Novel column chromatography device for separating traditional Chinese medicine components

Abstract

The utility model discloses a novel column chromatography device for separating traditional Chinese medicine components, and belongs to the field of traditional Chinese medicine component separation devices. The novel column chromatography device comprises a chromatography column body, a top cover, a bottom cover and a screen mesh assembly, the screen mesh assembly is arranged in the chromatography column body and composed of a single-layer screen mesh, a partition plate and a sealing ring, the screen mesh in the screen mesh assembly is round and is made of metal materials or non-metal materials, the partition plate in the screen mesh assembly is provided with holes and is made of stainless steel, and the sealing ring is arranged in the top cover. And a sealing ring is arranged on the periphery. The novel column chromatography device for separating the traditional Chinese medicine components is suitable for industrial production of pilot-scale tests and above levels, not only can greatly improve the utilization rate and the service life of the filler, prevent fine filler or material precipitates from blocking meshes and improve the production efficiency, but also is easy to install and replace the screen assembly, and is convenient to popularize and use. And the use cost is greatly saved.

Description

Technical Field

[0001] The utility model belongs to the technical field of separation of traditional Chinese medicine components and relates to a column chromatography device used for separation of traditional Chinese medicine components. Background Art

[0002] Chromatography columns are the backbone of column chromatography technology. Small-scale tests are generally made of glass, while pilot-scale and above column chromatography production is generally made of polypropylene or galvanized stainless steel. Depending on the sample and purification requirements, different fillers are used, including resins, silica gel, polyamide, gel, etc. Existing column chromatography devices use disc-type, nut-type, or sand-core-type sieve plates to retain fillers. To prevent smaller particle size fillers from leaking out, these disc-type, nut-type, or sand-core-type sieve plates are generally formed by pressing together multiple layers. Their pores are small and difficult to replace. They are generally used until the pores become blocked, causing the flow rate to slow sufficiently, and then discarded. Because the filler particle size can be uneven and the swelling coefficients in different solvents vary, leaking into the pores of the sieve plate can clog the sieve plate. Furthermore, during the elution process of the sample (especially traditional Chinese medicine extracts), due to changes in the solubility of the sample or impurities in the elution solvent, some flocs often precipitate, thereby clogging the sieve plate and extending the production cycle.

[0003] If such a problem is encountered in industrial production, it will lead to an increase in the amount of dead adsorption in the entire batch of materials, a decrease in yield, and even the waste of materials and fillers. Solving the problem of sieve plate blockage in the column chromatography process of traditional Chinese medicine extracts has always been the focus of research in this field. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a novel chromatography column device for separating components of traditional Chinese medicine. The novel column chromatography device for separating components of traditional Chinese medicine provided by the present invention not only significantly improves the utilization rate of expensive raw materials and avoids pore blockage caused by swelling of fillers in different solvents and precipitation of traditional Chinese medicine extracts during elution, but also features an easy-to-install and replaceable screen assembly, significantly reducing operating costs.

[0005] A novel column chromatography device for separating components of traditional Chinese medicine, the novel column chromatography device mainly comprising a chromatography column (1), a top cover (2), a bottom cover (3), and a screen assembly (4);

[0006] The top cover (2) and the bottom cover (3) are fixed to the column (1) by screws. The top cover (2) is provided with a water inlet (10) and a pressure port (12), and is provided with a water inlet switch (11) and a pressure port switch (13). The column has a filler inlet (8) at the upper end and a filler outlet (7) at the lower end. The column is provided with a sight glass (9). The bottom cover (3) is provided with a water outlet (5) and is provided with a water outlet switch (6).

[0007] The screen assembly (4) is located between the bottom cover (3) and the column (1), and the screen assembly (4) is composed of a screen (a), a perforated partition (b), and a sealing ring (c). The stacking order from bottom to top is the screen (a), the perforated partition (b), and the sealing ring (c);

[0008] The area from the screen assembly (4) to the lower edge of the filler inlet (8) is a filler filling area.

[0009] Furthermore, the traditional Chinese medicine ingredient is a traditional Chinese medicine extract.

[0010] Preferably, the screen in the screen assembly is a single layer with an aperture size of 50-300 mesh.

[0011] Preferably, the screen in the screen assembly is circular, and its diameter is consistent with the outer diameter of the column.

[0012] Preferably, the screen material in the screen assembly is metal or non-metal.

[0013] Further preferably, the metal material is stainless steel, copper, brass, aluminum and alloys thereof.

[0014] More preferably, the metal material is stainless steel.

[0015] Further preferably, the non-metallic material is nylon, polypropylene PP, polyethylene PE, or polyester fiber PET.

[0016] Preferably, the perforated partition in the screen assembly has a pore size of 5-10 mm and a thickness of 0.2-0.5 cm.

[0017] Preferably, the partition with holes in the screen assembly is circular in shape, and its diameter is consistent with that of the screen.

[0018] Preferably, the perforated partition in the screen assembly is made of metal.

[0019] More preferably, the metal material is stainless steel.

[0020] Preferably, the sealing ring is made of silicone or rubber.

[0021] Compared with the prior art, the present invention has the following beneficial results:

[0022] 1. The utility model provides a novel column chromatography device for separating components of traditional Chinese medicine. The mesh size of the screen assembly can be replaced according to the different fillers, and can meet the needs of almost all fillers.

[0023] 2. No need to treat the resin before column loading, and unqualified small particle fillers can be discarded through the sieve below.

[0024] 3. After loading the sample, it can solve the problem of impurities precipitating and clogging the sieve plate during the elution of traditional Chinese medicine components. It is especially suitable for column chromatography production at the pilot level and above.

[0025] 4. The screen assembly is extremely low in cost and easy to clean. It can be reused for a long time, saving production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 A schematic diagram of a novel column chromatography device for separating components of traditional Chinese medicine according to the present invention.

[0027] Legend: 1 column, 2 top cover, 3 bottom cover, 4 screen assembly, 5 water outlet, 6 water outlet switch, 7 filler outlet, 8 filler inlet, 9 sight glass, 10 water inlet, 11 water inlet switch, 12 pressure port, 13 pressure port switch.

[0028] Figure 2 Schematic diagram of the screen assembly in the device.

[0029] Legend: a. Screen in the screen assembly, b. Partition in the screen assembly, c. Sealing ring in the screen assembly. DETAILED DESCRIPTION

[0030] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the schematic diagrams in the accompanying drawings of the present invention. Although the present embodiment is shown in the drawings, it should be understood that the present disclosure can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, the purpose of providing this embodiment is to enable a more thorough understanding of the present disclosure and to fully convey the scope of the present disclosure to those skilled in the art.

[0031] like Figure 1 As shown, the column chromatography device for separating components of traditional Chinese medicine of the present invention mainly comprises a chromatography column (1), a top cover (2), a bottom cover (3), and a screen assembly (4). The top cover (2) and the bottom cover (3) are fixed to the column (1) by screws. The top cover (2) is provided with a water inlet (10) and a pressure port (12), and a water inlet switch (11) and a pressure port switch (13) are provided respectively. The column has a filler inlet (8) at the upper end and a filler outlet (11) at the lower end. 7), the column is provided with a sight glass (9), the bottom cover (3) is provided with a water outlet (5), and a water outlet switch (6), the screen assembly (4) is located between the bottom cover and the column, and is characterized in that the screen assembly (4) consists of a screen (a), a perforated partition (b) and a sealing ring (c), and the stacking order from bottom to top is the screen (a), the perforated partition (b), and the sealing ring (c), and the lower edge of the screen assembly (4) to the filler inlet (8) is the filler filling area.

[0032] The column body of the column chromatography device for separating components of traditional Chinese medicine of the utility model is made of galvanized stainless steel or polypropylene resin. The inner diameter of the chromatography column is n, and the diameter of the connection between the top cover and the base and the column body is m. A screen assembly (4) is provided inside the column body. The screen (a) in the screen assembly is circular, has an aperture of 50-300 meshes, and the screen diameter d should satisfy n<d<m. The material is metal (stainless steel, copper, brass, aluminum and alloy) or non-metallic material (nylon, polypropylene PP, polyethylene PE, polyester fiber PET), preferably stainless steel. The perforated partition (b) on the screen assembly is metal, preferably stainless steel, has a diameter consistent with the screen, and a thickness of 0.2-0.5 cm. The sealing ring (c) in the screen assembly is fitted with the partition and can be made of silicone or rubber and is replaceable.

[0033] Before separating the components of traditional Chinese medicine, place the screen assembly (4) on the bottom cover (3), and connect the bottom cover (3) to the column (1) with screws. After the leak detection is completed, the column is directly loaded without pre-treating the filler. After the column is loaded, soak it in solvent for 5-10 hours. After that, open the bottom valve (6), release the solvent, and replace it with the corresponding eluent. At the same time, discard the small particle filler through the screen assembly. The loading and elution process is consistent with the conventional column chromatography operation. If impurities are precipitated, they can pass through the lower screen smoothly. After use, the regenerable filler can be regenerated according to conventional operations. If other fillers need to be replaced, a screen with a suitable pore size can be selected according to the filler particle size for replacement. For the same chromatography column, the partition and the sealing ring do not need to be replaced.

[0034] Example 1 Novel column chromatography device structure

[0035] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0036] The cylinder is made of stainless steel. The screen is circular, with a diameter consistent with the outer diameter of the cylinder. It is a single-layer stainless steel screen with a pore size of 50 mesh. The perforated partition in the screen assembly is circular, with a diameter consistent with the screen, a pore size of 10 mm, and a thickness of 0.2 cm. It is made of stainless steel. The sealing ring is made of silicone.

[0037] Example 2 Novel column chromatography device structure

[0038] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0039] The cylinder is made of polypropylene resin. The screen is circular, with a diameter consistent with the outer diameter of the cylinder. It is a single-layer nylon screen with a pore size of 200 mesh. The perforated separator in the screen assembly is circular, with a diameter consistent with the screen, a pore size of 7 mm, and a thickness of 0.3 cm. It is made of stainless steel. The sealing ring is made of silicone.

[0040] Example 3 Novel column chromatography device structure

[0041] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0042] The cylinder is made of polypropylene resin. The screen is circular, with a diameter consistent with the outer diameter of the cylinder. It is a single-layer, 100-mesh sieve made of aluminum. The perforated separator in the screen assembly is circular, with a diameter consistent with the sieve, a 5mm pore size, and a thickness of 0.4cm. It is made of stainless steel. The sealing ring is made of rubber.

[0043] Example 4 Novel column chromatography device structure

[0044] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0045] The cylinder is made of polypropylene resin. The screen is circular, with a diameter consistent with the outer diameter of the cylinder. It is a single-layer, 300-mesh sieve made of polyethylene (PE). The perforated separator in the screen assembly is circular, with a diameter consistent with the sieve, a pore size of 8.5 mm, and a thickness of 0.5 cm. It is made of stainless steel. The sealing ring is made of rubber.

[0046] Example 5 Novel column chromatography device structure

[0047] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0048] The cylinder is made of polypropylene resin. The screen is circular, with a diameter consistent with the outer diameter of the cylinder. It is a single-layer screen with a pore size of 300 mesh and is made of polypropylene (PP). The perforated separator in the screen assembly is circular, with a diameter consistent with the screen, a pore size of 8.5mm, and a thickness of 0.5cm. It is made of stainless steel. The sealing ring is made of rubber.

[0049] Example 6 Novel column chromatography device structure

[0050] The utility model discloses a column chromatography device for separating components of traditional Chinese medicine, which is composed of a chromatography column, a top cover, a bottom cover and a screen assembly. The screen assembly is composed of a screen, a partition plate with holes and a sealing ring.

[0051] The cylinder is made of polypropylene resin. The screen is circular, with a diameter matching the outer diameter of the cylinder. It is a single-layer, 300-mesh sieve made of polyester (PET). The perforated separator in the screen assembly is circular, with a diameter matching the sieve, an 8.5mm pore size, and a thickness of 0.5cm. It is made of stainless steel. The sealing ring is made of rubber.

[0052] Example 7: Experimental Study on Isolation and Purification of Icariin Using a New Column Chromatography Device

[0053] The same batch of icariin extract concentrate was taken and enriched using a conventional column chromatography apparatus (purchased from Taicang Jiaye Environmental Protection Equipment Co., Ltd., model DN250) and a macroporous resin column chromatography apparatus for separation of Chinese medicine components in Example 1 of the present invention. The filler was polyamide, and the same eluent and elution volume were used. The time required for elution to complete was recorded. After the eluent was concentrated, the yield of icariin was determined. The experimental results are as follows:

[0054]

[0055] The test results show that, under the same conditions, conventional resin column chromatography devices cannot achieve the optimized elution flow rate during pilot tests due to the precipitation of impurities during the elution process, which prolongs the adsorption time of the target product on the resin and increases the amount of dead adsorption. However, the novel resin column chromatography device of the present invention has an adjustable elution flow rate and a screen assembly that allows precipitated impurities to pass through, greatly improving production efficiency. Therefore, from a comprehensive analysis of the need for resin treatment before sample loading, elution time, content, and yield, the novel column chromatography device has significant advantages.

[0056] Example 8: Experimental Study on Separation and Purification of Ginkgo Bilobalide Using a New Column Chromatography Apparatus

[0057] The same batch of ginkgo leaf extract concentrate was taken and enriched with a conventional column chromatography apparatus (purchased from Taicang Jiaye Environmental Protection Equipment Co., Ltd., model DN250) and a column chromatography apparatus for separating Chinese medicinal ingredients in Example 1 of the present invention. The filler was D101 resin. The same eluent and the same elution volume were used. The time required for elution to complete was recorded. After the eluent was concentrated, the yield of ginkgo lactones was determined. The experimental results are as follows:

[0058]

[0059]

[0060] The test results show that, under the same conditions, conventional resin column chromatography devices cannot achieve the optimized elution flow rate during small-scale tests due to the precipitation of impurities during the elution process, which prolongs the adsorption time of the target product on the filler and increases the amount of dead adsorption. However, the new column chromatography device of the utility model has an adjustable elution flow rate and a screen assembly that allows precipitated impurities to pass through. At the same time, neither the filler nor the extract requires complex processing before sample loading, greatly improving production efficiency. Comprehensive analysis shows that the new column chromatography device has obvious advantages compared to conventional chromatography columns.

[0061] When using the new column chromatography device of Examples 2-8 of the present invention to separate traditional Chinese medicine components, the filler and the extract do not require complicated processing before loading, which greatly improves production efficiency. In addition, the new column chromatography device of Examples 2-8 of the present invention can adjust the elution flow rate, precipitate and filter impurities, and has significant technical advantages in elution time, content, yield, etc., and can achieve better technical effects than conventional column chromatography devices in the prior art.

[0062] The above describes the basic principles and main features of the present invention, as well as the advantages of the present invention. Those skilled in the art should be aware that the above embodiments should not be considered as limitations of the present invention, and any improvements and perfections made based on the principles of the present invention fall within the scope of protection defined by the claims of the present invention.

Claims

1. A novel column chromatography device for separating components of traditional Chinese medicine, the novel column chromatography device mainly comprising a chromatography column (1), a top cover (2), a bottom cover (3), and a screen assembly (4); The top cover (2) and the bottom cover (3) are fixed to the column (1) by screws. The top cover (2) is provided with a water inlet (10) and a pressure port (12), and is provided with a water inlet switch (11) and a pressure port switch (13). The column has a filler inlet (8) at the upper end and a filler outlet (7) at the lower end. The column is provided with a sight glass (9). The bottom cover (3) is provided with a water outlet (5) and is provided with a water outlet switch (6). Its characteristics are: The screen assembly (4) is located between the bottom cover and the column, and the screen assembly (4) is composed of a screen (a), a perforated partition (b) and a sealing ring (c), and the stacking order from bottom to top is the screen (a), the perforated partition (b), and the sealing ring (c); The area from the screen assembly (4) to the lower edge of the filler inlet (8) is a filler filling area.

2. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The Chinese medicinal ingredients are Chinese medicinal extracts.

3. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The screen (a) in the screen assembly (4) is a single layer with an aperture size of 50-300 meshes; the screen (a) in the screen assembly (4) is circular with a diameter consistent with the outer diameter of the column.

4. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The screen (a) in the screen assembly (4) is made of metal or non-metal.

5. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 4, characterized in that: The metal material is selected from stainless steel, copper, brass, aluminum or alloys thereof, and the non-metal material is selected from nylon, polypropylene PP, polyethylene PE or polyester fiber PET.

6. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 5, characterized in that: The screen (a) in the screen assembly (4) is made of stainless steel.

7. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The perforated partition (b) in the screen assembly (4) has a pore diameter of 5-10 mm and a thickness of 0.2-0.5 cm.

8. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The perforated partition (b) in the screen assembly (4) is circular, and its diameter is consistent with that of the screen (a); the perforated partition (b) in the screen assembly (4) is made of metal.

9. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 8, characterized in that: The porous partition (b) in the screen assembly (4) is made of stainless steel.

10. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The sealing ring (c) is made of silicone or rubber.

11. The novel column chromatography device for separating components of traditional Chinese medicine according to claim 1, characterized in that: The filler is resin, polyamide or silica gel.

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