CN211528300U - Purification column and liquid chromatography device - Google Patents

Abstract

The utility model provides a purifying column and liquid chromatography device relates to the technical field that liquid chromatography detected. The purifying column comprises a column tube, the column tube is of a hollow columnar structure with two open ends, and the two open ends of the column tube are both communicated with filtering pieces; each filtering piece is communicated with a locking piece at one side far away from the column tube, and at least one mixer is communicated between the filtering piece and the locking piece at one end or two ends of the column tube. The mixer connected in the purification column can increase the contact of the mobile phase and the adsorption medium in the column tube, so that the effect of removing impurities in the mobile phase is better, the inhomogeneous mobile phase can be further mixed and converged, the uniform mixing effect of the mobile phase is realized, and the base line in the chromatogram is more stable.

Description

Purification column and liquid chromatography device

Technical Field

The utility model relates to a technical field that liquid chromatogram detected, concretely relates to purifying column and liquid chromatogram analytical equipment.

Background

Liquid chromatography is used frequently in the fields of biology, medicine, pharmacy, food science, etc., and is mainly used for separating, analyzing and isolating samples. It is easy to generate the famous and wonderful chromatographic peaks, which we call the famous peaks, during the liquid chromatographic separation process, especially during the gradient elution process, and these famous peaks are generated at the end of the gradient. The source of the Mohs peaks is various, theoretically, the Mohs peaks can be introduced into any node in the liquid chromatography system, and the Mohs peaks mainly come from the problems of solvents, instruments, residual bubbles of mobile phases, improper operation and the like according to the frequency of the Mohs peaks.

The cause of the Mohs' peak due to the solvent problem mainly includes impurities in the mobile phase, aqueous phase and other reagents (buffer salts, TFA, EDTA, etc.). The mobile phase is used as the basis of liquid chromatography and preparative chromatography separation, organic pollutants in the mobile phase cannot be well removed through a traditional mobile phase filtration mode, and new pollutants can be introduced, such as a traditional suction flask and a membrane filtration mode. Therefore, it is required to develop a new technology capable of efficiently removing impurities in a mobile phase and effectively removing a Mohs peak without introducing new contaminants.

SUMMERY OF THE UTILITY MODEL

In view of this, the utility model aims at providing a purification column, the blender of intercommunication can increase the contact of mobile phase and column tube internal adsorption medium in the purification column, reaches the better effect of removing impurity in the mobile phase, can make inhomogeneous mobile phase further mix, collects, realizes the effect that the mobile phase mixes the homogeneity, and the base line is more steady in letting the chromatogram.

The utility model provides a purifying column in a first aspect, which comprises a column tube, wherein the column tube is a hollow columnar structure with two open ends, and the two open ends of the column tube are both communicated with filtering pieces; each filtering piece is communicated with a locking piece at one side far away from the column tube, and at least one mixer is communicated between the filtering piece and the locking piece at one end or two ends of the column tube.

When adopting above-mentioned purification column to handle mobile phase, pack adsorption medium earlier in the pillar pipe, mobile phase flows in from the one end of ion purification column, flows through the retaining member in proper order, the blender, filter and reach the pillar intraduct, the inside adsorption medium of pillar pipe can adsorb the impurity in the mobile phase this moment, mobile phase flows out from the other end of pillar pipe after adsorption medium's purification in the pillar pipe, flows through filter, blender and retaining member in proper order, accomplishes mobile phase's purification process.

The fact that at least one mixer is communicated between the filtering element and the locking element at one end or two ends of the column tube means that: (1) the inlet end (the end where the mobile phase flows in) of the column tube in the purification column is communicated with one or more mixers; (2) the inlet end (the end where the mobile phase flows in) and the outlet end (the end where the mobile phase flows out) of the column tube in the purification column are communicated with one or more mixers.

The mobile phase treated by the purifying column can efficiently remove impurities in the mobile phase, hardly influences the shape and retention time of a chromatographic peak, has very obvious effect of removing the Mohs peak, ensures that some methods which have to be changed and abandoned due to the problems of the Mohs peak can be smoothly applied, and does not need to invest much time and energy by research and development personnel to treat the Mohs peak.

Further, on the technical scheme provided by the utility model's basis, the blender is both ends open-ended cavity columnar structure, and hollow portion's cross-sectional area reduces from both ends opening part to inside step by step.

The position where the cross-sectional area of the hollow portion is the smallest is not particularly limited, and the specific position may be, but is not limited to: the middle, one third, one fourth or one fifth of the mixer.

The cross-sectional area of the hollow portion of the mixer gradually decreases from the openings at both ends to the inside. Therefore, after the pipeline of the liquid chromatogram is communicated with the purifying column, one end of the mixer at the inlet end of the purifying column, which is close to the locking piece, can play a role in sealing, the contact area between the mobile phase and the filtering piece can be effectively enlarged at one end close to the column tube, the contact between the mobile phase and the adsorption medium in the column tube is increased, and the effect of better removing impurities in the mobile phase is achieved.

The mobile phase passes through the purification column, and after the adsorption medium adsorbs impurities in the mobile phase, the components of the mobile phase are relatively uneven, so that a base line in the chromatogram can drift, the end of the mixer at the outlet end of the purification column, which is close to the locking piece, can play a role in sealing, and the end of the mixer, which is close to the column tube, can further mix and collect uneven mobile phases, so that the effect of uniform mixing of the mobile phases is realized, and the base line in the chromatogram is more stable.

Further, on the technical scheme provided by the utility model's basis, the cavity columnar structure of blender includes any one in cylinder structure, triangle post structure, four corners post structure or the pentagon post structure.

The hollow columnar structure of the mixer is further limited and optimized, and the regular structures such as a conventional cylindrical structure, a triangular column structure, a quadrangular column structure or a pentagonal column structure can be selected, so that the processing difficulty of the mixer can be reduced, and the manufacturing cost can be reduced; and can select the structure that suits with the hollow column structure of column jacket, the cooperation installation of being convenient for makes the mobile phase more smooth and easy when flowing from it, makes the use of purifying column more convenient.

Further, the utility model provides a on the basis of the technical scheme, the blender is both ends open-ended hollow circular cylinder structure, and hollow portion's cross-sectional area reduces gradually from both ends opening part to middle part and forms the taper shape, and the space that two taper shapes meet the department is cylindricly.

The appearance of the preferred blender is a cylindrical structure, the hollow interior contains the structure of two cones, make the internal diameter of the blender taper inclined plane, can make the resistance when the mobile phase passes the conical space smaller, and two cones form a narrow channel of the cylindrical space in the middle part of the blender, can make the mobile phase mix more evenly before entering the column tube and after flowing out of the column tube and then flow out as the scattering shape fast again, can make the mobile phase contact with absorption medium in the column tube more fully after entering the column tube, achieve the better effect of removing the impurity in the mobile phase; and after the flow out of the column tube, the uneven mobile phase is further mixed, so that the effect of uniform mixing of the mobile phase is realized, and the base line in the chromatogram is more stable.

Further, the length of the mixer is 7.0-10mm, the length of the space at the joint is 0.8-1.2mm, and the inner diameter is 0.4-0.8 mm.

The length of the mixer may be, but is not limited to, 7.0mm, 7.5mm, 8.0mm, 8.5mm, 9.0mm, 9.5mm, or 10 mm.

The length of the cylindrical space where the two cones meet may be, but is not limited to, 0.8mm, 0.9mm, 1.0mm, 1.1mm, 1.2 mm; the inner diameter may be, but is not limited to, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8 mm.

The length of the mixer is preferably limited, so that the influence of the overlong length on normal use is avoided, and the influence of the overlong length on the converging and sealing effects of the mixer is avoided; the space size of the joint of the two cones is limited, the influence of overlong length and undersize inner diameter on the flowing speed of the mobile phase in the mixer can be avoided, the influence of overlong length and oversize inner diameter on the collection and sealing effect of the mixer can be avoided, and the using effect of the mixer and the purifying effect of the purifying column can be further improved.

Further, the utility model provides a on the basis of the technical scheme, the hollow column structure of pillar pipe includes any one of cylinder structure, triangle post structure, four corners post structure or pentagon post structure.

The hollow columnar structure of the column tube is further limited and optimized, and the regular structures such as a conventional cylindrical structure, a triangular column structure, a quadrangular column structure or a pentagonal column structure can be selected, so that the difficulty of mixing the column tube can be reduced, and the manufacturing cost can be reduced; and the cooperation installation of being convenient for makes the mobile phase more smooth and easy when flowing from it, makes the use of purifying column more convenient.

In a preferred embodiment of the present invention, the hollow cylindrical structure of the column tube is a cylindrical structure.

The shape of the preferable column tube is a cylindrical structure, the hollow interior of the preferable column tube is also a cylindrical structure, and compared with a triangular column structure, a four-corner column structure, a five-corner column structure or other structures, the cylindrical structure is more convenient to manufacture, is suitable for the cylindrical shape structure of a liquid chromatogram pipeline, and is convenient to install and apply; the hollow interior is cylindrical, the internal space is large, more adsorption media can be filled, and the contact area of the mobile phase and the adsorption media is increased; but also can reduce the friction between the inner wall of the column tube and the fluidity, so that the mobile phase can pass through more quickly and smoothly.

Furthermore, on the basis of the technical proposal provided by the utility model, the length of the column tube is 10-35mm, and the roughness of the inner wall is less than or equal to 5.0 μm; preferably, the column tube is a hollow cylindrical structure having an inner diameter of 1.5 to 7.6 mm.

The length of the vial may be, but is not limited to, 10mm, 12mm, 15mm, 18mm, 20mm, 22mm, 25mm, 28mm, 30mm, or 35 mm.

The column tube is a hollow cylindrical structure with an inner diameter of 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm, 4.5mm, 5mm, 5.5mm, 6mm, 6.5mm, 7mm, 7.5mm or 7.6 mm.

The length range and the inner diameter range of the column tube are optimized, so that the column tube has proper volume, more adsorption media can be filled to adsorb hydrophobic impurities, the retention time of a mobile phase in the column tube is delayed to be less than 1min, the column effect is not changed greatly, and the influence on the accuracy of a liquid chromatogram result is reduced.

The roughness of the inner wall is preferably less than or equal to 5.0 mu m, so that the friction force between the inner wall of the column tube and the fluidity can be reduced, the mobile phase can more quickly and smoothly pass through the column tube, the retention time of the mobile phase in the column tube is reduced, and the column effect change is reduced.

Further, the utility model provides a on the basis of technical scheme, filter the piece and be the sieve.

The sieve plates at two ends of the column tube can replace an on-line filter, so that solid particulate matters are effectively prevented from reaching the chromatographic column, and the column pressure rise caused by the blockage of the solid particulate matters is avoided. The aperture of the optimized sieve plate is smaller than that of the adsorption medium filled in the column tube, so that the adsorption medium can be prevented from scattering outwards when the adsorption medium is filled in the column tube, the contact area between the mobile phase and the sieve plate can be effectively enlarged, the resistance of the mobile phase when the mobile phase passes through is reduced, and the mobile phase can smoothly flow through.

Further, the utility model provides a on the basis of technical scheme, the retaining member is the nut, and the nut is for holding the hollow column structure who filters piece and blender, and the nut is close to the one end and the pillar can be dismantled with the pillar and be connected of pillar.

Ways of detachable connection include, but are not limited to: threaded connection, snap-fit connection, and hinged connection.

Adopt the nut to be the retaining member, and the nut is hollow columnar structure, will filter including piece and the blender parcel and become an organic whole with the pillar pipe, increase the leakproofness of whole purification post, avoid appearing the problem of weeping when purification treatment mobile phase. In addition, the nut is detachably connected with the two ends of the column tube, so that each part can be conveniently installed, and the adsorption medium can be conveniently filled in the column tube; and the cleaning nut, the mixer, the filter element and each part of the column tube can be separately cleaned when the purifying column is required to be cleaned, the cleaning effect is better, and the service life of the purifying column is prolonged.

In a preferred embodiment of the present invention, the column tube is a hollow cylindrical structure, the outer portions of the two ends are provided with external annular threads, the inner portion of the nut is provided with internal annular threads for cooperation, and the nut is connected with the two ends of the column tube by threads.

The preferred pillar pipe is the hollow circular cylinder structure, is provided with the screw thread on the circular outer wall at its length direction's both ends, is provided with the annular thread that the cooperation was used in the hollow structure inside of nut, and the pillar pipe adopts threaded connection's mode with being connected of nut, and threaded connection can improve the leakproofness of whole purification post, makes things convenient for equipment and dismantlement moreover, improves the holistic connection steadiness of purification post.

In a preferred embodiment of the present invention, a typical purification column assembly process comprises: (1) placing the mixer and the sieve plate in the cavity of the nut in sequence; (2) connecting a nut with the inlet end of the column tube in a threaded connection mode, and screwing; (3) filling a proper amount of adsorption medium in the column tube; (4) connecting the other nut with the outlet end of the column tube in a threaded connection mode, and screwing; and (5) finishing the assembly.

The utility model discloses the second aspect provides a liquid chromatography device, contains the purifying column.

The utility model adopts the above technical scheme following beneficial effect has:

1. the utility model provides a purifying column, the mixer of purifying column entry end can effectively enlarge the area of contact of mobile phase and filter piece, increases the contact of mobile phase and the adsorption medium in the column tube, reaches the better effect of removing the impurity in the mobile phase; the mixer at the outlet end can further mix and collect the uneven mobile phase, so that the effect of uniform mixing of the mobile phase is realized, and the base line in the chromatogram is more stable.

2. The utility model provides a purifying column, wherein the sieve at column tube both ends can replace on-line filter, prevents effectively that solid particle from reaching the chromatographic column, avoids rising because of the column pressure that solid particle blockked up and arouses, can also prevent that adsorption medium from scattering from the column tube.

Drawings

FIG. 1 is a schematic diagram of an exploded structure of a purification column;

FIG. 2 is an enlarged partial schematic view of FIG. 1 at A;

FIG. 3 is a schematic view showing the structure of a mixer in a purification column;

fig. 4 is a schematic structural view of the purification column.

Reference numerals: 1. a column tube; 2. a filter member; 21 sieve plate; 3. a locking member; 31. a nut; 4. a mixer.

Detailed Description

Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

Examples

A purification column, as shown in fig. 1 and 4, comprises a column tube 1, wherein the column tube 1 is a hollow cylindrical structure with two open ends; the both ends opening part of 1 length direction of pillar pipe all communicates and has filtered piece 2, and every one side intercommunication of filtering piece 2 and keeping away from pillar pipe 1 has a blender 4, and one side intercommunication that filters piece 2 is kept away from to blender 4 has a retaining member 3.

The column tube 1 is a hollow cylindrical structure with openings at two ends, the inner space is cylindrical, the length is 30mm, the inner diameter is 4.6mm, and the outer diameter is 7.0 mm. Annular external threads are arranged outside two ends in the length direction. The column tube 1 is filled with polystyrene anion exchange medium, the polystyrene anion exchange is spherical, the particle size of the polystyrene anion exchange is 300 μm, and the pore diameter is 300 nm. The column tube 1 is made of 316 stainless steel, and the roughness of the inner wall is less than or equal to 5.0 mu m.

As shown in figure 2, the openings at the two ends of the column tube 1 in the length direction are both communicated with a filtering piece 2, and the filtering piece 2 is a sieve plate 21. The sieve plate 21 is a disc-shaped structure with an aperture, the thickness of the sieve plate is 1mm, and the axial direction of the sieve plate coincides with the axial direction of the column tube 1. The circular middle part of the sieve plate 21 is provided with filter holes with the aperture of 2um-100 um. The circular edge is of a solid structure. The diameter of the sieve plate 21 is the same as the outer diameter of the column tube, and the thickness of the edge is the same as the wall thickness of the column tube 1.

As shown in fig. 3, one side of the sieve plate 21, which is far away from the column tube 1, is communicated with a mixer 4, the mixer 4 is a hollow cylindrical structure with openings at two ends, the internal space is cylindrical, the length is 8.0mm, the cross-sectional area of the hollow part gradually decreases from the openings at two ends to the middle part to form a cone, the space where the two cones are connected is cylindrical, the cylindrical length of the middle part is 1.0mm, and the inner diameter is 0.5 mm. The axial direction of the mixer 4 coincides with the axial direction of the column tube 1, and the outer diameter and the inner diameter of both ends are the same as the inner diameter and the outer diameter of the column tube 1.

One side of each mixer 4, which is far away from the column tube 1, is communicated with a locking piece 3, and the locking piece 3 is a nut 31. The nut 31 is of a hollow cylindrical configuration, and the inner wall of the end adjacent to the mixer 4 is provided with an internal thread which cooperates with the annular external thread of the column tube 1. The inner diameter of the end of the nut 31 near the mixer 4 is adapted to the outer diameter dimensions of the mixer 4 and the screening deck 21 so that the mixer 4 and the screening deck 21 can be received in the nut 31. The outer wall of the end of the nut 31 remote from the mixer 4 is hexagonal, and is internally provided with an annular internal thread which can be connected with a pipeline of a high performance liquid chromatograph.

The application process of this embodiment is as follows:

after filling the adsorption medium in the column tube 1 of purifying column, the intercommunication is between liquid chromatogram's blender and injector, and the one end that is close to the blender is the entry end of purifying column, and the one end that is close to the injector is the exit end of purifying column.

The mobile phase flows into the purifying column from the inlet end, sequentially flows through the nut 31, the mixer 4 and the sieve plate 21 to reach the inside of the column tube 1, and sequentially flows through the sieve plate 21, the mixer 4 and the nut 31 after being adsorbed by the adsorption medium in the column tube 1, and flows out of the purifying column from the outlet end, so that the purifying process of the mobile phase is completed.

The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalents and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. The purifying column is characterized by comprising a column tube (1), wherein the column tube (1) is of a hollow columnar structure with two open ends, and the two open ends of the column tube (1) are both communicated with filtering pieces (2); one side of each filtering piece (2) far away from the column tube (1) is communicated with a locking piece (3), and at least one mixer (4) is communicated between the filtering piece (2) and the locking piece (3) at one end or two ends of the column tube (1).

2. Purification column according to claim 1, wherein the mixer (4) is a hollow cylindrical structure open at both ends, the cross-sectional area of the hollow part decreasing from the opening at both ends to the inside.

3. Purification column according to claim 2, wherein the hollow cylindrical structure of the mixer (4) comprises any one of a cylindrical structure, a triangular cylindrical structure, a quadrangular cylindrical structure or a pentagonal cylindrical structure.

4. A purification column according to claim 2 or 3, wherein the mixer (4) is a hollow cylindrical structure with two open ends, the cross-sectional area of the hollow part gradually decreases from the two open ends to the middle part to form a cone, and the space where the two cones meet is cylindrical.

5. Purification column according to claim 4, characterized in that the length of the mixer (4) is 7.0-10mm, the length of the space where the connection is made is 0.8-1.2mm and the inner diameter is 0.4-0.8 mm.

6. Purification column according to claim 1, wherein the hollow cylindrical structure of the column tube (1) comprises any one of a cylindrical structure, a triangular cylindrical structure, a quadrangular cylindrical structure or a pentagonal cylindrical structure.

7. The purification column according to claim 6, wherein the length of the column tube (1) is 10-35mm, and the roughness of the inner wall is less than or equal to 5.0 μm; the inner diameter of the column tube (1) which is a hollow cylindrical structure is 1.5-7.6 mm.

8. Purification column according to claim 1, characterized in that the filter element (2) is a sieve plate (21).

9. Purification column according to claim 1, wherein the locking element (3) is a nut (31), the nut (31) being a hollow cylindrical structure capable of accommodating the filter element (2) and the mixer (4), the end of the nut (31) close to the column tube (1) being detachably connected to the column tube (1).

10. A liquid chromatography apparatus comprising the purification column of any one of claims 1 to 9.

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