Series-connection curved surface chromatographic column

Abstract

The utility model belongs to the technical field of chromatographic analysis, and discloses a series-connection curved surface chromatographic column, which comprises a column tube, a plurality of cylindrical tubes and a plurality of spherical shells, the cylindrical tubes and the spherical shells are connected in series, the spherical shells are positioned between two adjacent cylindrical tubes and are communicated with the two adjacent cylindrical tubes, and the cylindrical tubes and the spherical shells are connected in series. The inlet end of the column pipe is connected with a front baffle plate, the outlet end of the column pipe is connected with a rear baffle plate, and the front baffle plate and the rear baffle plate are star-shaped splitter plates with centers; the spherical shell is filled with a solid ball, and an arc-shaped runner is formed between the solid ball and the inner wall of the spherical shell; the cylindrical pipe and the arc-shaped flow channel are filled with filler. The utility model aims to increase the effective column volume, weaken the dilution effect and increase the column loading capacity, so as to obtain good chromatographic separation efficiency and facilitate the preparation and separation analysis of trace substances.

Description

Technical Field

[0001] The utility model relates to the technical field of chromatographic analysis, in particular to a series of curved surface chromatographic columns. Background Art

[0002] Liquid chromatography is an effective method for separation and differentiation of substances in instrumental analysis, mainly used in sample preparation and analysis. It is widely used in the fields of food, medicine, cosmetics and environment. The chromatographic column as the core part is the key part of liquid chromatography. Other chromatographic components, such as injection, infusion pump, pipeline, detector, etc., need to be designed and changed around the chromatographic column.

[0003] In chromatography, there are two phases, one of which is fixed and we call it the stationary phase; the other phase flows through the stationary phase continuously and we call it the mobile phase. The separation principle of chromatography is to use the different affinity of the various substances to be separated in the two phases, such as the distribution coefficient and adsorption capacity. Use external force to make the mobile phase (gas, liquid) containing the sample pass through the surface of a stationary phase that is fixed in a column or on a plate and is immiscible with the mobile phase. When the mixture carried in the mobile phase flows through the stationary phase, the components in the mixture interact with the stationary phase. Due to the differences in properties and structures of the components in the mixture, the magnitude and strength of the forces generated between the mobile phase and the stationary phase are different. As the mobile phase moves, the mixture undergoes repeated distribution equilibrium between the two phases, so that the retention time of each component by the stationary phase is different, and thus it flows out of the stationary phase in a certain order. Combined with appropriate post-column detection methods, the separation and detection of the components in the mixture can be achieved.

[0004] Liquid chromatography has made great progress in equipment environment and equipment capabilities from normal pressure to high pressure, from preparation to efficient analysis, but the chromatographic column, as its core, is still in a state of equal diameter. Whether the inner diameter of the column is from meter-level to micron-level, the inner diameter of the entire column pipeline remains consistent, in the form of a flat column bed, using the flow medium to push the column bed in the plane. During the flow process, the flow phase containing the sample is injected through the center, and the column bed formed by the sieved sample will diffuse radially or laterally, causing the final chromatographic peak to broaden or tail. With the changes in pressure, shaped fillers, and particle size, related problems have been well solved.

[0005] However, the development of the corresponding chromatographic fluid and plate theory still continues with the original empirical formula. The basic parameters cannot be further developed with the optimization of some accessories and supporting facilities, and there will be a final development bottleneck. For example, changes in particle size and pressure will just lose the overall column loading capacity, and also bring difficulties to the separation and detection of trace substances. The natural substance dilution effect of the original equal-diameter column itself also puts forward enrichment requirements for the detection of trace substances, which is also a bottleneck problem of existing chromatography. Summary of the Invention

[0006] The utility model aims to provide a series-connected curved surface chromatographic column, aiming to increase the effective column volume, weaken the dilution effect, increase the column load, so as to obtain good chromatographic separation performance, which is more conducive to the preparation, separation and analysis of trace substances.

[0007] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0008] A series-connected curved surface chromatographic column includes a column tube, the column tube includes a plurality of cylindrical tubes and a plurality of spherical shells connected in series, the spherical shells are located between two adjacent cylindrical tubes, and the spherical shells communicate with the two adjacent cylindrical tubes. The inlet end of the column tube is connected with a front baffle, and the outlet end of the column tube is connected with a rear baffle. Both the front baffle and the rear baffle are star-shaped shunt plates with a center; solid balls are filled in the spherical shells, and an arc-shaped flow channel is formed between the solid balls and the inner wall of the spherical shells; packing is filled in the cylindrical tubes and the arc-shaped flow channels.

[0009] Further, the spherical shell is a spherical shell or an elliptical spherical shell, the solid ball is a sphere or an ellipse, and the solid ball is located at the center of the spherical shell.

[0010] Further, the vertical distance from the outer surface of the solid ball to the inner wall of the spherical shell is the same; and the volume of the arc-shaped flow channel is the same as the volume of the cylindrical tube with the same length replacing the arc-shaped flow channel.

[0011] Further, the material of the column tube is any one of stainless steel, glass or resin; the materials of the front baffle and the rear baffle are both stainless steel; the material of the solid ball is stainless steel or ceramic; and the column tube is integrally formed.

[0012] The beneficial effects of the technical solution are:

[0013] 1. The raw materials of the chromatographic column adopted by the utility model are rich, the cost is low, and it is friendly to the environment;

[0014] 2. Compared with the original equal-diameter column body, the utility model adds an arc-shaped flow channel part, and by adding inert solid balls, the effective empty volume is the same as that of the conventional equal-diameter column. When the fluid or sample bed flows through the arc-shaped flow channel, it will generate a split type. The relevant fluid or sample bed passes through a longer length than the conventional equal-diameter straight column bed due to flowing through the arc-shaped flow channel, and due to the flow pattern change of first dispersion and then convergence in the arc-shaped flow channel, the substances in the sample are separated on more separation plates, and at the same time, the dilution effect of the original equal-diameter straight column is weakened, the effective column volume is increased, the chromatographic separation performance is improved, and the overall column load is also increased, which is conducive to the preparation and analysis of trace substances.

[0015] 3. The physical properties of the chromatographic column of the present utility model improve the effective column volume of the sample. Through the alternation of dispersion and convergence of the flow pattern in the arc-shaped flow channel, the value of the theoretical column volume can be effectively increased, the number of theoretical plates per unit length can be effectively transformed and improved, and due to the change in the effective volume, the number of independent variables in the theoretical plate formula is increased, providing a new parameter for the optimization of chromatographic separation. Description of the Drawings

[0016] Figure 1 It is a schematic structural diagram of the series-connected curved surface chromatographic column of the present utility model;

[0017] The names of the corresponding marks in the drawings are:

[0018] Front baffle 1, column tube 2, cylindrical tube 3, solid ball 4, rear baffle 5, spherical shell 6, packing 7. Specific Embodiments

[0019] The following combines the attached Figure 1 drawings and embodiments to further elaborate on the present invention in detail:

[0020] The chromatographic column includes an analytical column, a semi-preparative column, and a preparative column. The analytical column is used for analysis, determination of content or impurities, and has a smaller diameter, usually less than 5 mm; the semi-preparative column is a chromatographic column between the analytical column and the preparative column, and its diameter is generally slightly larger than 5 mm. It can be used for analytical testing and also for a small amount of preparation; the preparative column is used for component separation and collecting components, and has a larger diameter compared to the semi-preparative column. The preparative column is more often used in purifying drugs. A series-connected curved surface chromatographic column of the present invention includes a series-connected curved surface analytical column, a series-connected curved surface preparative column, and a series-connected curved surface semi-preparative column. The experiment in Example 1 is a comparative experiment between the series-connected curved surface semi-preparative column of the present invention and a conventional equal-diameter semi-preparative column, and the experiments in Examples 2-4 are comparative experiments between the series-connected curved surface analytical column of the present invention and a conventional equal-diameter analytical column.

[0021] Example 1

[0022] A tandem curved surface chromatography semi-preparative column, comprising a column tube 2 integrally formed. The column tube 2 includes two identical cylindrical tubes 3 and three identical spherical shells 6 connected in series. The spherical shell 6 is a spherical shell, and the spherical shell 6 is located between two adjacent cylindrical tubes 3 and is in communication with the two adjacent cylindrical tubes 3. The column tube 2 is successively a cylindrical tube 3, a spherical shell 6, a cylindrical tube 3, a spherical shell 6, and a cylindrical tube 3 from left to right. A front baffle 1 is connected to the inlet end of the column tube 2, and a rear baffle 5 is connected to the outlet end of the column tube 2. Both the front baffle 1 and the rear baffle 5 are sieve plates of a stainless steel strip center star-shaped flow dividing plate; Each spherical shell 6 is filled with solid balls 4. An arc-shaped flow channel is formed between the solid balls 4 and the inner wall of the spherical shell 6. The solid balls 4 are also solid spherical balls. The solid balls 4 are located at the center of the spherical shell 6 to make the outer surface of the spherical shell 6 parallel to the inner surface of the spherical shell 6. The vertical distance from any point on the outer surface of the solid ball 4 to the inner wall of the spherical shell 6 is the same, so that the height of the arc-shaped flow channel is the same; And the volume of the arc-shaped flow channel is equal to the volume of the cylindrical tube 3 with the same axial length as the arc-shaped flow channel replaced. The diameter of the solid ball 4 is smaller than the inner diameter of the cylindrical tube 3; The cylindrical tube 3 and the arc-shaped flow channel are filled with a filler 7;

[0023] In this embodiment, the material of the column tube 2 is stainless steel. The length of the column tube 2 is 300 mm. The inner diameter of the cylindrical tube 3 is 20 mm. The two spherical shells 6 are respectively located at the 100 mm and 200 mm positions of the column tube 2. The inner radius of the spherical shell 6 is 14.8 mm. The radius of the solid ball 4 is 9.5 mm. The material of the solid ball 4 is stainless steel; The filler 7 is a C18 filler with a particle size of 30 μm.

[0024] The tandem curved surface chromatography semi-preparative column of this embodiment and a conventional equal-diameter semi-preparative column are respectively tested with lovastatin in red yeast rice as the semi-preparation target. A lovastatin solution with a concentration of 3 mg / L is prepared. The solvent is an aqueous solution of 70% ethanol. After separation by the chromatographic column, it is detected by an ultraviolet detector. Among them, the inner diameter of the conventional equal-diameter semi-preparative column is 20 mm, the column length is 300 mm, the material of the semi-preparative column is a stainless steel main body, and it is filled with a C18 filler with a particle size of 30 μm. The detection results are shown in Table 1 below. Column 1 is a conventional equal-diameter semi-preparative column, and Column 2 is the tandem curved surface chromatography semi-preparative column of this embodiment:

[0025] Table 1

[0026]

[0027]

[0028] The yield refers to the ratio of the lovastatin content obtained by preparative chromatography separation to the added amount. There is no significant difference in the yield between Column 1 and Column 2. In the case of approximate yields, the tandem curved surface chromatography analysis column of this embodiment has a better theoretical plate number, indicating a better separation effect.

[0029] Example 2

[0030] The difference between this embodiment and Embodiment 1 is as follows:

[0031] In this embodiment, the length of the column tube 2 is 250 mm, the inner diameter of the cylindrical tube 3 is 4.6 mm, the two spherical shells 6 are respectively located at 83 mm and 166 mm of the column tube 2, the inner radius of the spherical shell 6 is 3.4 mm, the radius of the solid sphere 4 is 2 mm; the packing 7 is C18 packing with a particle size of 5 μm, and the tandem curved surface chromatographic column of this embodiment is a tandem curved surface chromatographic analysis column.

[0032] The tandem curved surface chromatographic analysis column of this embodiment and a conventional equal-diameter analysis column were respectively tested with lovastatin in red yeast rice as the analysis target. A lovastatin solution with a concentration of 3 mg / L was prepared, and the solvent was an aqueous solution of 70% ethanol. After separation by the chromatographic column, it was detected with an ultraviolet detector. Among them, the inner diameter of the conventional equal-diameter analysis column is 4.6 mm, the column length is 250 mm, the material of the analysis column is a stainless steel main body, and it is filled with C18 packing with a particle size of 5 μm.

[0033] The detection results are shown in Table 2 below. Column 1 is a conventional equal-diameter analysis column, and Column 2 is the tandem curved surface chromatographic analysis column of this embodiment:

[0034] Table 2

[0035]

[0036]

[0037] The test results show that the tandem curved surface chromatographic analysis column of this embodiment has a higher theoretical plate number than the conventional equal-diameter analysis column, indicating that the effective column volume of the chromatography of the tandem curved surface chromatographic analysis column of the embodiment has been improved. At the same time, the tailing factor of the tandem curved surface chromatographic analysis column of this embodiment is smaller than that of the conventional equal-diameter analysis column, further indicating that the tandem curved surface column has a smaller column broadening, indicating that there is a higher effective concentration of the substance to be detected in the unit void volume, and the effective sample loading amount can also be improved.

[0038] Embodiment 3

[0039] The difference between this embodiment and Embodiment 2 is as follows:

[0040] In this embodiment, the inner radius of the spherical shell 6 is 7 mm.

[0041] The tandem curved surface chromatographic column of this embodiment and a conventional equal-diameter analytical column were respectively tested with aflatoxin B1 in oats as the analysis target. A solution of aflatoxin B1 with a concentration of 0.5 mg / L was prepared, and the solvent was an aqueous solution of 70% ethanol. After separation by the chromatographic column, it was detected with a fluorescence detector. Among them, the inner diameter, column length, material, and packing 7 of the conventional equal-diameter analytical column were the same as those of the conventional equal-diameter analytical column in Example 2. The test results are shown in the following table. Column 1 is the conventional equal-diameter analytical column, and column 2 is the tandem curved surface chromatographic column of this embodiment:

[0042] Table 3

[0043]

[0044]

[0045] The test results show that when the inner diameter of the spherical shell 6 is enlarged, the separation effect cannot be effectively obtained. When the inner diameter of the spherical shell 6 is enlarged to nearly twice the inner radius of the spherical shell 6 in Example 2, a separation efficiency similar to that of a conventional analytical column can be obtained.

[0046] Example 4

[0047] The difference between this embodiment and Example 2 is:

[0048] In this embodiment, the inner radius of the spherical shell 6 is 3 mm.

[0049] The tandem curved surface chromatographic column of this embodiment and a conventional equal-diameter analytical column were respectively tested with aflatoxin B1 in oats as the analysis target. A solution of aflatoxin B1 with a concentration of 0.5 mg / L was prepared, and the solvent was an aqueous solution of 70% ethanol. After separation by the chromatographic column, it was detected with a fluorescence detector. Among them, the inner diameter, column length, material, and packing 7 of the conventional equal-diameter analytical column were the same as those of the conventional equal-diameter analytical column in Example 2. The test results are shown in the following table. Column 1 is the conventional equal-diameter analytical column, and column 2 is the tandem curved surface chromatographic column of this embodiment:

[0050] Table 4

[0051]

[0052]

[0053] The experimental results show that when the inner diameter of the spherical shell 6 is reduced, the chromatographic separation ability cannot be greatly improved. The reason is the reduction of the effective column volume, which also indicates that the inner diameter design of the spherical shell 6 of the tandem curved surface chromatographic column should have a certain control range. It further shows that when the volume of the arc-shaped flow channel is equal to that of a cylindrical tube with the same axial length as the arc-shaped flow channel, the chromatographic separation efficiency can be greatly improved.

[0054] The above are only the embodiments of the present utility model, and common general technical solutions or characteristics in the solutions are not described in detail herein. It should be noted that for those skilled in the art, without departing from the technical solution of the present utility model, several deformations and improvements can be made, and these should also be regarded as the protection scope of the present utility model, and these will not affect the implementation effect of the present utility model and the practicality of the patent. The protection scope required by this application shall be subject to the content of its claims, and the specific implementation manners and the like recorded in the specification can be used to interpret the content of the claims.

Claims

1. A tandem curved surface chromatographic column, characterized in that, It includes a column tube (2), and the column tube (2) includes a plurality of cylindrical tubes (3) and a plurality of spherical shells (6) connected in series. The spherical shells (6) are located between two adjacent cylindrical tubes (3), and the spherical shells (6) communicate with the two adjacent cylindrical tubes (3). A front baffle (1) is connected to the inlet end of the column tube (2), and a rear baffle (5) is connected to the outlet end of the column tube (2). Both the front baffle (1) and the rear baffle (5) are star-shaped shunt plates with a center; solid balls (4) are filled in the spherical shells (6), and an arc-shaped flow channel is formed between the solid balls (4) and the inner wall of the spherical shells (6); packing (7) is filled in the cylindrical tubes (3) and the arc-shaped flow channels.

2. The series-connected curved surface chromatographic column according to claim 1, wherein: The spherical shell (6) is a spherical shell or an elliptical spherical shell, the solid ball (4) is a sphere or an ellipsoid, and the solid ball (4) is located at the center of the spherical shell (6).

3. The tandem curved surface chromatographic column according to claim 1, wherein: The vertical distance from the outer surface of the solid ball (4) to the inner wall of the spherical shell (6) is the same; and the volume of the arc-shaped flow channel is the same as the volume of a cylindrical tube (3) with the same length replacing the arc-shaped flow channel.

4. The tandem curved surface chromatographic column according to claim 1, characterized in that: The material of the column tube (2) is any one of stainless steel, glass or resin; the materials of the front baffle (1) and the rear baffle (5) are both stainless steel; the material of the solid ball (4) is stainless steel or ceramic; and the column tube (2) is integrally formed.

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