Extraction process of schisandra chinensis in Shenqi schisandra chinensis capsule

Abstract

The invention relates to the technical field of traditional Chinese medicine extraction processes, in particular to an extraction process of schisandra chinensis in Shenqi schisandra chinensis capsules. An extraction process of schisandra chinensis in a Shenqi schisandra chinensis capsule comprises the following steps: S1, firstly, removing a shell of the Shenqi schisandra chinensis capsule, and then performing non-polar supercritical extraction on a filler of the Shenqi schisandra chinensis capsule by taking CO2 as a solvent and methanol as an entrainer to obtain a supercritical fluid extraction effluent; s2, the supercritical fluid extraction effluent is analyzed, and a schisandrin B extract is obtained; s3, the schisandrin B extract is purified through AB-8 resin, and a schisandrin B purified product is obtained. The product extracted by the extraction process of the schisandra chinensis in the Shenqi schisandra chinensis capsule disclosed by the invention has higher content of schisandrin B.

Description

Technical Field

[0001] The present application relates to the technical field of traditional Chinese medicine extraction technology, and more specifically, it relates to an extraction technology of Schisandra chinensis in Shenqi Schisandra chinensis capsules. Background Art

[0002] Shenqi Schisandra Capsule is a Chinese patent medicine mainly composed of Schisandra chinensis, Codonopsis pilosula, and Astragalus membranaceus, with corn starch as an auxiliary material. It has the effects of strengthening the spleen and replenishing qi, calming the mind and tranquilizing the nerves. It has a certain effect in treating insomnia, nightmares, forgetfulness, fatigue, palpitations, shortness of breath, spontaneous sweating and other symptoms caused by insufficient qi and blood, and deficiency of both heart and spleen.

[0003] Schisandra chinensis is one of the important ingredients of Codonopsis pilosula and Schisandra chinensis capsules. Extracting effective ingredients from it can further study its pharmacological effects and detect the content of effective ingredients in Shenqi Schisandra chinensis capsules. The chemical components of Schisandra chinensis mainly include lignans and volatile oil components. The components of lignans include schisandrin A, schisandrin B, schisandrin C, schisandrin A, schisandrin B, schisandrin ester A, schisandrin ester B, etc. Among them, schisandrin B is considered to be one of the main effective ingredients of Schisandra chinensis medicinal materials.

[0004] At present, the main extraction method of schisandrin B is water bath heating reflux extraction. However, schisandrin B contains oxygen rings in its structure. Therefore, during water bath heating reflux extraction, long-term heating and reflux will destroy the effective ingredients, resulting in a low extraction content of schisandrin B. Summary of the invention

[0005] In order to improve the defect of low content of schisandrae B extracted by conventional water bath heating reflux extraction method, the present application provides an extraction process of schisandrae in Shenqi Schisandrae Chinensis Capsules.

[0006] The present application provides a process for extracting Schisandra chinensis from Shenqi Schisandra chinensis capsules, which adopts the following technical solution: A process for extracting Schisandra chinensis from Shenqi Schisandra chinensis capsules comprises the following steps: S1. First, remove the outer shell of the Shenqi Schisandra capsule, and then use CO2 as a solvent and methanol as an entrainer to perform non-polar supercritical extraction on the Shenqi Schisandra capsule filling to obtain a supercritical fluid extraction effluent; S2, analyzing the supercritical fluid extraction effluent to obtain schisandra chinensis B extract; S3, soaking the AB-8 resin in an ethanol solvent, then filtering and washing with ethanol until there is no turbidity, washing the AB-8 resin with distilled water until there is no ethanol, and soaking it in distilled water for later use; The moisture on the surface of the AB-8 resin is absorbed dry, and then the dried AB-8 resin is added to the schisandra chinensis B extract and shaken, and then filtered. The filtered AB-8 resin is added to distilled water and shaken, and then immersed in methanol and shaken, filtered, and the filtrate is taken and analyzed again to obtain purified schisandra chinensis B.

[0007] Compared with the ethanol reflux extraction method, the supercritical CO2 extraction method of the present application avoids the loss of schisandrin B caused by long-term heating. At the same time, the extraction equipment is simple, the operation is easy, the organic solvent residue is small, the extraction rate of the effective ingredient is high, and the impurities are small.

[0008] At the same time, AB-8 resin is also used in this application to purify the schisandrin B extract. Specifically, schisandrin B is a low-polarity small molecule compound, and AB-8 resin is a weakly polar macroporous adsorption resin. It does not contain any functional groups, and the pore surface is extremely hydrophobic. It can adsorb organic matter in the solution through the action of the hydrophobic part in the small molecule, thereby adsorbing schisandrin B.

[0009] However, the adsorption and desorption of schisandrin B on AB-8 resin are the result of the competition between the adsorption of macroporous adsorption resin and the solubility of solvent. When the adsorption effect produced by intermolecular forces is dominant, the effective ingredient is adsorbed on the resin. When the solubility of the solvent is dominant, the schisandrin B component is eluted from the resin.

[0010] Therefore, in the subsequent water washing process, the water-soluble impurities such as proteins, pigments, inorganic salts, etc. present in the schisandrin B extract have a large solubility in water, and the weakly polar AB-8 resin has a weak adsorption force on these impurities, making the impurities easily washed away by water, thereby achieving the purpose of impurity removal; and schisandrin B has poor water solubility and is easily soluble in methanol. Therefore, in the subsequent methanol washing, schisandrin B can be dissolved in methanol, thereby achieving the purification and collection of schisandrin B.

[0011] Preferably, in S1, the feeding amount of the filling material of the Shenqi Schisandra capsule is 180-220 g; and / or; The extraction pressure is 20-40Mpa; and / or; The extraction temperature is 30-50°C; and / or; The extraction time is 1-3h; and / or; CO2 flow rate 8-12kg / h.

[0012] Pressure is one of the important parameters in supercritical CO2 extraction. Increasing the pressure will not only increase the density of CO2, but also reduce the mass transfer distance and increase the mass transfer efficiency between the solute and the solvent, thereby promoting the extraction of schisandrin B. However, the density of CO2 under high pressure is relatively large and its compressibility is low. It is difficult to significantly increase the solubility rate by increasing the pressure. Therefore, after comprehensive consideration, 30MPa is the best extraction pressure.

[0013] The increase in temperature can increase the diffusion coefficient of molecules, reduce the viscosity of supercritical CO2 fluid, increase the mass transfer coefficient, and thus promote the extraction. However, when the temperature is too high, the density of supercritical CO2 fluid decreases and the solubility rate of components decreases, which is not conducive to extraction. In addition, too high a temperature will increase operating energy consumption and increase costs. Therefore, 40°C is the best extraction temperature.

[0014] As the extraction time increases, the mass transfer reaches a good state and the extraction rate per unit time increases. However, as the extraction time is further extended, the extraction rate gradually decreases due to the decrease in the content of the components to be separated in the extraction object. Therefore, 2h is the best extraction time.

[0015] Preferably, in S2 and S3, the analysis process is divided into two stages, the first stage analysis pressure is 5-10Mpa, the first stage analysis temperature is 35-50°C; the second stage analysis pressure is 4-8MPa, the second stage analysis temperature is 35-45°C.

[0016] Preferably, the specific steps of S3 are: Soak the AB-8 resin in 2 volumes of ethanol solvent for 24 hours, then filter and wash with ethanol until there is no turbidity, wash the AB-8 resin with distilled water until there is no ethanol, and soak it in distilled water for later use; The moisture on the surface of the AB-8 resin is absorbed dry, and then 1-2g of the dry AB-8 resin is added to 40-60ml of schisandra B extract, and the mixture is shaken at 20-30°C for 24h at a shaking speed of 50-70r / min. The mixture is then filtered, and the filtered AB-8 resin is added to 40-60ml of distilled water, and the mixture is shaken at 20-30°C for 1-3h. The mixture is then soaked in methanol, shaken at 20-30°C for 24h, filtered, and the filtrate is taken. The filtrate is analyzed again. The analysis process is divided into two stages. The first stage analysis pressure is 5-10Mpa, and the first stage analysis temperature is 35-50°C; the second stage analysis pressure is 4-8MPa, and the second stage analysis temperature is 35-45°C, to obtain purified schisandra B.

[0017] Preferably, the step of detecting the schisandrin B content of the purified schisandrin B is: First, add chromatographic methanol to 8-12 mg of purified schisandrin B, oscillate ultrasonically for 25-35 min, transfer quantitatively to a 10 ml volumetric flask, dilute to scale with methanol, shake well, filter through a 0.45 μm microporous membrane, and perform HPLC analysis; Chromatographic conditions of HPLC: Chromatographic column: Symmetry-C 18 Chromatographic column (4.6 mm × 180 mm, 5 μm); Mobile phase: methanol-water (70:30); Column temperature: 20°C; Injection volume: 10 μL; Detection wavelength: 254nm; Flow rate: 1.0 mL / min; Finally, the schisandrin B content of the purified schisandrin B was obtained using the schisandrin B standard curve.

[0018] Preferably, in S1, the operation of removing the shell of the Shenqi Schisandrae Chinensis Capsule is performed by an automatic shelling machine; The automatic shelling machine comprises a conveying plate, a shelling assembly and a collecting assembly, wherein the conveying plate is used to transfer the Shenqi Schisandra capsules from the rotating vibration plate to the shelling assembly, the shelling assembly is used to remove the shell of the Shenqi Schisandra capsules, and the collecting assembly is used to separate and store the shell of the Shenqi Schisandra capsules and the filling of the Shenqi Schisandra capsules; The conveying plate is gradually inclined downward from the rotating vibration disk toward the collecting assembly, and a baffle for limiting the movement of the Shenqi Schisandra capsule is provided at one end of the conveying plate away from the rotating vibration disk, a chute is provided on the conveying plate, one end of the Shenqi Schisandra capsule passes through the chute, and the other end of the Shenqi Schisandra capsule is mounted on the conveying plate; The shelling assembly includes a base rotatably connected to the conveying plate, a clamping claw slidably connected to the base, and a driving member arranged on the base, the driving member drives the clamping claw to move, the clamping claw clamps one end of the ginseng, astragalus and schisandra capsule passing through the slide groove, the driving member drives the base and the clamping claw to rotate, and the clamping claw cooperates with the conveying plate to shell the ginseng, astragalus and schisandra capsule.

[0019] Preferably, the driving member comprises a driving cylinder, a driving rack fixedly connected to the output end of the driving cylinder, a driving gear fixedly connected to the end of the conveying plate, and a slide fixedly connected to the side wall of the driving rack, the driving rack is slidably connected to the base through the slide, a compression spring is provided on one side of the slide, and one end of the compression spring away from the slide is connected to the clamping claw; The driving rack drives the clamping jaw to move through the slide plate, and after the clamping jaw clamps the Shenqi Schisandra Capsule, the driving rack and the driving gear are meshed with each other, and the slide plate still has room to move, and the movement of the driving rack drives the rotation of the base.

[0020] Preferably, a limiting shaft is provided at both ends of the clamp, and the compression spring and the slide plate are sequentially passed through the end of the limiting shaft away from the clamp; a limiting nut is provided at the end of the limiting shaft away from the clamp, and the inner wall of the limiting nut abuts against the outer wall of the slide plate.

[0021] Preferably, the collecting assembly includes a collecting box and a filter plate, the collecting box is placed directly below the conveying plate and the shelling assembly, the filter plate is mounted in the collecting box, the filter plate is inclined, the filter plate is used to collect the outer shell of the ginseng, astragalus and schisandra capsules, and the collecting box is used to collect the filling of the ginseng, astragalus and schisandra capsules.

[0022] When performing the extraction process of Schisandra chinensis in Ginseng, Astragalus and Schisandra chinensis Capsules, a large amount of Ginseng, Astragalus and Schisandra chinensis Capsules filler is required, and the manual shelling operation of Ginseng, Astragalus and Schisandra chinensis Capsules is rather cumbersome and has poor detection efficiency. The automatic shelling machine in the present application can effectively improve the shelling efficiency of Ginseng, Astragalus and Schisandra chinensis Capsules.

[0023] Specifically, when it is necessary to peel the ginseng, astragalus and schisandra capsules, the staff can first add excess ginseng, astragalus and schisandra capsules to the rotating vibration disk, and then under the action of the rotating vibration disk, a number of ginseng, astragalus and schisandra capsules are gradually transferred to the conveying plate, that is, one end of the ginseng, astragalus and schisandra capsules passes through the slide groove, and the other end of the ginseng, astragalus and schisandra capsules is placed on the conveying plate.

[0024] When the slide is filled with ginseng, astragalus and schisandra capsules, the driving cylinder first drives the slide plate to move through the driving rack, and the slide plate drives the clamping claw to move and clamp one end of the ginseng, astragalus and schisandra capsule passing through the slide, and at this time, the driving rack and the driving gear are just engaged.

[0025] After that, the driving rack continues to move, and because a compression spring is provided between the slide plate and the clamping claw, the slide plate still has room for movement; at the same time, because the driving gear is fixedly connected to the sliding plate, and the base is rotatably connected to the sliding plate, the movement of the driving rack will directly drive the base to rotate, thereby completing the shelling operation of the Shenqi Schisandra capsule, and the filling of the Shenqi Schisandra capsule will be directly transferred to the collection box. After that, when the base is reset, the shell of the Shenqi Schisandra capsule will also fall off and accumulate in the corner under the tilting effect of the filter plate.

[0026] Preferably, the extraction process of Schisandra chinensis in the Shenqi Schisandrae Chinensis Capsule is also used to extract Schisandrae Chinensis ester A, Schisandrin A, Calycosin-containing glucoside and Spinosin in the Shenqi Schisandrae Chinensis Capsule.

[0027] In summary, this application has the following beneficial effects: 1. Supercritical CO2 extraction avoids the loss of schisandrin B caused by long-term heating. At the same time, the extraction equipment is simple, easy to operate, with less organic solvent residue, high extraction rate of effective ingredients and less impurities.

[0028] 2. In this application, AB-8 resin is also used to purify the schisandrin B extract. Schisandrin B is a low-polarity small molecule compound, and AB-8 resin is a weakly polar macroporous adsorption resin. It does not contain any functional groups, and the pore surface is extremely hydrophobic. It can adsorb organic matter in the solution through the action of the hydrophobic part in the small molecule, thereby adsorbing schisandrin B; However, the adsorption and desorption of Schisandrin B on AB-8 resin is the result of the competition between the adsorption of macroporous adsorption resin and the solubility of solvent. When the adsorption effect produced by the intermolecular force is dominant, the effective ingredient is adsorbed on the resin. When the solubility of the solvent is dominant, Schisandrin B is eluted from the resin. Therefore, in the subsequent water washing process, the water-soluble impurities such as proteins, pigments, inorganic salts, etc. present in the schisandrin B extract have a large solubility in water, and the weakly polar AB-8 resin has a weak adsorption force on these impurities, making the impurities easily washed away by water, thereby achieving the purpose of impurity removal; and schisandrin B has poor water solubility and is easily soluble in methanol. Therefore, in the subsequent methanol washing, schisandrin B can be dissolved in methanol, thereby achieving the purification and collection of schisandrin B. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a structural diagram of an automatic shelling machine; Figure 2 It is a schematic diagram of the structure of the shelling component; Figure 3 It is an exploded schematic diagram of the shelling assembly; Figure 4 It is a schematic diagram of the structure of the gripper; Figure 5 It is a schematic diagram of the structure of the collection component.

[0030] Figure numerals: 1. conveying plate; 2. shelling assembly; 3. collecting assembly; 11. baffle; 12. slide; 21. base; 22. clamp; 23. driving member; 31. collecting box; 32. filter plate; 231. driving cylinder; 232. driving rack; 233. driving gear; 234. slide plate; 235. compression spring; 236. limiting shaft; 237. limiting nut. DETAILED DESCRIPTION

[0031] The following is combined with Figure 1-5 , Examples 1 to 7 and Comparative Example 1 further illustrate the present application in detail.

[0032] Example 1 A process for extracting Schisandra chinensis from Shenqi Schisandra chinensis capsules comprises the following steps: S1. First, remove the outer shell of the Shenqi Schisandra capsule, and then use CO2 as a solvent and methanol as an entrainer to perform non-polar supercritical extraction on the Shenqi Schisandra capsule filling to obtain a supercritical fluid extraction effluent; Among them, the Shenqi Schisandra capsule is homemade, the feeding amount of the Shenqi Schisandra capsule filler is 200g; the extraction pressure is 30Mpa; the extraction temperature is 40℃; the extraction time is 1-3h; the CO2 flow rate is 10kg / h; In addition, the operation of removing the outer shell of the Shenqi Schisandrae Chinensis Capsule is performed by an automatic shelling machine.

[0033] Reference Figure 1 The automatic shelling machine comprises a conveying plate 1, a shelling assembly 2 and a collecting assembly 3. The conveying plate 1 is used to transfer the Shenqi Schisandra capsules from the rotating vibration plate to the shelling assembly 2, the shelling assembly 2 is used to remove the shell of the Shenqi Schisandra capsules, and the collecting assembly 3 is used to separate and store the shell of the Shenqi Schisandra capsules and the filling of the Shenqi Schisandra capsules.

[0034] Reference Figure 1 and Figure 2 The conveying plate 1 gradually tilts downward from the rotating vibration disk toward the collecting component 3, and the end of the conveying plate 1 away from the rotating vibration disk is fixedly connected with a baffle 11 for limiting the movement of the ginseng, astragalus and schisandra capsules. A slide groove 12 is provided on the upper end surface of the conveying plate 1. One end of the ginseng, astragalus and schisandra capsules passes through the slide groove 12, and the other end of the ginseng, astragalus and schisandra capsules is mounted on the conveying plate 1.

[0035] When it is necessary to shell the ginseng, astragalus and schisandra capsules, the staff can first add excess ginseng, astragalus and schisandra capsules to the rotating vibration disk, and then under the action of the rotating vibration disk, a number of ginseng, astragalus and schisandra capsules are gradually transferred to the conveying plate 1, that is, one end of the ginseng, astragalus and schisandra capsules passes through the slide groove 12, and the other end of the ginseng, astragalus and schisandra capsules is mounted on the conveying plate 1.

[0036] Reference Figure 2 and Figure 3The shelling assembly 2 includes a base 21 rotatably connected to the conveying plate 1, a clamping jaw 22 slidably connected to the base 21, and a driving member 23 arranged on the base 21. The driving member 23 drives the clamping jaw 22 to move, and the clamping jaw 22 clamps one end of the ginseng, astragalus and schisandra capsule passing through the slide groove 12. The driving member 23 drives the base 21 and the clamping jaw 22 to rotate, and the clamping jaw 22 cooperates with the conveying plate 1 to shell the ginseng, astragalus and schisandra capsule.

[0037] Specifically, the driving member 23 includes a driving cylinder 231, a driving rack 232 fixedly connected to the output end of the driving cylinder 231, a driving gear 233 fixedly connected to the end of the conveying plate 1, and a slide plate 234 fixedly connected to the side wall of the driving rack 232. The driving rack 232 is slidably connected to the base 21 through the slide plate 234. A compression spring 235 is fixedly connected to one side of the slide plate 234. The end of the compression spring 235 away from the slide plate 234 is fixedly connected to the clamp 22.

[0038] When the chute 12 is filled with the Shenqi Schisandra capsule, the driving cylinder 231 first drives the slide plate 234 to move through the driving rack 232, and the slide plate 234 drives the clamping jaw 22 to move and clamp one end of the Shenqi Schisandra capsule that passes through the chute 12. At this time, the driving rack 232 is just meshed with the driving gear 233. After that, the driving rack 232 continues to move, and since a compression spring 235 is provided between the slide plate 234 and the clamping jaw 22, the slide plate 234 still has a margin for movement; at the same time, since the driving gear 233 is fixedly connected to the sliding plate, and the base 21 is rotatably connected to the sliding plate, the movement of the driving rack 232 will directly drive the base 21 to rotate, thereby completing the shelling operation of the Shenqi Schisandra capsule.

[0039] Reference Figure 3 and Figure 4 The two ends of the clamping jaw 22 are fixedly connected to the limiting shaft 236, and the end of the limiting shaft 236 away from the clamping jaw 22 is penetrated by the compression spring 235 and the slide plate 234 in sequence; the end of the limiting shaft 236 away from the clamping jaw 22 is threadedly connected to the limiting nut 237, and the inner wall of the limiting nut 237 abuts against the outer wall of the slide plate 234. Therefore, when the driving rack 232 is reset, the movement of the slide plate 234 can drive the clamping jaw 22 to reset, so that the contact clamping jaw 22 locks the shell of the Shenqi Schisandra capsule, prompting the shell of the Shenqi Schisandra capsule to be transferred to the collection box 31.

[0040] Reference Figure 5 The collecting assembly 3 includes a collecting box 31 and a filter plate 32. The collecting box 31 is placed directly below the conveying plate 1 and the shelling assembly 2. The filter plate 32 is set in the collecting box 31. The filter plate 32 is set obliquely. The filter plate 32 is used to collect the shell of the Shenqi Schisandra capsule, and the collecting box 31 is used to collect the filling of the Shenqi Schisandra capsule.

[0041] It should be noted that in this embodiment, the fixed connection can be selected according to actual conditions by using conventional fixed connection methods such as one-piece molding, welding fixation, bolt connection, etc.; the rotational connection can be selected according to actual conditions by using conventional rotational connection methods such as pin connection, etc.; the sliding connection can be selected according to actual conditions by using conventional sliding connection methods such as slide grooves and slide rails.

[0042] S2. Analyze the supercritical fluid extraction effluent to obtain schisandra chinensis B extract.

[0043] S3, soaking the AB-8 resin in 2 volumes of ethanol solvent for 24 hours, then filtering and washing with ethanol until there is no turbidity, washing the AB-8 resin with distilled water until there is no ethanol, and soaking it in distilled water for later use; The moisture on the surface of the AB-8 resin was absorbed dry, and then 1.5 g of dry AB-8 resin was added to 50 ml of schisandra chinensis B extract, shaken at 25°C for 24 hours at a shaking speed of 60 r / min, and then filtered. The filtered AB-8 resin was added to 50 ml of distilled water, shaken at 25°C for 2 hours, and then soaked in methanol, shaken at 25°C for 24 hours, filtered, and the filtrate was taken and analyzed again to obtain purified schisandra chinensis B.

[0044] Among them, AB-8 resin was purchased from Tianjin Haoju. In S2 and S3, the analysis process is divided into two levels. The first-level analysis pressure is 10Mpa, and the first-level analysis temperature is 45°C; the second-level analysis pressure is 8MPa, and the second-level analysis temperature is 40°C.

[0045] It should be noted that the extraction process of Schisandra chinensis in the Shenqi Schisandrae Chinensis Capsules of the present application can also be used to extract the effective contents of Schisandrae Chinensis ester A, Schisandrin A, flavonoid glucoside and Spinosin in the Shenqi Schisandrae Chinensis Capsules, and the detection is to adaptively adjust the detection parameters according to the actual situation.

[0046] Example 2 The difference from Example 1 is that in S1, the extraction pressure is 20 MPa.

[0047] Example 3 The difference from Example 1 is that in S1, the extraction pressure is 40 MPa.

[0048] Example 4 The difference from Example 1 is that in S1, the extraction temperature is 30°C.

[0049] Example 5 The difference from Example 1 is that in S1, the extraction temperature is 50°C.

[0050] Example 6 The difference from Example 1 is that in S1, the extraction time is 1 h.

[0051] Example 7 The difference from Example 1 is that in S1, the extraction time is 3 h.

[0052] Comparative Example 1 A process for extracting schisandra chinensis B by solvent reflux, wherein ethanol is used as the extraction medium, and the process parameters are as follows: The feed amount is 50g, the solvent concentration is 70%; the material-liquid ratio is 7:1; the extraction time is 2.5h, the number of extractions is 3 times, and the extraction temperature is 80℃.

[0053] Performance testing Three samples were taken from Examples 1 to 7 and Comparative Example 1, and then the content of Schisandrin B in all samples was tested. The specific testing steps are as follows: First, add chromatographic methanol to 10 mg of sample, oscillate ultrasonically for 30 min, transfer quantitatively to a 10 ml volumetric flask, dilute to scale with methanol, shake well, filter through a 0.45 μm microporous membrane, and perform HPLC analysis; Chromatographic conditions of HPLC: Chromatographic column: Symmetry-C 18 Chromatographic column (4.6 mm × 180 mm, 5 μm); Mobile phase: methanol-water (70:30); Column temperature: 20°C; Injection volume: 10 μL; Detection wavelength: 254nm; Flow rate: 1.0 mL / min; Finally, the schisandrin B content of the sample was obtained through the schisandrin B standard curve.

[0054] The test data are shown in Table 2.

[0055] Table 2 Test data table of Example 1 to Example 8 and Comparative Example 1

[0056] Referring to Example 1 and Comparative Example 1 and in combination with Table 2, it can be seen that the content of schisandrin B in Example 1 is significantly improved compared with Comparative Example 1, which shows that compared with the ethanol reflux extraction method, the supercritical CO2 extraction method of the present application can further improve the extraction content of schisandrin B.

[0057] The reason is that the supercritical CO2 extraction method of the present application avoids the loss of schisandrin B caused by long-term heating, and the extraction equipment is simple, easy to operate, with less organic solvent residue, high effective ingredient extraction rate, and less impurities. At the same time, AB-8 resin is also used in the present application to purify the schisandrin B extract, and the extraction content of schisandrin B is further improved by removing impurities.

[0058] The mechanism of AB-8 resin is as follows: Schisandrin B is a low-polarity small molecule compound, while AB-8 resin is a weakly polar macroporous adsorption resin that does not contain any functional groups. The pore surface is extremely hydrophobic and can adsorb organic matter in the solution through the action of the hydrophobic part of the small molecule, thereby adsorbing Schisandrin B.

[0059] However, the adsorption and desorption of schisandrin B on AB-8 resin are the result of the competition between the adsorption of macroporous adsorption resin and the solubility of solvent. When the adsorption effect produced by intermolecular forces is dominant, the effective ingredient is adsorbed on the resin. When the solubility of the solvent is dominant, the schisandrin B component is eluted from the resin.

[0060] Therefore, in the subsequent water washing process, the water-soluble impurities such as proteins, pigments, inorganic salts, etc. present in the schisandrin B extract have a large solubility in water, and the weakly polar AB-8 resin has a weak adsorption force on these impurities, making the impurities easily washed away by water, thereby achieving the purpose of impurity removal; and schisandrin B has poor water solubility and is easily soluble in methanol. Therefore, in the subsequent methanol washing, schisandrin B can be dissolved in methanol, thereby achieving the purification and collection of schisandrin B.

[0061] With reference to Examples 1 to 3 and in combination with Table 2, it can be seen that, relative to Example 1, the content of schisandrin B in Example 2 is significantly reduced, and the content of schisandrin B in Example 3 is also slightly reduced, which indicates that increasing the extraction pressure can effectively increase the extraction content of schisandrin B, but excessive pressure will lead to a decrease in the extraction content of schisandrin B.

[0062] The reason is that pressure is one of the important parameters in supercritical CO2 extraction. Increasing the pressure will not only increase the density of CO2, but also reduce the mass transfer distance, increase the mass transfer efficiency between the solute and the solvent, and thus promote the extraction of schisandrin B. However, the density of CO2 under high pressure is relatively large and its compressibility is low. It is difficult to significantly increase the solubility rate by increasing the pressure. Therefore, after comprehensive consideration, 30MPa is the best extraction pressure.

[0063] Referring to Example 1 and Example 4-Example 5 and combining with Table 2, it can be seen that compared with Example 1, the content of schisandrin B in Example 4-Example 5 is reduced, which shows that increasing the temperature can effectively increase the extraction content of schisandrin B, but if the temperature is too high, the extraction content of schisandrin B will decrease.

[0064] The reason is that the increase in temperature can increase the diffusion coefficient of molecules, causing the viscosity of the supercritical CO2 fluid to decrease and the mass transfer coefficient to increase, thereby promoting the extraction. However, when the temperature is too high, the density of the supercritical CO2 fluid decreases and the solubility rate of the components decreases, which is not conducive to the extraction. In addition, too high a temperature will increase operating energy consumption and increase costs. Therefore, 40°C is the best extraction temperature.

[0065] With reference to Example 1 and Example 6-Example 7 and in combination with Table 2, it can be seen that, relative to Example 1, the content of schisandrin B in Example 6 is significantly reduced, and the content of schisandrin B in Example 7 is only slightly increased. This shows that increasing the extraction time can effectively increase the extraction content of schisandrin B, but if the time is too long, the extraction content of schisandrin B does not change substantially.

[0066] The reason is that as the extraction time increases, the mass transfer reaches a good state and the extraction rate per unit time increases. However, as the extraction time is further extended, the extraction rate gradually decreases due to the decrease in the content of the components to be separated in the extraction object. Therefore, 2h is the best extraction time.

[0067] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed, but such modifications are protected by patent law as long as they are within the scope of the claims of the present application.

Claims

1. A process for extracting Schisandrae Chinensis from Shenqi Schisandrae Chinensis Capsules, characterized in that: The following steps are involved: S1. First, remove the outer shell of the Shenqi Schisandra capsule, and then use CO2 as a solvent and methanol as an entrainer to perform non-polar supercritical extraction on the Shenqi Schisandra capsule filling to obtain a supercritical fluid extraction effluent; S2, analyzing the supercritical fluid extraction effluent to obtain schisandra chinensis B extract; S3, soaking the AB-8 resin in an ethanol solvent, then filtering and washing with ethanol until there is no turbidity, washing the AB-8 resin with distilled water until there is no ethanol, and soaking it in distilled water for later use; The moisture on the surface of the AB-8 resin is absorbed dry, and then the dried AB-8 resin is added to the schisandra chinensis B extract and shaken, and then filtered. The filtered AB-8 resin is added to distilled water and shaken, and then immersed in methanol and shaken, filtered, and the filtrate is taken and analyzed again to obtain purified schisandra chinensis B.

2. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: In S1, the feeding amount of the Shenqi Schisandrae Chinensis Capsule filling material is 180-220 g; and / or; The extraction pressure is 20-40Mpa; and / or; The extraction temperature is 30-50°C; and / or; The extraction time is 1-3h; and / or; CO2 flow rate 8-12kg / h.

3. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: In S2 and S3, the analysis process is divided into two stages. The first stage analysis pressure is 5-10Mpa, and the first stage analysis temperature is 35-50°C; the second stage analysis pressure is 4-8MPa, and the second stage analysis temperature is 35-45°C.

4. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: The specific steps of S3 are: Soak the AB-8 resin in 2 volumes of ethanol solvent for 24 hours, then filter and wash with ethanol until there is no turbidity, wash the AB-8 resin with distilled water until there is no ethanol, and soak it in distilled water for later use; The moisture on the surface of the AB-8 resin is absorbed dry, and then 1-2g of the dry AB-8 resin is added to 40-60ml of schisandra B extract, and the mixture is shaken at 20-30°C for 24h at a shaking speed of 50-70r / min. The mixture is then filtered, and the filtered AB-8 resin is added to 40-60ml of distilled water, and the mixture is shaken at 20-30°C for 1-3h. The mixture is then soaked in methanol, shaken at 20-30°C for 24h, filtered, and the filtrate is taken. The filtrate is analyzed again, and the analysis process is divided into two stages. The first stage analysis pressure is 5-10Mpa, and the first stage analysis temperature is 35-50°C; the second stage analysis pressure is 4-8MPa, and the second stage analysis temperature is 35-45°C, to obtain purified schisandra B.

5. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: The steps of detecting the schisandrin B content of the purified schisandrin B are as follows: First, add chromatographic methanol to 8-12 mg of purified schisandrin B, oscillate ultrasonically for 25-35 min, transfer quantitatively to a 10 ml volumetric flask, dilute to scale with methanol, shake well, filter through a 0.45 μm microporous membrane, and perform HPLC analysis; Chromatographic conditions of HPLC: Chromatographic column: Symmetry-C 18 Chromatographic column (4.6 mm × 180 mm, 5 μm); Mobile phase: methanol-water (70:30); Column temperature: 20°C; Injection volume: 10 μL; Detection wavelength: 254nm; Flow rate: 1.0 mL / min; Finally, the schisandrin B content of the purified schisandrin B was obtained using the schisandrin B standard curve.

6. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: In S1, the operation of removing the shell of Shenqi Schisandrae Chinensis Capsule is performed by an automatic shelling machine; The automatic shelling machine comprises a conveying plate (1), a shelling assembly (2) and a collecting assembly (3); the conveying plate (1) is used to transfer the ginseng, astragalus and schisandra capsules from the rotating vibration plate to the shelling assembly (2); the shelling assembly (2) is used to remove the shells of the ginseng, astragalus and schisandra capsules; and the collecting assembly (3) is used to separate and store the shells of the ginseng, astragalus and schisandra capsules and the fillings of the ginseng, astragalus and schisandra capsules; The conveying plate (1) is gradually inclined downward from the rotating vibration disk toward the collecting assembly (3), and a baffle (11) for limiting the movement of the ginseng, astragalus and schisandra capsule is provided at one end of the conveying plate (1) away from the rotating vibration disk, and a slide groove (12) is provided on the conveying plate (1), one end of the ginseng, astragalus and schisandra capsule passes through the slide groove (12), and the other end of the ginseng, astragalus and schisandra capsule is mounted on the conveying plate (1); The shelling assembly (2) comprises a base (21) rotatably connected to the conveying plate (1), a clamping jaw (22) slidably connected to the base (21), and a driving member (23) arranged on the base (21); the driving member (23) drives the clamping jaw (22) to move, and the clamping jaw (22) clamps one end of the ginseng, astragalus and schisandra capsule passing through the slide groove (12); the driving member (23) drives the base (21) and the clamping jaw (22) to rotate, and the clamping jaw (22) cooperates with the conveying plate (1) to shell the ginseng, astragalus and schisandra capsule.

7. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 6, characterized in that: The driving member (23) comprises a driving cylinder (231), a driving rack (232) fixedly connected to the output end of the driving cylinder (231), a driving gear (233) fixedly connected to the end of the conveying plate (1), and a slide plate (234) fixedly connected to the side wall of the driving rack (232); the driving rack (232) is slidably connected to the base (21) via the slide plate (234); a compression spring (235) is provided on one side of the slide plate (234); an end of the compression spring (235) away from the slide plate (234) is connected to the clamping claw (22); The driving rack (232) drives the clamping jaw (22) to move via the slide plate (234), and after the clamping jaw (22) clamps the Shenqi Schisandrae Chinensis Capsule, the driving rack (232) and the driving gear (233) are meshed with each other, and the slide plate (234) still has room for movement, and the movement of the driving rack (232) drives the base (21) to rotate.

8. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 7, characterized in that: A limiting shaft (236) is provided at both ends of the clamping jaw (22), and the compression spring (235) and the slide plate (234) are sequentially passed through the end of the limiting shaft (236) away from the clamping jaw (22); a limiting nut (237) is provided at the end of the limiting shaft (236) away from the clamping jaw (22), and the inner wall of the limiting nut (237) abuts against the outer wall of the slide plate (234).

9. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 6, characterized in that: The collecting assembly (3) comprises a collecting box (31) and a filter plate (32); the collecting box (31) is placed directly below the conveying plate (1) and the shelling assembly (2); the filter plate (32) is mounted in the collecting box (31); the filter plate (32) is arranged at an angle; the filter plate (32) is used to collect the outer shell of the ginseng, astragalus and schisandra capsule; and the collecting box (31) is used to collect the filling of the ginseng, astragalus and schisandra capsule.

10. The extraction process of Schisandra chinensis in Shenqi Schisandra chinensis capsule according to claim 1, characterized in that: The extraction process of schisandra chinensis in ginseng, astragalus and schisandra chinensis capsules is also used for extracting schisandra chinensis ester A, ...calycosin-containing glucoside and spinosin in ginseng, astragalus and schisandra chinensis capsules.

Images