the filter 4 in the axial direction of the chamber can be regulated regardless of the wearing of the stopper 5. Further, in the form of FIG. 10, a filter having no flexibility can be used as the filter 3.

Moreover, the form shown in FIGS. 11-13 may also be sufficient as the stopper 5. FIG.
The plug 15 shown in FIG. 11 is made of, for example, silicon rubber. The plug 15 has a hook-shaped cross-section that is bent toward the first cylindrical part 10 after protruding from the peripheral edge of the disk part 9 to the plug 5 instead of the second cylindrical part 11. A stop edge 16 is provided. When the stopper 15 is mounted, the flange portion 6 is fitted to the locking edge 16. The plug 15 also functions in the same manner as the plug 5 of FIG.

The plug 25 shown in FIG. 12 is also made of, for example, silicon rubber. The plug 25 includes a truncated cone-shaped plug body 26, a cylindrical recess 27 having a diameter smaller than the diameter of the distal end surface formed on the distal end surface of the plug body 26, and the recess 27 penetrating the stopper body 26. A passage 28 that opens to the bottom surface and the other end surface of the plug body 26, protrudes in a direction parallel to the other end surface from the other end edge of the plug body 26, then protrudes toward the tip of the plug body 26, and further to the plug body 26 A locking edge 29 having a hook-like cross-sectional shape is formed. The circular diameter at the distal end of the plug body 26 is smaller than the diameter of the chamber, and the circular diameter at the proximal end of the plug body 26 is larger than the diameter of the chamber. When the plug 25 is mounted, the distal end portion of the plug body 26 contacts the filter 4 and presses the filter 4 toward one end of the chamber. Further, when the stopper 25 is mounted, the flange portion 6 is fitted to the locking edge 29.

  Since the plug 25 is always open, the eluent can be supplied at an intermediate pressure while the plug 25 is mounted, and the filler can be washed while the plug 25 is mounted. Further, since the plug 25 also has the concave portion 27 at the tip, similarly to the plug 5, for example, a fiber lump or a filter for collecting dirt to be washed out can be packed in the concave portion 27 and used for cleaning the filler. .

  The plug 35 shown in FIG. 13 is made of, for example, a fluorine-based resin. The plug 35 includes a cylindrical plug body 36 and an O-ring 37 that is fitted to the outer peripheral surface of the plug body 36. The diameter of the plug body 36 is 0.1 to 1.0 mm smaller than the diameter of the chamber. The stopper body 36 is formed with a cylindrical recess 38 having a diameter smaller than the diameter of one end face of the stopper body. Further, a recess having a depth about half the thickness of the O-ring 37 is provided on the outer peripheral surface of the plug body 36, and the O-ring 37 is fitted in the recess. When the plug 35 is mounted, one circular end edge of the plug body 36 contacts the filter 4 and the O-ring 37 is in close contact with the inner peripheral surface of the chamber. The other end surface of the plug body 36 has a thickness of 1.0 to 10.0 mm.

  The plug 35 can block the other end of the chamber while restricting the movement of the filter 4 with a simple configuration. Further, since the plug body 36 can be formed of a rigid material, the plug 35 can be formed of a material having excellent chemical resistance such as a fluorine resin. Furthermore, since the other end surface of the plug body 36 is formed thin, the plug 35 can be used for cleaning the filler by making a hole in the other end surface of the plug body 36. Furthermore, since the plug 35 also has a concave portion 38 at the tip, like the plug 5, a collecting member such as a fiber lump or a filter for collecting dirt to be washed out is accommodated in the concave portion 38, and Can be used for cleaning.

  The plugs 15, 25, and 35 are also provided with through holes in the same manner as the plug 5, and the other end of this hole is formed in a female screw hole, and a connector is separately connected to the female screw hole, so that these plugs are connected directly to the barrel. It is possible to separate and purify specific components from the mixture while being attached to the other end of the unit.

The column of the present invention may have the form shown in FIG.
The column of FIG. 14 includes a straight body part 41 forming a cylindrical chamber, a tip part 42 provided continuously with one end of the straight body part, filters 43 and 44 for preventing leakage of the filler, And a plug 45 for detachably closing the other end of the chamber. The straight body portion 41 is formed of the same material and transparency as the straight body portion 1. The straight body portion 41 has screw portions 46 and 47 that are detachable connecting portions at both ends, and concave portions 48 and 49 that are provided at both ends of the chamber in order to fit the filters 43 and 44. In addition, the same filler as FIG. 1 is filled between the filters 43 and 44 in the chamber.

  The distal end portion 42 is connected to the other screw portion 51 to be screwed to the screw portions 46 and 47, a tapered portion 52 formed continuously to the screw portion 51, and formed to be continuous to the tapered portion 52. And a passage 53 that communicates with each other.

The filters 43 and 44 are circular or disc-shaped filter paper or resin filters having a diameter larger than the diameter of the chamber, smaller than the diameter of the recesses 48 and 49, and smaller than the width of the recesses 48 and 49. It is a filter which has flexibility, such as.

  As shown in FIG. 15, the plug 45 includes a disk portion 55 having substantially the same diameter as the outer diameter of the straight body portion 41, a first cylindrical portion 56 that stands up from the center portion of the disk portion 55, and the disk portion 55. A second cylindrical portion 57 that rises from the periphery, and another screw portion 58 that is formed at the tip of the inner peripheral surface of the second cylindrical portion 57 and is screwed to the screw portions 46 and 47. ing. The first cylindrical portion 56 has an outer diameter smaller than the diameter of the chamber, protrudes from the disk portion 55 substantially in the same manner as the second cylindrical portion 57, and is made of an elastic material such as silicon rubber. Is formed. When the plug 45 is attached, the tip of the first cylindrical portion 56 abuts on and presses the filter 44. The disk part 55, the second cylindrical part 57, and the screw part 58 are made of, for example, a fluorine resin such as PTFE.

  When the column shown in FIG. 14 is used for separation and purification, a second straight body 61 is connected instead of the stopper 45 as shown in FIG. The second straight body portion 61 is made of the same material as the straight body portion 1 and has the same transparency. The second straight body portion 61 has another screw portion 62 that is screwed to the screw portions 46 and 47 at one end of the inner peripheral surface. The second straight body portion 61 is screwed to the other end of the straight body portion 41 by the screw portion 62. At the time of separation and purification, the eluent is supplied from the other end of the second straight body portion 61 by a pump.

  The column of FIG. 14 changes the direction of the straight body 41 and cleans the threaded portion 47 of the other end of the straight body 41 and the threaded portion 51 of the tip 42 when cleaning the filler, as shown in FIG. The screw portion 46 at one end of the straight body portion 41 and the screw portion 62 of the second straight body portion 61 are screwed together, and a cleaning solvent is supplied from the other end of the second straight body portion 61 by a pump. To do.

  The column of FIG. 14 can be suitably stored after the washing by attaching plugs 45 to both ends of the straight body portion 41 as shown in FIG.

  Alternatively, in the column of FIG. 14, similarly to the stopper 5, a hole penetrating the disk portion 55 is formed in the central portion of the disk portion 55 of the stopper 45, and the opening on the other end side of this hole is formed into a female screw hole. One or both of one end and the other end of the straight body portion 41 are closed with a plug 45 provided with a female screw hole, and a separate connector is connected to the female screw hole of the plug 45 to separate or purify specific components from the mixture. Alternatively, the column can be washed.

  In the column of FIG. 14, the front end portion 42, the plug 45, and the second straight body portion 61 are detachable from the straight body portion 41, and the straight body portion 41, the front end portion 42, the plug 45, and the second Since each of the straight body portions 61 is mounted by the same connecting portion, the separation and purification use and the washing use can be properly used only by changing the direction of the straight body portion 41. This is effective from the viewpoint of omitting the work of recombination of the apparatus between cleaning and cleaning.

  Further, in the column of FIG. 14, since the straight body part 41, the tip part 42, the plug 45, and the second straight body part 61 are mounted by the same connecting part, only the packed layer is sealed or liquid-sealed. Can be saved.

  Further, the column of FIG. 14 is more effective from the viewpoint of preventing the leakage of the packing material and the collapse of the packed bed because the first cylindrical portion 56 of the plug 45 contacts the filters 43 and 44 when the plug 45 is mounted. It is.

The column of the present invention may have the form shown in FIG.
The column in FIG. 19 is connected to one end of a straight body 71 made of a fluororesin (PFA) that forms a cylindrical chamber, and connects one end of the chamber to the outside. A tip 72 having a passage with a smaller diameter than the chamber; and a liquid permeability, disposed at one end and the other end of the packed bed formed when the chamber is filled with the filler, A pair of filters 73 and 74 for preventing leakage, and a movable plug 75 for detachably closing the other end of the chamber are included. On the other end of the outer peripheral surface of the straight body portion 71, a screw portion 76 into which the movable plug 75 is screwed is formed.

  The distal end portion 72 is integrated with the straight body portion 71, is connected to one end of the chamber, and is tapered to a tapered portion 77 that gradually decreases from the diameter of the chamber, and is connected to the distal end of the tapered portion 77. And a passage 78 communicating with the outside. For example, the passage 78 has a female screw hole whose diameter is increased at the tip, and a connector can be separately connected to the female screw hole.

  Each of the filters 73 and 74 is a disk-like filter having the same diameter as the chamber, and is, for example, a PTFE filter.

  As shown in FIGS. 19 and 20, the movable plug 75 is inserted into the chamber, an inner plug 79 inserted into the chamber, first and second O-rings 80 and 81 fitted on the inner plug 79, and the chamber. A cylindrical holding tube 82 fitted to the inner plug 79 and the other end of the inner plug 79 are inserted, and a threaded portion of the straight body portion 71 is in contact with the other end of the holding tube 82 fitted to the inner plug 79. And an end cap 83 fastened to the other end of the straight body portion 71. The movable plug 75 is also made of a fluorine resin except for the O-ring.

  The inner plug 79 includes a cylindrical body 84, a flange portion 85 formed in one end of the cylindrical body 84, and a groove provided around the circumferential surface of the cylindrical body 84 in which the holding cylinder 82 is externally fitted. 86 and a passage 87 that penetrates the inner plug 79 in the axial direction of the cylindrical body 84. A circular recess 88 having a diameter smaller than the diameter of the chamber is formed on one end face of the flange portion 85 and constitutes one end of the passage 87. The passage 87 has a female screw hole whose diameter is enlarged at the other end, and a connector can be separately connected to the female screw hole.

  The first O-ring 80 is externally fitted to the cylindrical body 84 so as to contact the flange portion 85. The second O-ring 81 is fitted in the groove 86.

  The holding cylinder 82 is a cylindrical body, and at one end thereof, a tapered surface is formed by gradually increasing the diameter from the inner periphery to the outer periphery. When the presser cylinder 82 is externally fitted to the cylindrical body 84, the presser cylinder 82 contacts the first O-ring 80, and the inner peripheral wall of the presser cylinder 82 contacts the second O-ring 81. It is formed as follows.

  The end cap 83 includes a cylindrical portion 89 having an outer diameter larger than that of the straight body portion 71, a disk-shaped top plate 90 that closes the other end of the cylindrical portion 89, and a circular opening 91 formed at the center of the top plate 90. And have. A screw portion 92 that is screwed with the screw portion 76 of the straight body portion 71 is formed on the inner peripheral surface of the cylindrical portion 89. The diameter of the opening 91 is larger than the outer diameter of the cylindrical body 84 and smaller than the outer diameter of the holding cylinder 82.

  The length of the screw portion 76 in the axial direction of the straight body portion 71 is equal to or longer than the length of the screw portion 92 in the axial direction of the end cap 83. Further, the axial length of the inner plug 79 is such that when the inner plug 79 is inserted from the other end of the straight body portion 71, the other end of the inner plug 79 is connected to the end cap 83. The length protrudes from the opening 91. Further, the axial length of the pressing cylinder 82 is such that the filler is filled in the chamber, and when the inner plug 79 is inserted from the other end of the straight barrel 71, the other end of the pressing cylinder 82 is the straight barrel 71. It protrudes from the other end, and is in contact with the top plate 90 of the end cap 83 fastened by the screw portion 76.

For example, the column in FIG. 19 is filled with a filler up to a position E1 at one end of the threaded portion 76 in the chamber. A filter 74 is disposed at the other end of the packed bed in the room. The first and second O-rings 80, 81 are arranged at predetermined positions on the inner plug 79, the presser cylinder 82 is externally fitted to the cylindrical body 84, and the inner plug 79 so that the flange portion 85 abuts on the filter 74. Is inserted from the other end of the straight body portion 71, and the end cap 83 is fastened to the straight body portion 71 while the other end of the inner plug 79 protruding from the other end of the straight body portion 71 is inserted into the opening 91. A movable stopper 75 is attached. As the end cap 83 is fastened, the holding cylinder 82 is pressed toward one end of the straight body 71, and the inclined surface of the holding cylinder 82 presses the first O-ring 80 toward the inner wall of the straight body 71, Between the inner wall and the outer peripheral surface of the inner plug 79 is sealed with a first O-ring 80, and the other end of the chamber is closed with a movable plug 75.

  The column of FIG. 19 supplies an eluent and a sample solution to the packed bed from the passage 87 connected to the connector in the female screw hole or from the other end of the straight body 71 with the movable stopper 75 removed. Can be used to separate compounds in a sample. In the column shown in FIG. 19, the packed bed is washed (backwashed) by supplying a washing solvent to the packed bed through a passage 77 connected to the connector in the female screw hole, for example, with the movable stopper 75 attached. can do.

  Further, in the column of FIG. 19, the movable plug 75 has the position of the inner plug 79 in the axial direction of the straight body portion 71 according to the position of the other end of the packed bed and the threadable length of the screw portions 76 and 92. Can be changed. For example, as shown in FIG. 21, the column shown in FIG. 19 has an actual filling amount larger than the planned filling amount of the filler, or the filling length increases due to the additional filling of the filler. Even when the end position deviates from the initial position E1 to E2 on the other end side, the other end of the chamber can be closed by the movable plug 75 while the packed bed is pressed.

  Further, in the column of FIG. 19, by using an inner plug that does not have the passage 87, or a plug (for example, a rubber plug or a luer lock) that seals the other end of the passage 87 with respect to the inner plug 79 is further mounted. By doing so, the chamber can be closed liquid-tightly.

  Further, for example, as shown in FIG. 22, the column of FIG. 19 is filled with the packed bed, or the other end side of the packed layer becomes dirty and the other end side of the packed layer is cut away, so that the packing length is reduced. Even when the position of the other end of the packed bed is deviated from E1 to E3 on the one end side of E1, the movable plug 75 is further tightened to press the packed bed in the pressed state. Can close the other end of the chamber.

  As shown in FIG. 23, the movable stopper 75 is a stopper in which the holding cylinder 82 is integrally provided on the outer periphery of the opening 91 inside the end cap 83 and the holding cylinder 82 and the end cap 83 are integrated. Good.

  Further, as shown in FIG. 24, a disc-shaped filter 93 that fits into the recess 88 may be inserted into the recess 88 of the flange portion 85 in the inner plug 79. According to such a configuration, the filter 74 can be omitted in the column of FIG.

  Further, in place of the depression 88, a depression 94, which is a radially formed groove, may be formed on one end face of the flange portion 85 in the inner plug 79, as shown in FIG. The one end surface may be a flat surface having no depression as shown in FIG.

Furthermore, as shown in FIGS. 27 and 28, the movable stopper 75 may be a stopper that can fix the relative positional relationship between the inner stopper and the end cap in the axial direction of the straight body portion 71. The movable plug 95 shown in FIGS. 27 and 28 is a movable plug except that it further includes a screw portion 96 formed on the outer peripheral surface of the other end of the cylindrical body 84 of the inner plug 79 and a nut 97 screwed into the screw portion 96. 75 and the same configuration. The threaded portion 96 is formed from the other end of the cylindrical body 84 with a length larger than the length that the cylindrical body 84 protrudes from the other end of the end cap 83 when the movable plug 95 is attached.

  The movable plug 95 is attached to the other end of the straight barrel portion 71 by the same operation as the movable plug 75 until the end cap 83 is fastened to the straight barrel portion 71. In the movable stopper 95, a nut 97 is further fastened to the cylindrical body 84 protruding from the end cap 83. By fastening the nut 97, the position of the inner plug 79 is fixed with respect to the end cap 83 in the axial direction of the straight body portion 71. For example, displacement of the inner plug 79 due to vibration is prevented, and the inner plug 79 and the filling layer are prevented. Is more effective from the viewpoint of preventing the filler from leaking and maintaining the filling state of the filler.

  In addition, since the movable plug 95 can fix the position of the flange portion 85 at an arbitrary position in the axial direction of the straight body portion 71, the separation end and the other end surface of the filter 74 are separated as shown in FIG. It is also possible to provide a gap D that allows passage of the eluent between the end face on one end side of the flange portion 85 facing this. The formation of such a gap during separation and purification means that when the eluent from the passage 87 is passed through the packed bed through the filter 74, the column in the radial direction of the column is formed at the other end of the packed bed. This is even more effective from the viewpoint of uniformly dispersing the eluent to the inner surface (the other end edge of the packed bed) or the vicinity thereof.

  For example, as shown in FIG. 30, the movable plugs 75 and 95 can be configured to have only the first O-ring 80 by omitting the second O-ring 81.

  The column of the present invention may be the column shown in FIG. The column in FIG. 31 has the same configuration as the column in FIG. 19 except that it has a cylindrical straight body portion 100 and a fixing plug 101 that closes one end of the cylindrical straight body portion 100 instead of the straight body portion 71.

  The straight body portion 100 has a screw portion 102 on the outer peripheral surface of one end portion. The fixing plug 101 includes a cylindrical portion 103 having an outer diameter larger than that of the straight body portion 100, a disc 104 that closes one end of the cylindrical portion 103, a circular recess 105 formed on the other end surface of the disc 104, And a passage 106 penetrating the center of the plate 104. A threaded portion that is screwed into the threaded portion 102 is formed on the inner peripheral surface of the cylindrical portion 103, and a groove 107 is provided around one end of the inner peripheral surface of the cylindrical portion 103.

  The recess 105 is formed in a circular shape having a diameter larger than the inner diameter of the straight body portion 100 and smaller than the outer diameter of the straight body portion. The recess 105 accommodates a disc-shaped filter 108 that fits into the recess 105. The diameter of the front end portion of the passage 106 is enlarged, and this front end portion is formed as a female screw hole to which a connector can be connected. An O-ring 109 is fitted in the groove 107. The screw part 102 is formed in the axial direction of the straight body part 100 to have a length equal to or longer than the length of the screw part on the inner peripheral surface of the cylindrical part 103.

  When the fixing plug 101 is fastened to the threaded portion 102 of the straight body portion 100, the filter 108 closes one end of the straight body portion 100, and the one end portion of the straight body portion 100 and the O-ring 109 are in close contact with each other. One end of the straight body 100 is closed by 101. By using such a fixing plug 101, one end of the straight body 100 can be closed openably.

  In the column of FIG. 31, as shown in FIG. 32, a movable stopper 110 may be used instead of the fixed stopper 102. The movable stopper 110 has the same configuration as the movable stopper 75, for example. According to such a configuration, one end of the straight body portion 100 can be freely opened and closed, and also on one end side of the straight body portion 100, the position of one end of the packed bed and the screwable length of the threaded portion. Accordingly, the position of the inner plug of the movable plug 110 in the axial direction of the straight body portion 100 can be changed, which is more effective from the viewpoint of maintaining the filling state of the filler.

[Example 1]
Using the column shown in FIG. 1, optical resolution of trans-stilbene oxide (t-SO) was performed. CHIRALPAK AD (registered trademark of Daicel Chemical Industries, Ltd.) was used as the filler. The particle size of the filler was 20 μm and the ratio of the packed bed length to the chamber diameter was 3.9.

  The column was attached to a column chromatography apparatus (YFLC-A1-580, manufactured by Yamazen Co., Ltd. The column temperature was 25 ° C. and the detection wavelength was 254 nm. 18.0 mL of methanol was used as an eluent in the column. 1 mL of a sample having a t-SO concentration of 50 g / L was driven in. The amount of t-SO that was driven in once was 50 mg. A sample having a concentration of 50 g / L was injected with 2 mL, and the amount of t-SO input was 100 mg, and the obtained chromatogram is shown in FIG.

  Thus, the column of this example can be applied to optical resolution using an eluent of 100% methanol.

[Example 2]
A mixed solvent of n-hexane and 2-propanol (n-hexane / 2-propanol = 90/10 (volume ratio)) was used as the eluent, the sample concentration was changed, and the sample injection amount was increased. In the same manner as in Example 1, t-SO optical resolution was performed. In this example, 40 mL of a sample having a t-SO concentration of 10 g / L was injected. The amount of t-SO implantation is 400 mg. Further, 60 mL of a sample having a t-SO concentration of 10 g / L was injected. At this time, the amount of t-SO implantation is 600 mg. The obtained chromatogram is shown in FIG.

  Thus, the column of this embodiment can be applied to optical resolution using an eluent with low polarity. In addition, by using an eluent having a more appropriate composition in this way, the amount of sample can be increased, and more optically resolved components can be obtained by a single injection. Even in such a large amount of sample implantation, it is possible to perform appropriate optical resolution with a good component separation state.

  In recent years, attention has been paid to reducing the environmental load, and there is a tendency to reduce the environmental load even in the field of research. In the field of research, inexpensive instruments may be used disposable from the viewpoint of the reliability and convenience of the experimental results. However, from the viewpoint of reducing the environmental burden, such usage is not preferred and is not specified. This may be a cause of hindering the use of expensive experimental materials such as In addition to the functions of the conventional product, the present invention can be used repeatedly in normal phase chromatography by enhancing the functionality of a medium pressure liquid chromatography column that is usually provided at a low price. It is possible to use packing materials that were not used in the conventional products, and it is expected that the applications in medium-pressure liquid chromatography in the research field will be expanded and research results will be expanded.

1, 21, 31, 41, 71, 100 Straight body part 2, 12, 42, 72 Tip part 3, 4, 43, 44, 73, 74, 93, 108 Filter 5, 15, 25, 35, 45 Plug 6 , 85 Flange part 7, 52, 77 Tapered part 8, 18, 28, 53, 78, 87, 106 Passage 9, 55 Disk part 10, 56 First cylindrical part 11, 57 Second cylindrical part 16, 29 Stop edge 22, 48, 49 Convex part 26, 36 Plug body 27, 32, 38 Concave part 37, 109 O-ring 46, 47, 51, 58, 62, 76, 92, 96, 102 Thread part 61 Second straight body Portions 75, 95, 110 Movable plug 79 Inner plug 80 First O-ring 81 Second O-ring 82 Holding cylinder 83 End cap 84 Column body 86, 107 Groove 88, 94, 105 Recess 89, 103 Cylindrical portion 90 Top plate 9 Opening 97 Nut 101 Fixing plug 104 Disc A Arrow indicating the direction in which the eluent is supplied during separation and purification D Clearance between filter 74 and flange 85 E1 Initial position of the other end of the packed bed E2 Straight body from E1 Position of the other end of the packed bed when shifted to the other end side of E3 E3 Position of the other end of the packed bed when shifted from E1 to one end side of the straight body part

Claims (15)

In a plastic medium pressure liquid chromatography column for packing particulate filler,
A column for medium pressure liquid chromatography, wherein the plastic is a fluororesin. A straight body made of fluororesin that forms a cylindrical chamber;
A distal end portion having a passage having a diameter smaller than that of the chamber, connected to one end of the straight body portion, and connecting one end of the chamber and the outside;
A pair of filters that have liquid permeability and are disposed at one end and the other end of a filling layer that is formed when the chamber is filled with a filler to prevent leakage of the filler. The medium-pressure liquid chromatography column according to claim 1, wherein   The tip has a tapered portion that is connected to one end of the chamber and gradually decreases from the diameter of the chamber, and a passage that connects to the tip of the tapered portion and communicates the tapered portion with the outside. The column for medium pressure liquid chromatography according to claim 2.   The column for medium pressure liquid chromatography according to claim 2 or 3, wherein a ratio of an axial length of the chamber to a diameter of the chamber is 2 or more.   The column for medium pressure liquid chromatography according to any one of claims 2 to 4, further comprising a plug for detachably closing the other end of the chamber.   The column for medium pressure liquid chromatography according to claim 5, further comprising a passage that communicates between the chamber and the outside when the plug closes the other end of the chamber with the plug.   The said stopper further has a recessed part which forms a hollow with respect to the said chamber when the other end of the said chamber is plugged with the said stopper, The said channel | path connects the recessed part and the exterior. Or the column for medium pressure liquid chromatography of 6.   The medium pressure according to any one of claims 5 to 7, further comprising a restricting portion that restricts movement of the filter arranged at the other end of the packed bed in the direction of the other end of the chamber. Column for liquid chromatography.   When the other end of the chamber is closed with the stopper, the restricting portion protrudes from the stopper into the chamber and is in contact with the filter disposed at the other end of the packed bed. The column for medium pressure liquid chromatography according to claim 8, wherein the column is a medium pressure liquid chromatography column.   The column for medium pressure liquid chromatography according to claim 8 or 9, wherein the stopper is a movable stopper capable of adjusting a position of closing the chamber in an axial direction of the straight body portion. A fluororesin-made straight body part forming a cylindrical chamber, and a tip having a passage having a diameter smaller than that of the chamber, connected to one end of the straight body part and connecting one end of the chamber to the outside A pair of filters that have liquid permeability and are disposed at one end and the other end of the filling layer that is formed when the chamber is filled with the filler, and for preventing leakage of the filler, Column for medium pressure liquid chromatography having a plug that detachably closes the other end of the chamber, and a restricting portion that restricts movement of the filter disposed at the other end of the packed bed in the direction of the other end of the chamber. And a prepacked column for medium pressure liquid chromatography packed with a particulate filler,
The filter is disposed at one end and the other end of a packed bed made of a filler contained in the chamber, and movement of the filter on the other end side in the other end direction of the chamber is restricted by the restriction portion. , Prepacked column.   The prepack column according to claim 11, wherein a particle size of the filler is 10 μm or more.   The prepacked column according to claim 11 or 12, wherein an organic solvent is further contained in the chamber.   The prepack column according to any one of claims 11 to 13, wherein the filler has a separating agent for optical isomers as a separating agent.   The prepack column according to any one of claims 11 to 14, further comprising a movable stopper capable of adjusting a position of closing the chamber in an axial direction of the straight body portion as the stopper and the restriction portion.

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