Device for separating, purifying and preparing triptolide content determination sample in tripterygium wilfordii-containing preparation

Abstract

The utility model relates to the technical field of determination samples, and discloses a device for separating, purifying and preparing a triptolide content determination sample in a tripterygium wilfordii-containing preparation, which comprises a bottom plate and a support plate, an iron stand is fixedly connected on the bottom plate, one end of the iron stand far away from the bottom plate is fixedly connected with a connecting rod, and the other end of the iron stand is fixedly connected with the support plate. The end, away from the iron support, of the connecting rod is fixedly connected with a clamp, and a separation column is clamped on the clamp. According to the device, multiple steps of filtering, separating, purifying and concentrating are integrated and can be carried out at the same time, the experiment time is saved, the device is high in mobility and can be assembled and used on a common laboratory table top, dependence on a fuming cupboard is overcome, a negative pressure system can be formed in the solvent evaporation process, the concentration process is accelerated, and the concentration efficiency is improved. Meanwhile, the glass cover and the water bath kettle system below the glass cover can play a role in drying under reduced pressure, so that the evaporation temperature can be reduced in a reduced pressure environment, and the damage to thermally unstable components can be reduced.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of sample determination, especially to a device for separating, purifying and preparing a sample for determining the content of triptolide in a triptolide-containing preparation. BACKGROUND

[0002] Tripterygium wilfordii Hook. f. is a plant of Celastraceae, and its main medicinal parts are roots or xylem of roots. It is bitter and cold in nature, and belongs to the liver and kidney channels. It has the functions of expelling wind and dampness, promoting blood circulation to remove meridian obstruction, relieving swelling and pain, killing insects and detoxifying. It is mainly produced in Zhejiang, Jiangsu, Anhui, Fujian, Guangdong and other places. Tripterygium wilfordii has complex chemical components and wide pharmacological effects. It has been widely used in the treatment of rheumatoid arthritis, nephritis, lupus erythematosus, diabetes and various skin diseases. Among them, triptolide is one of the main effective components of Tripterygium wilfordii. Triptolide belongs to diterpenoids. Studies have shown that it has anti-inflammatory, antitumor and immunosuppressive activities, antioxidant and antirheumatoid effects. These characteristics make it have important application value in the medical field.

[0003] But the content of triptolide in the plant of Tripterygium wilfordii Hook.f. is not high, and the traditional extraction process is complex, which needs to be separated by multiple extraction and chromatography. This not only consumes time and effort, but also has low utilization rate and concentration of medicinal materials, and it is difficult to achieve the ideal application effect. Passing the extraction liquid through the neutral alumina column is a relatively common method for removing impurities from Tripterygium wilfordii medicinal materials and preparations, but the operation method or steps described in the existing reports are too complicated (for example, the patent with the application publication number CN109239213A needs to go through 10 steps of "ultrasonic extraction - filtration - washing the filter residue twice - combining the filtrate and concentrating - methanol redissolution - column - acetone elution - eluent concentration - methanol redissolution - constant volume" when preparing the test solution of the test product), or the solvents used are highly toxic (for example, the patent with the publication number CN101339168A uses chloroform for extraction; "Gedan Dan, Gao Jiarong, Bao Xuemei, et al. Determination of triptolide and red element content in Tripterygium wilfordii slices from different producing areas by UHPLC [J]. Guangzhou Chemical Industry, 2020, 48(16): 91-93." uses acetonitrile solution for extraction and dichloromethane solution for elution; "Li Yungui, Qiao Yina, Zhang Li, et al. Determination of triptolide content in different parts of Tripterygium wilfordii under different interplanting modes by HPLC [J]. Anhui Agricultural Sciences, 2019, 47(23): 219-221." uses chloroform solution for extraction and diethyl ether solution for elution), or the solvents used in the whole process are complex (for example, "Gao Li, Nie Zhongbiao, Yue Xiaohua, et al. Determination of triptolide content in Tripterygium wilfordii medicinal materials from different producing areas [J]. Shanxi Journal of Traditional Chinese Medicine, 2012, 28(08): 42-44." first uses 95% ethanol for extraction, then uses ethyl acetate for elution after concentration and column, and then uses 95% ethanol for extraction after concentration). In addition, toxic solvents such as chloroform, dichloromethane and acetone are often used in the extraction, separation and purification process. In order to protect the safety of the operator, the column passing, elution and concentration processes are usually carried out in a fume hood, which has high requirements for experimental conditions and is not flexible in operation place. Therefore, a simple, flexible and safe separation, purification and preparation device is needed for preparing the test product for determining the content of triptolide in Tripterygium wilfordii preparations. Practical new type content

[0004] The purpose of the present application is to solve the problems existing in the prior art, and a device for separating, purifying and preparing the sample for determining the content of triptolide in Tripterygium wilfordii preparations is provided.

[0005] In order to achieve the above object, the utility model discloses the following technical scheme: a device for separating, purifying and preparing the sample for determining the content of triptolide in tripterygium wilfordii preparation, including bottom plate, support plate, the bottom plate is fixedly connected with iron stand, one end of the iron stand away from the bottom plate is fixedly connected with connecting rod, one end of the connecting rod away from the iron stand is fixedly connected with the clamp, and the clamp is clamped with the separation column, the top of the separation column is placed with the wrinkle funnel, and the middle part of the separation column is provided with the degreasing cotton, and the bottom of the separation column is fixedly connected with the liquid outlet pipe.

[0006] As a further description of the above technical scheme:

[0007] The both ends of the support plate are fixedly connected with the limiting plate, a group of the limiting plate is rotatably connected with the drive shaft, one end of the drive shaft is fixedly connected with the rotating disc, one end of the drive shaft away from the rotating disc is fixedly connected with the two-way screw rod, one end of the two-way screw rod away from the drive shaft is rotatably connected with the limiting plate, the both sides of the two-way screw rod are rotatably connected with the screw block, the screw block is rotatably connected with the support connecting rod, and one end of the support connecting rod away from the screw block is rotatably connected with the water bath pot.

[0008] As a further description of the above technical scheme:

[0009] The water bath pot is attached with the glass cover, and a sealing rubber strip is arranged between the water bath pot and the glass cover, the water bath pot is provided with a round hole, the round hole can be placed with the evaporation dish, and the glass cover can cover above the evaporation dish.

[0010] As a further description of the above technical scheme:

[0011] The glass cover is rotatably connected with the air pump, and the glass cover is rotatably connected with the rubber plug, the rubber plug is rotatably connected with the liquid outlet pipe, and one end of the liquid outlet pipe away from the separation column is located in the interior of the glass cover.

[0012] As a further description of the above technical scheme:

[0013] The support plate is rotatably connected with the telescopic rod, and one end of the telescopic rod away from the support plate is rotatably connected with the water bath pot.

[0014] As a further description of the above technical scheme:

[0015] The support plate is provided with the sliding groove, the sliding groove is rotatably connected with the sliding block, and one end of the sliding block away from the sliding groove is rotatably connected with the screw block.

[0016] As a further description of the above technical scheme:

[0017] The bottom of the support plate is rotatably connected with the support leg, the support leg is provided with four groups, and the four groups of support legs are evenly distributed on the bottom of the support plate.

[0018] The utility model has the following beneficial effects:

[0019] 1. The utility model discloses a filter, separation, purification, concentration multiple steps are integrated, can be carried out simultaneously, save experiment time, the device can be movable, can be assembled and used on the ordinary laboratory mesa, overcome the dependence on the fume hood, and the evaporation solvent process can form a negative pressure system, accelerate the concentration process, the glass cover and the lower water bath system can play the role of the drying under reduced pressure after close adhesion, under the reduced pressure environment, can reduce the evaporation temperature, can reduce the damage to the heat labile component. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 A structure diagram of the device for separating, purifying and preparing the sample for determining the content of triptolide in the tripterygium-containing preparation is provided in the utility model Figure 1 ;

[0021] Figure 2 A structure diagram of the device for separating, purifying and preparing the sample for determining the content of triptolide in the tripterygium-containing preparation is provided in the utility model Figure 2 ;

[0022] Figure 3 A partial sectional view of the device for separating, purifying and preparing the sample for determining the content of triptolide in the tripterygium-containing preparation is provided in the utility model

[0023] Figure 4 A Figure 2 enlarged view of A in the utility model is provided

[0024] Figure 5 A Figure 3 enlarged view of B in the utility model is provided

[0025] LEGEND

[0026] 1, base plate, 2, iron stand, 3, connecting rod, 4, clamp, 5, separation column, 6, pleated funnel, 7, absorbent cotton, 8, liquid outlet pipe, 9, support plate, 10, limit plate, 11, drive shaft, 12, turntable, 13, two-way threaded rod, 14, threaded block, 15, support connecting rod, 16, sliding groove, 17, sliding block, 18, water bath, 19, round hole, 20, glass cover, 21, evaporating dish, 22, air pump, 23, rubber plug, 24, telescopic rod, 25, support leg, 26, first piston, 27, second piston, 28, third piston. DETAILED DESCRIPTION

[0027] Clearly, the described embodiments are merely a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the protection scope of the present application.

[0028] Embodiment: please refer to Figures 1-5 The utility model provides a kind of for separating, purifying and preparation of the device of the sample for determining the content of triptolide in triptolide preparation, including bottom plate 1, support plate 9, and the iron stand 2 of fixed connection is connected on bottom plate 1, the end of iron stand 2 away from bottom plate 1 is fixedly connected with connecting rod 3, the end of connecting rod 3 away from iron stand 2 is fixedly connected with clamp 4, and clamp 4 is clamped with separation column 5, and the top of separation column 5 is placed with wrinkle funnel 6, and the middle part of separation column 5 is provided with absorbent cotton 7, the absorbent cotton 7 can be removed, while the bottom of separation column 5 is fixedly connected with liquid outlet pipe 8, and third piston 28 is equipped on liquid outlet pipe 8, while first piston 26 and second piston 27 are equipped on glass cover 20, and suction pump 22 is equipped on second piston 27.

[0029] Working principle: first open the third piston 28 on the outlet pipe 8, while the second piston 27 on the suction pump 22 is in the closed state, the end of the suction pump is connected to the exhaust filter (toxic solvent vapor adsorption treatment), then rotate the rotating disc 12, the rotating disc 12 drives the driving shaft 11 to rotate, the driving shaft 11 drives the bidirectional threaded rod 13 to rotate, the bidirectional threaded rod 13 drives the two sets of threaded blocks 14 to move relative to each other, the two sets of threaded blocks 14 drive the support connecting rod 15 to rotate, the support connecting rod 15 drives the water bath pot 18 to rise and fall, so that the water bath pot 18 and the upper glass cover 20 are in a separated state (the lower edge of the cover is about 3-5 cm away from the plane of the water bath pot 18), the evaporating dish 21 is located directly below the outlet pipe 8 of the separation column 5, and the lower end is about 2-3 cm away from the upper edge of the evaporating dish 21; adjust the temperature of the water bath pot 18 to the appropriate (60-70℃), slowly pour the extracted solution containing tripterygium preparation into the upper end of the creased funnel 6 (filter paper has been placed), wash the drug residue with an appropriate amount of extraction solvent, pour it into the creased funnel for filtration, wash 2-3 times, the filtered solution (primary filtrate) drops onto the filter paper 7 (to prevent the filler from being washed up), the relevant components in the primary filtrate are adsorbed after the filler (Al2O3), and the liquid is about to drop from the outlet pipe 8. Open the suction pump 22 (the glass cover 20 acts as a ventilation cover to remove the solvent vapor evaporated) before the liquid drops from the outlet pipe 8. Slowly add the eluent from the upper end of the creased funnel 6 to elute the triptolide adsorbed in the filler, and the eluate flows into the lower evaporating dish 21. After water bath heating, the solvent is evaporated, and the solvent vapor is removed through the outlet of the second piston 27 on the suction pump 22. When the liquid in the upper separation column 5 no longer falls naturally, adjust the height of the water bath pot to match the glass cover (there is a sealing strip in the groove), the residual liquid in the filler column is further sucked out, and when there is no liquid dropping, close the third piston 28 on the outlet pipe 8, so that a negative pressure environment is formed in the glass cover 20, the boiling point of the solvent is reduced, and the evaporation is accelerated. After the solvent in the evaporating dish 21 is evaporated, close the piston 27 on the suction pump 22, close the suction pump 22, open the first piston 26 on the glass cover 20, so that the air pressure inside and outside the glass cover 20 is consistent, adjust the height of the glass cover to separate from the water bath pot, take out the evaporating dish 21, and the residue in the dish is the sample containing triptolide after separation, purification and enrichment. After being redissolved and constant volume with a suitable solvent, it can be used for quantitative analysis.

[0030] As a preferred implementation, the two ends of the support plate 9 are fixedly connected with the limiting plates 10, a set of limiting plates 10 is rotatably connected with the driving shaft 11 penetrating through, one end of the driving shaft 11 is fixedly connected with the rotating disc 12, one end of the driving shaft 11 away from the rotating disc 12 is fixedly connected with the bidirectional threaded rod 13, one end of the bidirectional threaded rod 13 away from the driving shaft 11 is rotatably connected with the limiting plate 10, the two sides of the bidirectional threaded rod 13 are threadedly connected with the threaded blocks 14, the threaded blocks 14 are hingedly connected with the support connecting rods 15, one end of the support connecting rods 15 away from the threaded blocks 14 is hingedly connected with the water bath pot 18.

[0031] As shown in Figure 3 : the threaded blocks 14 are provided in two groups, and the two groups of threaded blocks 14 are connected to the left-handed and right-handed of the bidirectional threaded rod 13 respectively.

[0032] As a preferred implementation, the water bath pot 18 is attached with the glass cover 20, and a sealing rubber strip is arranged between the water bath pot 18 and the glass cover 20, the water bath pot 18 is provided with the round hole 19, the evaporation dish 21 is placed on the round hole 19, and the glass cover 20 can cover the evaporation dish 21.

[0033] As shown in Figure 1 : this facilitates the separation and combination of the glass cover 20 and the water bath pot 18.

[0034] As a preferred implementation, the glass cover 20 is fixedly connected with the air suction pump 22 penetrating through, and the glass cover 20 is fixedly connected with the rubber plug 23, the rubber plug 23 is fixedly connected with the liquid outlet pipe 8 penetrating through, and one end of the liquid outlet pipe 8 away from the separation column 5 is located inside the glass cover 20.

[0035] As shown in Figure 3 : the air suction pump 22 is provided with the second piston 27, and the third piston 28 is arranged on the liquid outlet pipe 8 and located directly above the evaporation dish 21.

[0036] As a preferred implementation, the support plate 9 is fixedly connected with the telescopic rods 24, and one end of the telescopic rods 24 away from the support plate 9 is fixedly connected with the water bath pot 18.

[0037] As shown in Figure 3 : the telescopic rods 24 are provided in four groups, and the four groups of telescopic rods 24 are uniformly distributed on the support plate 9 and the water bath pot 18.

[0038] As a preferred implementation, the support plate 9 is provided with the sliding groove 16, the sliding block 17 is slidingly connected in the sliding groove 16, and one end of the sliding block 17 away from the sliding groove 16 is fixedly connected with the threaded block 14.

[0039] As shown in Figure 5 : the sliding block 17 slides in the sliding groove 16, which can limit and guide the movement of the threaded block 14.

[0040] As a preferable embodiment, the bottom of the support plate 9 is fixedly connected with support legs 25, and the support legs 25 are provided in four groups, which are evenly distributed on the bottom of the support plate 9.

[0041] Finally, it should be noted that: the above only for the preferred embodiments of the present application, and is not intended to limit the present application, although the foregoing embodiments of the present application have been described in detail, for those skilled in the art, it still can be modified, or part of the technical features of the equivalent replacement, within the spirit and principles of the present application, any modification, equivalent replacement, improvement, etc., should be included within the scope of the present application.

Claims

1. A device for separating, purifying and preparing a sample for determining the content of triptolide in a triptolide preparation, comprising a bottom plate (1) and a support plate (9), characterized in that: An iron frame (2) is fixedly connected to the bottom plate (1), a connecting rod (3) is fixedly connected to one end of the iron frame (2) away from the bottom plate (1), a clamp (4) is fixedly connected to one end of the connecting rod (3) away from the iron frame (2), a separation column (5) is clamped on the clamp (4), a pleated funnel (6) is placed on the top of the separation column (5), and a cotton ball (7) is provided in the middle of the separation column (5), and a liquid outlet pipe (8) is fixedly connected to the bottom of the separation column (5).

2. The device for separating, purifying and preparing a sample for determining the content of triptolide in a tripterygium wilfordii preparation according to claim 1, wherein: The two ends of the support plate (9) are fixedly connected to the limit plates (10), and a driving shaft (11) is rotatably connected to one group of the limit plates (10). One end of the driving shaft (11) is fixedly connected to a turntable (12), and the end of the driving shaft (11) away from the turntable (12) is fixedly connected to a bidirectional threaded rod (13). The end of the bidirectional threaded rod (13) away from the driving shaft (11) is rotatably connected to the limit plates (10), and threaded blocks (14) are threadedly connected to the two sides of the bidirectional threaded rod (13). A supporting connecting rod (15) is hinged on the threaded block (14), and the end of the supporting connecting rod (15) away from the threaded block (14) is hinged to a water bath (18).

3. The device for separating, purifying and preparing a sample for determining the content of triptolide in a tripterygium wilfordii preparation according to claim 2, wherein: A glass cover (20) is attached to the water bath (18), and a sealing strip is provided between the water bath (18) and the glass cover (20). A circular hole (19) is provided on the water bath (18), an evaporating dish (21) can be placed on the circular hole (19), and the glass cover (20) can cover the evaporating dish (21).

4. The device for separating, purifying and preparing a sample for determining the content of triptolide in a triptolide preparation according to claim 3, wherein: An air pump (22) is fixedly connected to the glass cover (20), and a rubber stopper (23) is fixedly connected to the glass cover (20). The rubber stopper (23) is fixedly connected to the liquid outlet pipe (8), and the end of the liquid outlet pipe (8) away from the separation column (5) is located inside the glass cover (20).

5. The device for separating, purifying and preparing a sample for determining the content of triptolide in a tripterygium wilfordii preparation according to claim 4, characterized in that: A telescopic rod (24) is fixedly connected to the support plate (9), and one end of the telescopic rod (24) away from the support plate (9) is fixedly connected to the water bath (18).

6. The device for separating, purifying and preparing a sample for determining the content of triptolide in a triptolide preparation according to claim 5, characterized in that: The support plate (9) is provided with a sliding groove (16), a slider (17) is slidably connected in the sliding groove (16), and one end of the slider (17) away from the sliding groove (16) is fixed to the threaded block (14).

7. The device for separating, purifying and preparing a sample for determining the content of triptolide in a triptolide-containing preparation according to claim 6, characterized in that: The bottom of the support plate (9) is fixedly connected with support legs (25), and the support legs (25) are provided in four groups, and the four groups of support legs (25) are evenly distributed on the bottom of the support plate (9).

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