CN113634011B

CN113634011B - Production integrated system of composite extraction composition of red pine and red plum, composite extraction composition of red pine and red plum and preparation method of composite extraction composition

Info

Publication number: CN113634011B
Application number: CN202110972305.9A
Authority: CN
Inventors: 曹华; 陈贤
Original assignee: Ganeng Biotechnology Shanghai Co ltd
Current assignee: Ganeng Biotechnology Shanghai Co ltd
Priority date: 2021-08-24
Filing date: 2021-08-24
Publication date: 2022-03-08
Anticipated expiration: 2041-08-24
Also published as: CN113634011A

Abstract

The application relates to the technical field of daily chemicals, and particularly discloses a production integrated system of a composite refined extract composition of a red plum, the composite refined extract composition of the red plum and a preparation method of the composite refined extract composition. The production integrated system comprises an extraction tank, a liquid storage tank and a heat exchanger, wherein the extraction tank is an integrated under-pressure extraction tank for extraction and separation integration of alkaloid active ingredients; the circulation that the convection current was drawed, was filtered and adsorbs to go on in step through the area is pressed and is drawed, solves the compound essence of pine red plum and prepares inefficiency with traditional technology for the composition, and the active matter heats the oxidation in solution for a long time, and the alcohol solvent remains the amazing of skin and the extraction process medicinal material active ingredient and remains big drawback.

Description

Production integrated system of composite extraction composition of red pine and red plum, composite extraction composition of red pine and red plum and preparation method of composite extraction composition

Technical Field

The invention relates to the technical field of daily chemicals, in particular to a production integrated system of a composite refined extract composition of a red plum, the composite refined extract composition of the red plum, a preparation method and application.

Background

With the wide use of cosmetics and the increasing severity of environmental pollution, the skin of modern people is more and more sensitive, which is mainly manifested by pruritus, dryness, dandruff, redness, swelling, inflammation and the like, the medical treatment mode is to use products such as antibiotics, hormones and the like for skin treatment, but the products such as antibiotics, hormones and the like cannot be used for a long time due to the particularity of the products, so that daily care products with the function of relieving the skin sensitivity phenomenon become an important choice for consumers. Daily care products have strict regulation requirements, and mainly used soothing components are mainly made of natural plants or traditional Chinese medicine raw materials, but at present, the raw materials mainly have better performance on instant itching relieving, slight anti-inflammation and barrier repair, and the components with good red removing and swelling reducing effects are rare, so that the development of the components has practical market demands.

The preparation of plant raw materials in the field of daily chemicals has the difficulty of traditional plant extraction, and the difficulty is also a special pain point in the use process of daily chemicals. The traditional plant extraction has many defects, such as low extraction efficiency, long process flow, more impurities, easily oxidized active ingredients, large adsorption residue of medicinal materials and the like; when the plant extract components are used in the daily chemical field, the plant extract components are indiscriminately used for long-term external use, and if the traditional extraction and refining method is adopted, for example, ethanol, methanol, petroleum ether and the like are used as solvents, part of human-specific allergy can be caused due to solvent residues, and new stimulus can be generated due to oxidation of the plant components in the extraction process to cause allergy to people who use the plant extract components. The extraction efficiency can be better improved and the dissolution of impurities can be reduced by the extraction technology under pressure.

At present, the extraction under pressure of the related technology is realized by pumping a solvent into a closed tank body, and the extraction under pressure of the related technology generally adopts intermittent static extraction, and the osmotic force of the solvent to medicinal material cells is increased by increasing the pressure in the tank body, so that the aim of enhancing the extraction efficiency of effective components is fulfilled.

However, the main effective component of the formula is a alkaloid substance, the solubility of the alkaloid substance in water is low, and the alkaloid substance is generally extracted by using a methanol or ethanol solution; in the field of daily chemicals, in order to avoid the stimulation of methanol or ethanol residue on skin, propylene glycol or 1, 3-butanediol solution is also selected as an extraction solvent, but the two solvents have poor solubility and are very difficult to filter; and traditional static area is pressed and is extracted and cause the medicinal material easily to pile up, has also influenced the extraction efficiency of arrangement.

It is therefore desirable to provide a method for extracting alkaloid active ingredients with high extraction yield and without skin irritation.

Disclosure of Invention

In order to improve the extraction rate and reduce the stimulation of alcohol solvent residue on skin, the application provides a production integrated system of a composite refined extract composition of the red plum, the composite refined extract composition of the red plum, a preparation method and application.

In a first aspect, the present application provides an integrated system for producing a composite refined extract composition of red plum of pine, which adopts the following technical scheme:

a production integrated system of a composite refined extract composition of a red plum of pine comprises an extraction tank, a liquid storage tank and a heat exchanger; the extraction tank is an integrated under-pressure extraction tank for extracting and separating alkaloid active ingredients;

a washing liquid inlet pipeline is arranged at the top of the extraction tank, a powder-water suspension inlet pipeline, a medicine residue outlet pipeline and an absorption raffinate backflow inlet pipeline are arranged on the side wall of the extraction tank, an absorption raffinate outlet and a washing liquid outlet pipeline are arranged at the bottom of the extraction tank, and a valve F8 is arranged on the washing liquid outlet pipeline;

a distributor and a ceramic membrane tube are arranged in the extraction tank, and the end part of the distributor close to the side wall of the extraction tank is connected with an adsorption residual liquid reflux inlet pipeline; the ceramic membrane tube is filled with resin, the end part of the ceramic membrane tube close to the adsorption residual liquid outlet is in threaded connection with a screw cap, a sintering plate is arranged in the screw cap, and the sintering plate is abutted against the bottom of the ceramic membrane tube;

a liquid inlet pipeline of the liquid storage tank is connected with an adsorption residual liquid outlet through a valve F9; a liquid supplementing pipeline is arranged at the top of the liquid storage tank, an outlet at the bottom of the liquid storage tank is connected with a heat exchange inlet pipeline of the heat exchanger through a valve F12 and a delivery pump, and the delivery pump is provided with a control valve F13 in parallel through a delivery pipeline; the control valve F13 is in electric signal connection with a pressure detection meter on the extraction tank;

and a heat exchange outlet pipeline of the heat exchanger is connected with an adsorption residual liquid reflux inlet pipeline.

By adopting the technical scheme, the internal diffusion process of extraction is promoted by extraction under pressure, and the extraction efficiency is enhanced; through the circulating extraction which is synchronously carried out by the pressurized convection extraction, the filtration and the adsorption, the gradient distribution of the concentration difference outside the medicinal material cells can be effectively broken, meanwhile, as the effective components (namely the alkaloids substances) are continuously adsorbed by the resin in the ceramic membrane tube, the adsorption residual liquid continuously flows back into the extraction tank again and continuously keeps a larger concentration difference with the medicinal material cells, so that the extraction can be continuously carried out, namely, the alcohol-soluble components can be effectively extracted by only using water as an extraction solvent, and the problem that the effective components are oxidized to reduce the extraction rate by transferring the effective components in time is solved; simultaneously, the stimulation of solvent residues formed by using solvents such as methanol or ethanol and the like to the skin is avoided from the source; in addition, the adsorption residual liquid is heated by the heat exchanger and then flows back to the extraction tank in two directions, so that the medicinal materials in the extraction tank can be in a suspended state, the accumulation of the medicinal materials is reduced, and the contact area between the medicinal materials and the adsorption residual liquid is increased; meanwhile, the permeation of the solvent (namely the adsorption residual liquid) to the medicinal materials can be effectively accelerated by increasing the pressure in the extraction tank, the extraction process of the effective components in the medicinal materials is further accelerated, and the extraction efficiency and the extraction rate are improved.

Preferably, an upper distributor and a lower distributor are arranged in the extraction tank, and an upper adsorption residual liquid reflux inlet pipeline and a lower adsorption residual liquid reflux inlet pipeline are arranged on the side wall of the extraction tank; a first return pipe 221 and a second return pipe 222 are connected in parallel on a heat exchange outlet pipeline of the heat exchanger, the first return pipe 221 is connected with the upper distributor through an upper adsorption residual liquid reflux inlet pipeline through a valve F3, the second return pipe 222 is connected with the lower distributor through a lower adsorption residual liquid reflux inlet pipeline through a valve F4, and a plurality of ceramic membrane tubes are vertically and uniformly distributed in a cavity of the extraction tank between the upper distributor and the lower distributor.

By adopting the technical scheme, the suspension of the medicinal powder-water is placed in the cavity between the upper distributor and the lower distributor (namely the upper distributor and the lower distributor), so that the medicinal materials are in a suspension state, the accumulation of the medicinal materials can be effectively reduced, the contact area between the medicinal materials and the adsorption residual liquid is increased, and the extraction and adsorption of effective components are facilitated. And secondly, the convection extraction of the medicinal materials by the upper distributor and the lower distributor can effectively break the gradient distribution of extracellular concentration difference, and meanwhile, as the effective components are continuously adsorbed by the resin, the concentration difference between the solvent (namely the adsorption residual liquid) and the medicinal materials is always kept close to the blank solvent in the extraction process, thereby being beneficial to improving the extraction efficiency and the extraction rate.

Preferably, the top of the extraction tank is also provided with an emptying pipe orifice for adjusting the pressure in the extraction tank, and the emptying pipe orifice is provided with a valve F7; and the top of the liquid storage tank is provided with an exhaust valve F14.

In a second aspect, the application provides a composite refined extract composition of red plum, which adopts the following technical scheme:

the composite refined extract composition of the pine and red plum is prepared from the following raw materials in parts by weight: 40-50 parts of pine red plum leaves, 25-35 parts of tetrandra root and 15-35 parts of lotus;

the preparation method comprises pretreating raw materials, extracting, removing residue with materials, and resolving to obtain a compound refined extract composition of Pinus koraiensis and flos Pruni mume; in the extraction process, a production integrated system of the composite refined extraction composition of the red plum is adopted for carrying out convection pressure extraction, and the composite refined extraction composition of the red plum is obtained.

By adopting the technical scheme, the pine red plum leaves and the tetrandra root all contain a large amount of alkaloid active ingredients, and after the integrated system is adopted for extraction, the extraction rate and the extraction efficiency can be improved, only water is used as an extraction solvent for effective extraction, and the stimulation of the alcohol solvent residue on the skin is also reduced from the source.

In a third aspect, the application provides a preparation method of a composite refined extract composition of a red plum, which adopts the following technical scheme:

a preparation method of a composite refined extract composition of a red plum of pine comprises the following steps:

1) pretreatment of raw materials:

pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding water, and mixing to obtain medicinal powder-water suspension;

distilling flos Nelumbinis with water to obtain distillate, adding alcohol solvent, refrigerating at 1-6 deg.C for 12-20 hr, and microfiltering to obtain resolution solution; the alcohol solvent is selected from 1, 3-butanediol or 1, 3-propanediol;

2) extraction: adding the powder-water suspension obtained in the step 1) into the production integrated system for multiple-time circulating extraction, and adsorbing the extracted active ingredients by resin in the ceramic membrane tube;

3) and (4) slag discharging with materials: discharging the dregs extracted in the step 2) out of the production integrated system, and discharging washing water after the ceramic membrane tube is cleaned by water;

4) and (3) analysis: adding the resolving liquid obtained in the step 1) to resolve the resin in the production integrated system to obtain a composite bougainvillea glabra refined extract composition; wherein the specific requirement of the analysis operation is to continuously introduce an analysis solution into the production integrated system and elute the active ingredients adsorbed on the resin, and the elution speed of the analysis solution is 0.3-0.6 mL/cm²And s, the elution ratio of the analysis solution is 3 to 4 times of the volume of the resin.

Through adopting above-mentioned technical scheme, adopt circulation extraction solvent (being water) to take the pressure to extract, filter and the adsorption operation effective component in the medicinal material to this constantly adsorbs the effective component in the medicinal material in the resin, thereby has effectively promoted the forward of the operation of extracting and has gone on, helps improving extraction efficiency. And then, after medicine dregs are discharged, adding the analytic solution into an extraction tank for elution operation, so that the alkaloid active ingredients adsorbed on the resin can be dissolved in an alcohol solvent (1, 3-butanediol or 1, 3-propanediol), and filtering to obtain the required pine and red plum composite refined extract composition, wherein the extraction efficiency and the extraction rate of the pine and red plum composite refined extract composition obtained after verification are high.

Preferably, in 1), the amount of water added into the coarse powder is 4-6 times of the weight of the coarse powder, the coarse powder and the water are uniformly mixed by a colloid mill after being added with the water, and the mixture enters an extraction tank from an inlet pipeline of the powder-water suspension.

By adopting the technical scheme, after the medicinal materials are crushed by the colloid mill and become medicinal powder, the contact area between the medicinal materials and the solvent is increased, and the extraction efficiency and the extraction rate of effective components in the medicinal materials are improved.

Preferably, in the step 1), the amount of water added into the lotus flowers is 8-10 times of the weight of the lotus flowers, and the extraction is stopped when the weight of the distillate reaches 4-6 times of the weight of the lotus flowers.

Preferably, in 2), water is added into the liquid storage tank, the amount of the added water is 6-10 times of the weight of the medicinal materials of the tetrandra root and the folium pruni pini, the extraction temperature is 50-70 ℃, the pressure is controlled to be 2-3 bar, and the extraction time is 1-1.5 h.

By adopting the technical scheme, the temperature and the pressure are increased, the penetration of the solvent to the medicinal materials can be accelerated, the extraction process is accelerated, and the dissolution of impurities is reduced.

Preferably, the resin is macroporous adsorption resin, the aperture of the ceramic membrane tube is 100-200 nm, and the aperture of the sintering plate is 5-10 μm.

By adopting the technical scheme, the pore diameters of the ceramic membrane tube and the sintering plate are limited, so that the balance between the interception of impurities and the water flow speed can be achieved, and the extraction efficiency and the extraction quality of effective components are improved while the higher extraction efficiency is kept.

In a fourth aspect, the application provides an application of the composite extract composition of the red plum in cosmetics, wherein the addition amount of the composite extract composition of the red plum in the cosmetics is 0.5-10% by weight.

In summary, the present application has the following beneficial effects:

1. the circulation that the convection current was drawed, was filtered and absorption was carried out in step through taking the area to this application is drawed, solves the compound essence of pine red plum and extracts traditional extraction process's of composition preparation inefficiency, and the active matter heats the oxidation in solution for a long time, and the alcohol solvent remains the amazing of skin and the big drawback of extraction process medicinal material active ingredient residue.

2. The preferred circulation extraction solvent (being water) that adopts of this application carries out the area to take pressure to extract, filters and the absorption operation in the active ingredient of medicinal material to this constantly adsorbs the active ingredient in the medicinal material in the resin, thereby has effectively promoted the forward of the operation of extracting and has gone on, helps improving extraction efficiency.

3. This application is preferred to adopt the colloid mill to smash the medicinal material and makes it become after the powder, has increased the area of contact between medicinal material and the solvent, helps improving the extraction efficiency and the extraction rate of active ingredient in the medicinal material.

Drawings

Fig. 1 is a schematic structural diagram of embodiment 1 of the present application.

Fig. 2 is a sectional view taken along line a-a of fig. 1.

Fig. 3 is a schematic structural view of an extraction tank of embodiment 1 of the present application in fig. 1.

Fig. 4 is an enlarged view of a direction a in fig. 3.

Description of reference numerals: 1. a liquid storage tank; 2. a cavity; 3. an extraction tank; 4. a wash liquor inlet conduit; 5. a powder-water suspension inlet pipe; 6. a dregs outlet pipeline; 7. the absorption raffinate flows back to the inlet pipeline; 71. an upper adsorption raffinate reflux inlet pipe; 72. the lower adsorption residual liquid flows back to the inlet pipeline; 8. an adsorption raffinate outlet line; 9. a wash liquor outlet conduit; 10. a ceramic membrane tube; 11. a distributor; 12. closing the plate; 13. opening a hole; 14. an externally threaded tube; 15. a screw cap; 16. sintering the plate; 17. a through hole; 18. a liquid inlet pipeline; 19. a heat exchanger; 20. A liquid outlet pipeline; 21. a delivery pump; 22. a return pipe; 221. a first return pipe; 222. a second return pipe; 23. A spray head; 25. a first sealing cover; 26. a second sealing cover; 27. a first emptying pipe; 28. a second emptying pipe; 29. A sight glass.

Detailed Description

The present application will be described in further detail with reference to the following drawings and examples.

The raw materials used in the examples of the present application are commercially available products unless otherwise specified.

The embodiment of the application discloses a production integrated system of a composite refined extract composition of a red plum. Referring to fig. 1, the integrated production system includes an extraction tank 3, a liquid storage tank 1 and a heat exchanger 19, and the three parts are communicated through a pipeline to form a circulating loop, and the application adopts deionized water (simply called water) as an extraction solvent and performs a process of extracting and separating alkaloid active ingredients in plants (or a composite bougainvillea glabra refined extract composition) through a circulating convection extraction mode.

Referring to fig. 1, a first sealing cover 25 is detachably connected to the top of the extraction tank 3, three upper cover lugs (not marked in the figure) are welded to the first sealing cover 25, three tank upper lugs (not marked in the figure) corresponding to the upper cover lugs are welded to the side wall of the extraction tank 3 close to the first sealing cover 25, and the upper cover lugs and the tank upper lugs can be locked by fastening bolts after being overlapped. The end part of the first sealing cover 25 far away from the extracting tank 3 is provided with a washing liquid inlet pipeline 4 and a first emptying pipe 27, the washing liquid inlet pipeline 4 is provided with a valve F5, and the first emptying pipe 27 is provided with a valve F6.

Referring to fig. 1, the side wall of the extraction tank 3 is provided with a powder-water suspension inlet pipe 5, a herb residue outlet pipe 6, a vent pipe two 28, two raffinate adsorption reflux inlet pipes 7 and two sight glasses 29. Wherein, the powder-water suspension inlet pipe 5 is positioned above the dregs outlet pipe 6. A valve F1 is arranged on the medicinal powder-water suspension inlet pipe 5, and a valve F2 is arranged on the medicinal dreg outlet pipe 6. The two raffinate return inlets 7 are sequentially divided into an upper raffinate return inlet 71 and a lower raffinate return inlet 72 from top to bottom, the upper raffinate return inlet 71 is provided with a valve F3, and the lower raffinate return inlet 72 is provided with a valve F4. The second vent 28 is installed on the side wall of the extraction tank 3 near and below the reflux inlet 71 of the upper adsorption raffinate, and a valve F7 is installed on the second vent 28. Two sight glasses 29 adopt transparent glass to make to fix at two relative lateral walls of extracting jar 3 through the ring flange, the operator can see through above-mentioned glass sight glass 29 and extract the interior liquid level height of jar 3, perhaps the suspended state of medicinal material, very convenient.

Referring to fig. 1, the bottom of the extracting tank 3 is detachably connected with a second sealing cover 26, the second sealing cover 26 and the first sealing cover 25 are arranged in an up-and-down corresponding manner, three lower cover engaging lugs are welded on the side wall of the second sealing cover 26, three tank lower engaging lugs corresponding to the lower cover engaging lugs are welded on the side wall of the extracting tank 3 close to the second sealing cover 26, and the lower cover engaging lugs and the tank lower engaging lugs can be locked by fastening bolts after being overlapped. An adsorption raffinate outlet pipe 8 and a washing liquid outlet pipe 9 are installed at the end of the second sealing cover 26 far away from the extraction tank 3, a valve F9 is installed on the adsorption raffinate outlet pipe 8, and a valve F8 is installed on the washing liquid outlet pipe 9.

Referring to fig. 2 and 3, a cavity 2 for holding powder-water suspension is formed inside the extraction tank 3, two sealing plates 12 are fixedly connected to the inner wall of the extraction tank 3 and spaced apart from each other, and the two sealing plates 12 are arranged in parallel along the height direction of the extraction tank 3 and divide the cavity 2 inside the extraction tank 3 into an upper region, a middle region and a lower region. Wherein the washing liquid inlet pipeline 4 and the first emptying pipe 27 are communicated with the cavity 2 in the upper area; the powder-water suspension inlet pipeline 5, the medicine residue outlet pipeline 6, the emptying pipe two 28 and two adsorption residual liquid reflux inlet pipelines 7 are communicated with the cavity 2 in the middle area; the raffinate outlet line 8 and the wash outlet line 9 communicate with the cavity 2 in the lower region.

Referring to fig. 2, the upper and lower seal plates 12 are formed with 9 openings 13 formed therein so as to penetrate the three regions. One of the openings 13 is located on the central axis of the extraction tank 3, and the other eight openings 13 are evenly distributed around the central axis and form an enclosure. Referring to fig. 2 and 3, in the present embodiment, in order to indicate the sealing plate 12 in different orientations, the sealing plate 12 adjacent to the raffinate outlet line 8 is referred to as a lower sealing plate, and the sealing plate 12 adjacent to the wash inlet line 4 is referred to as an upper sealing plate. Nine external threaded pipes 14 are integrally formed on the outer wall of the lower sealing plate, which is away from the ceramic membrane tube 10, the external threaded pipes 14 are arranged in one-to-one correspondence with the openings 13 on the lower sealing plate, and the upper and lower sealing plates 12 and the external threaded pipes 14 are made of 304 stainless steel metal materials in this embodiment.

Referring to fig. 3 and 4, one end of each external thread tube 14 extends into the inner wall of the opening 13 of the lower sealing plate and is abutted against the inner wall of the opening 13 of the lower sealing plate, a screw cap 15 is screwed on the end of the external thread tube 14 extending towards the direction of the washing liquid outlet pipeline 9, a cylindrical sintering plate 16 is arranged in the screw cap 15, the diameter of the sintering plate 16 is 5-10 μm, and the diameter of the sintering plate 16 is selected to be 6 ± 0.5 μm in the embodiment. A circular through hole 17 is formed in the center of the screw cap 15, the diameter of the through hole 17 is smaller than the diameter of the sintered plate 16, in this embodiment, the diameter of the through hole 17 is 4/5 of the diameter of the sintered plate 16, and both the inner wall of the external threaded pipe 14 and the annular rubber gasket on the screw cap 15 are abutted against the sintered plate 16.

Referring to fig. 3, a vertically arranged ceramic membrane tube 10 is inserted into two corresponding openings 13 at the upper and lower sides of two seal plates 12, the ceramic membrane tube 10 is cylindrical, a plurality of micropores are densely distributed on the wall of the ceramic membrane tube 10, and the pore diameter of each micropore is 100-200 nm. The ceramic membrane tube 10 is filled with resin, which is macroporous adsorption resin in this embodiment, and can be used for adsorbing active ingredients in the medicinal materials, so as to reduce the content of the active ingredients in the solvent and make the active ingredients close to a blank solvent (that is, the solvent in this embodiment is water, which is referred to as a solvent for short).

In order to form the instant adsorption of the resin to the effective components, the upper end of the ceramic membrane tube 10 is clamped on the upper closing plate; the lower end of the ceramic membrane tube 10 is clamped in the through hole 17 of the lower sealing plate, and the horizontal height of the lower end surface of the ceramic membrane tube 10 is slightly lower than that of the upper surface of the lower sealing plate. The lower end of the ceramic membrane tube 10 is inserted into the opening 13 of the lower sealing plate and is abutted against the external thread tube 14, and the resin in the ceramic membrane tube 10 is also directly contacted with the sintering plate 16. So that the analysis liquid can enter the ceramic membrane tube 10 from the upper area to analyze the resin and then flow out from the lower area after analysis; the inside that the extract can lean on pressure to get into ceramic membrane pipe 10 by ceramic membrane pipe 10 outside in the middle region, and then by the resin adsorption active ingredient after, the remaining liquid gets into the interior circulation of lower district and draws, accomplishes the synchronous integrated design who draws and adsorb to form the resin to the instant absorption of active ingredient, improved the adsorption efficiency of resin to active ingredient.

Referring to fig. 2 and 3, the upper and lower closing plates 12 are each provided with a distributor 11 on a side away from each other, the distributors 11 are located in the extraction cavity 2, and the two distributors 11 are arranged opposite to each other, and the distributors 11 are composed of an upper distributor and a lower distributor. Nine ceramic membrane tubes 10 are vertically and evenly distributed in the cavity 2 of the extraction tank 3 between the two distributors 11. The end part of the distributor 11 close to the side wall of the extraction tank 3 is connected with an adsorption residual liquid reflux inlet pipeline 7; meanwhile, the end of the distributor 11 far away from the adsorption raffinate reflux inlet pipeline 7 is provided with a spray head 23, and the spray head 23 is a common spray head in the embodiment. Eight spray heads 23 are uniformly distributed on the outer wall of the distributor 11, and each spray head 23 passes through the corresponding closing plate 12 and extends towards the ceramic membrane tube 10. The residual adsorption liquid (namely the solvent) can be sprayed into the middle area cavity 2 from the eight spray heads 23 at the moment, so that the residual adsorption liquid is reused, the reuse rate of the solvent is improved, convection extraction is realized, and the influence of accumulation of the medicinal materials on the extraction efficiency due to pressure extraction is avoided.

Referring to fig. 1, the liquid storage tank 1 is provided at the top thereof with a liquid inlet pipe 18 and an emptying valve F14, the liquid inlet pipe 18 is connected to a valve F9, and the liquid storage tank 1 can be used for storing the adsorption residual liquid. The bottom of the liquid storage tank 1 is provided with a liquid outlet pipeline 20, the liquid outlet pipeline 20 at the bottom of the liquid storage tank is provided with two branches, one branch is provided with a valve F11 which can be used for discharging the adsorption residual liquid in the liquid storage tank 1 out of a circulating system formed by the liquid storage tank 1 and the extraction tank 3; along the water flow direction on the other branch, a liquid outlet pipeline 20 at the bottom of the liquid storage tank is connected with a heat exchange inlet pipeline of the heat exchanger 19 through a valve F12 and a delivery pump 21, the delivery pump 21 is provided with a control valve F13 in parallel through a delivery pipeline, and the control valve F13 in the embodiment is selected as an electromagnetic valve; the control valve F13 is connected with the pressure detecting meter of the extracting tank 3 by electric signals, so that the operator can control the pressure in the extracting tank 3 by controlling the valve opening of the control valve F13, thereby achieving the function of controlling the pressure in the extracting tank 3. Furthermore, the heat exchange outlet line of the heat exchanger is connected to the raffinate reflux inlet line 7 via reflux line 22.

Referring to fig. 1, the return pipe 22 is composed of a first return pipe 221 and a second return pipe 222. A first return pipe 221 and a second return pipe 222 are connected in parallel on a heat exchange outlet pipeline of the heat exchanger 19, the first return pipe 221 is connected to the upper distributor through an upper adsorption residual liquid return inlet pipeline 71 through a valve F3, the second return pipe 222 is connected to the lower distributor through a lower adsorption residual liquid return inlet pipeline 72 through a valve F4, and the convection state is adjusted by adjusting the opening degrees of F3 and F4.

Referring to fig. 1, the operator locks the first and second sealing caps 25 and 26 and closes the valves F1, F2, F5, F6, F7, F8, F10, F11, and F14 at the same time, so as to seal the extracting tank 3. All valves in the embodiment of the application can adopt electromagnetic valves; meanwhile, the bypass control pressure is adjusted through a tank body pressure controller (not shown in the figure) and a control valve F13 on the extraction tank 3, the pressure difference inside and outside the medicinal material cell is kept, the quick extraction of the effective components in the medicinal material cell is facilitated, and the efficiency is improved.

Preparation example

Preparation example 1: a method for producing a resolving liquid comprising: distilling flos Nelumbinis with 10 times of water to obtain 5 times of distillate, adding 1, 3-butanediol at equal ratio, refrigerating at 4 deg.C for 12 hr, and passing through 0.2 μm membrane to obtain solution.

Preparation example 2: a method for producing a resolving liquid comprising: distilling flos Nelumbinis with 8 times of water to obtain 5 times of distillate, adding 1, 3-propylene glycol at equal ratio, refrigerating at 4 deg.C for 13 hr, and passing through 0.2 μm membrane to obtain solution.

Preparation example 3: a method for producing a resolving liquid comprising: distilling flos Nelumbinis with 9 times of water to obtain 5 times of distillate, adding 1, 3-butanediol at equal ratio, refrigerating at 4 deg.C for 14 hr, and passing through 0.2 μm membrane to obtain solution.

Examples

Example 1: a composite refined extract composition of a pine and red plum is prepared from the following raw materials in parts by weight (kg): 50kg of pine red plum leaves, 35kg of tetrandra root and 15kg of lotus flowers.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding 4 times of water, mixing with colloid mill, adding into extraction tank, adding 6 times of water into liquid storage tank, heating to 50 deg.C with heat exchanger, feeding into upper and lower distributors, filling the extraction tank, and regulating the relative opening of valve F3 and valve F4 to form convection extraction. Extracting at 3bar for 1.5h, discharging, cleaning, adding 3 times of the resolving solution of preparation example 1, and eluting at 0.3ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Example 2: a composite refined extract composition of a pine and red plum is prepared from the following raw materials in parts by weight (kg): 40kg of pine red plum leaves, 25kg of tetrandra root and 35kg of lotus flowers.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding 6 times of water, mixing with colloid mill, adding into extraction tank, adding 4 times of water into liquid storage tank, heating to 70 deg.C with heat exchanger, feeding into upper and lower distributors, filling the tank, and regulating the relative opening of valve F3 and valve F4 to form convection extraction. The extraction pressure is 2bar, the extraction time is 1h, discharging and cleaning are carried out after the extraction is finished, then 4 times of the eluent of the preparation example 2 is added for elution, and the elution speed is 0.6ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Example 3: a composite refined extract composition of a pine and red plum is prepared from the following raw materials in parts by weight (kg): 45kg of pine leaf and red plum leaf, 30kg of tetrandra root and 25kg of lotus flower.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding 5 times of water, mixing with colloid mill, adding into extraction tank, adding 5 times of water into liquid storage tank, heating to 60 deg.C with heat exchanger, feeding into upper and lower distributors, filling the tank, and regulating the relative opening of valve F3 and valve F4 to form convection extraction. Extracting at 2.5bar for 75min, washing, adding 3.5 times of the solution of preparation example 3, and eluting at 0.45ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Comparative example

Comparative example 1: the difference between the composite refined extract composition of the pine and the red plum in the embodiment 1 is that: the amount of the composition used varies.

The composite refined extract composition of the pine and red plum is prepared from the following raw materials in parts by weight (kg): 55kg of pine red plum leaves, 40kg of tetrandra root and 5kg of lotus flowers.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding 4 times of water, mixing with colloid mill, adding into extraction tank, adding 6 times of water into liquid storage tank, heating to 50 deg.C with heat exchanger, feeding into upper and lower distributors, filling the tank, and regulating the relative opening of valve F3 and valve F4 to form convection extraction. Extracting at 3bar for 1.5h, discharging, cleaning, adding 3 times of the resolving solution of preparation example 1, and eluting at 0.3ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Comparative example 2: the difference between the composite refined extract composition of the pine and the red plum in the embodiment 1 is that: the amount of the composition used varies.

The composite refined extract composition of the pine and red plum is prepared from the following raw materials in parts by weight (kg): 35kg of pine red plum leaves, 20kg of tetrandra root and 45kg of lotus flowers.

Comparative example 3: the difference between the composite refined extract composition of the red plum and the comparative example 2 is that: the difference of the preparation method is that the conventional stirring extraction is adopted.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, adding 10 times of water, stirring at 50 deg.C, and extractingTaking for 1.5h, filtering, and concentrating to obtain the following medicinal materials: the concentrated solution was adsorbed on a resin at a ratio of 2:1, and then 3 times the amount of the eluent of preparation example 1 was added thereto to elute at a rate of 0.3ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Comparative example 4: the difference between the composite refined extract composition of the red plum and the comparative example 2 is that: the difference of the preparation method is that the conventional extraction under pressure is adopted.

The preparation method comprises the following steps: pulverizing folium Pini and radix Stephaniae Tetrandrae into coarse powder, extracting with 10 times of water at 50 deg.C under pressure for 1.5 hr, filtering, and concentrating to obtain the following medicinal materials: the concentrated solution was adsorbed on a resin at a ratio of 2:1, and then 3 times the amount of the eluent of preparation example 1 was added thereto to elute at a rate of 0.3ml/cm²And s, obtaining the composite refined extract composition of the pine and red plum.

Data analysis

Test one: physical and chemical property detection test objects: the composite extract compositions of the red pine berries prepared in examples 1 to 3 were used as test samples 1 to 3, and the composite extract compositions of the red pine berries prepared in comparative examples 1 to 4 were used as control samples 1 to 4.

The test method comprises the following steps:

(one) stability test (d): the sample to be tested has the longest time of no color change and no precipitation under the conditions of 4 ℃, 48 ℃ and normal temperature illumination.

(II) an alkaloid detection method: according to the principle that alkaloids and hydrogen ions generate cations in a medium with certain pH, some acid dyes can be dissociated into anions under the condition and are quantitatively combined with the cations to form colored complexes, and the colored complexes can be quantitatively extracted by an organic solvent, tetrandrine is used as a standard substance and bromothymol blue is quantitatively developed at 414nm by an ultraviolet spectrophotometer under the condition that the pH is 7.60, and alkaloids in medicinal materials can be detected under the condition that the alkaloids can be developed with the bromothymol blue, so that the content of the relative total alkaloids can be obtained.

The alkaloid extraction rate is alkaloid extraction mass ÷ theoretical mass of alkaloid in medicinal materials multiplied by 100%;

the residue alkaloid yield of the medicine residue is (the residue alkaloid mass in the medicine residue plus the extracted liquid mass of the medicine residue multiplied by the alkaloid content of the extracting solution) ÷ the theoretical mass of the alkaloid in the medicinal materials multiplied by 100%;

wherein, the theoretical mass of the alkaloid in the medicinal materials is as follows: pulverizing the raw materials into 80 mesh powder, adding 30 times of 50% ethanol solution, ultrasonic extracting for 30min, and filtering; and repeating the above extraction for 2 times on filter residues, combining three extracting solutions, and testing the content of the alkaloid.

The residual quality of alkaloid in the dregs of a decoction is as follows: filtering the medicinal materials until no water drops, adding 30 times of 50% ethanol solution, ultrasonic extracting for 30min, and filtering; and repeating the above extraction for 2 times on filter residues, combining three extracting solutions, and testing the content of the alkaloid.

(III) DPPH clearance: the diphenylpicrylphenylhydrazine free radical (2, 2-diphenyl-1-piperidinylhydrazyl, DPPH) is a stable organic free radical, and the stability of the diphenylpicrylphenylhydrazine free radical mainly comes from resonance stabilization and steric hindrance of 3 benzene rings, so that unpaired electrons clamped on nitrogen atoms in the diphenylpicrylphenylhydrazine free radical cannot play the corresponding electron pairing role. The degree of oxidation resistance can be shown by measuring the ability of a substance to scavenge DPPH.radical.

Pipette 90. mu.l of 2X 10^-4Adding mol/L DPPH into a 96-well plate, and respectively adding 10 mu L of rutin standard substances or drugs to be detected with different concentrations, wherein three concentrations are arranged in parallel; a control group containing 90. mu.l of DPPH solution and 10. mu.l of ethanol solution and a blank group containing anhydrous ethanol were set. Reacting at room temperature for 30min, and rapidly measuring absorbance at 517nm with MD microplate reader.

DPPH radical clearance (%) [1-Ai/Ao ] × 100%;

a0- (blank control withholding control group absorbance);

ai- (drug group withholding control group absorbance);

wherein the DPPH radical scavenging ability at least 3 concentrations is measured and IC is calculated₅₀I.e. the concentration of the sample solution at which the inhibition of DPPH is 50%, IC₅₀The smaller the oxidation resistance, the stronger the oxidation resistance.

TABLE 1

By combining examples 1-3 and comparative examples 1-4 and table 1, it can be seen that the alkaloid extraction rate of examples 1-3 is significantly higher than that of comparative examples 1-4, the residue rate of examples 1-3 is significantly lower than that of comparative examples 1-4, and the obtained products of examples 1-3 are light in color (less in impurities) and far superior in stability to the obtained products of comparative examples 1-4.

As can be seen by combining examples 1-3, comparative examples 1-2 and Table 1, the products obtained in examples 1-3 have better DPPH clearance than comparative examples 1-2, indicating that the specific proportions of the formulations of examples 1-3 according to the present invention are beneficial for improving antioxidant efficacy.

As can be seen by combining examples 1-3 and comparative examples 3-4 with Table 1, the DPPH clearance of the products obtained in examples 1-3 is significantly better than that of comparative examples 3-4, which indicates that the antioxidant effect of the products obtained by the preparation method of examples 1-3 is significantly better than that of comparative examples 3-4, which may be related to both the high extraction rate and the antioxidant protection of the active ingredients during the process.

And (2) test II: efficacy test results test subjects: the composite extract compositions of the red pine berries prepared in examples 1 to 3 were used as test samples 1 to 3, and the composite extract compositions of the red pine berries prepared in comparative examples 1 to 4 were used as control samples 1 to 4.

The test method comprises the following steps:

1. capsaicin stimulation model

Capsaicin can activate a mouse receptor (TRPV1) to induce peripheral pain, a chemical stimulation induced mouse pain model is established by injecting capsaicin to the sole of a mouse, the analgesic effect of a sample to be tested is further investigated, TRPV1 is also a heat-sensitive channel, and the inhibition of TRPV1 can effectively remove red.

Experimental materials: capsaicin, absolute ethyl alcohol, deionized water, a 50ul sample injector, an electronic balance, Kunming mice (20 +/-2 g) and indometacin liniment.

The experimental method comprises the following steps: taking 90 healthy Kunming mice, each half of the mice, carrying out adaptive feeding, then randomly dividing the mice into 9 groups, each group comprising 10 mice, namely, a model control group, a positive drug group (indometacin liniment), a 5% dose group of example 1, a 5% dose group of example 2, a 5% dose group of example 3, a 5% dose group of comparative example 1, a 5% dose group of comparative example 2, a 5% dose group of comparative example 3 and a 5% dose group of comparative example 4. The hair on the back of the mouse is cut off by a razor 24h before the experiment, and then the hair removal cream is used for hair removal, and the area is 3 x 3cm². The back of each group of mice is respectively dosed with 0.2ml/d, the administration is continuously carried out for 7d, capsaicin (16mg/100 ml; 20ul) is injected into the right foot sole after the last administration for 1h, the times and the duration of right foot licking of the mice within 5min are observed and recorded, the duration of right foot licking is taken as an index, the groups are subjected to difference significance analysis, the inhibition rate is calculated, and the treatment effect of the drug to be tested on the pain model is evaluated, which is shown in the data of table 2.

2. Haemolysis test of red blood cells

The degree of damage to the cell membrane was evaluated by measuring the amount of hemoglobin leaking from the red blood cells, and the greater the amount of hemoglobin leaking, the greater the damage. The experimental model group was stimulated with 0.1% SDS, and the inhibitory effect of each group of active substances on the stimulation of SDS hemolysis was tested.

RBC hemolysis assay: the collected blood sample (sheep blood) was dispensed into a 10mL polyethylene sterile centrifuge tube and centrifuged at 1500Xg for 15min at room temperature. The supernatant was carefully aspirated with a disposable syringe and discarded. RBCs in the centrifuge tubes were shuffled 4 times with PBS buffer equal to whole blood under the same conditions. The process removes a large amount of white blood cells, plasma and yellow debris. Adding a proper amount of glucose into RBC in the centrifugal tube to make the final concentration of the glucose be 10mmol/L, and sealing and storing. And storing in a refrigerator at 4 ℃ for later use. Before the experiment, RBC was allowed to stand, the temperature was allowed to stabilize at room temperature, and PBS was used to adjust the final concentration of RBC to 8X 10⁹one/mL is ready for use, and the whole process is operated aseptically.

Experimental group (sample + SDS): respectively adding 500 μ L of test sample into 1.5mL EP tube, adding 210 μ L of PBS, mixing, adding 250 μ L of RBC, shaking and incubating for 30min, taking out, adding 40 μ L of SDS solution with mass concentration of 1.0mg/mL, and shaking and incubating for 10 min.

Model group: to a 1.5mL EP tube, 710. mu.L of PBS and then 250. mu.L of RBC were added, followed by shaking and incubation for 30min, and then the mixture was taken out, 40. mu.L of SDS solution with a mass concentration of 1.0mg/mL was added, and shaking and incubation for 10 min. After centrifugation at a centrifugation speed of 11180Xg for 1min, 3 groups of reactions were terminated, and the supernatant was measured for absorbance at a wavelength of 530nm in a 1cm cuvette, and the hemolysis inhibition rate was calculated according to the following formula and registered in Table 3.

Hemolysis inhibition rate ═ (model group absorbance-experiment group absorbance) ÷ model group absorbance × 100%; experimental results and discussion

TABLE 2

Note: p <0.01, as compared to model group.

From the experimental results of table 2, it can be seen that the extract of rubus parvifolius of examples 1-3 of the present application is comparable to the positive control in inhibiting trpv1 at a dose of 5%, and is significantly superior to the effect of comparative examples 1-4.

TABLE 3

Group number	Group of	Hemolysis inhibition ratio (%)
			1	Model control group	——
2	5% dose group of example 1	34.66
			3	Example 2 5% dose group	32.75
4	5% dose group of example 3	35.12
			5	5% dose group of comparative example 1	20.87
6	5% dose group of comparative example 2	19.05
			7	5% dose group of comparative example 3	12.55
8	5% dose group of comparative example 4	11.46

As can be seen from the experimental results, the refined extract of the prunella pinicola red obtained in examples 1-3 of the present application has a significant inhibitory effect on the stimulation of hemolysis caused by SDS, and is significantly superior to the effects of comparative examples 1-4.

Application example

Application example 1: the raw material composition and the dosage of the shower gel containing the pine and the red plum are shown in a table 4.

TABLE 4

The preparation method of the rose mallow shower gel comprises the following steps: 1. adding deionized water into the main pot, heating, adding ALS28 and N70, stirring at 80 ℃ until the raw materials are dissolved and transparent, adding the residual raw materials of the phase A, and stirring until the raw materials are completely dissolved and cooled; 2. cooling to 60 deg.C, adding B phase raw material, and stirring at low speed until completely dissolved and dispersed; and 3, cooling to 45 ℃, sequentially adding the C-phase raw materials, and slowly stirring until the C-phase raw materials are completely dissolved.

Application example 2: a Pinghong plum emulsion has the raw materials and dosage shown in Table 5.

TABLE 5

The preparation method of the pine and red plum emulsion comprises the following steps: 1. adding deionized water into the main pot, stirring and heating, sequentially adding phase A raw materials, heating to 85 deg.C, and keeping the temperature for 20 min; 2. heating premix 2 to 80 ℃ for dissolving and transparency, adding EMT10 into premix 2, stirring until the dispersion is uniform, starting a main pot for homogenization, sequentially adding the B-phase raw materials into the main pot, stirring in vacuum for homogenization for 5-10min until the state is uniform, and cooling; 3. cooling to 45 deg.C, adding the C phase raw materials, stirring to dissolve uniformly to obtain the final product.

Application example 3: a Pinghong Mei shui (pine and Red plum water) has the raw material composition and dosage shown in Table 6.

TABLE 6

The preparation method of the pine red plum water comprises the following steps: 1. adding deionized water into the main pot, sequentially adding phase A raw materials under stirring, heating to 85 deg.C, and maintaining the temperature for 20 min; 2. cooling to 45 deg.C, adding B phase raw material, stirring until it is dissolved uniformly.

Application example 4: the raw material composition and the dosage of the pine and red plum essence are shown in table 7.

TABLE 7

The preparation method of the pine and red plum essence comprises the following steps: 1. adding deionized water into the main pot, sequentially adding phase A raw materials under stirring, heating to 85 deg.C, and maintaining the temperature for 20 min; 2. cooling to 45 deg.C, adding B phase raw material, stirring until it is dissolved uniformly.

The specific embodiments are merely illustrative of the present application and are not restrictive of the present application, and those skilled in the art can make modifications of the embodiments as required without any inventive contribution thereto after reading the present specification, but only protected by the patent laws within the scope of the claims of the present application.

Claims

1. The preparation method of the composite refined extract composition of the red plum is characterized by comprising the following steps:

1) pretreatment of raw materials:

2) extraction: adding the suspension of the powder and water obtained in the step 1) into a production integrated system for multiple times of circulating extraction, and adsorbing the extracted active ingredients by resin in a ceramic membrane tube (10);

3) and (4) slag discharging with materials: discharging the dregs extracted in the step 2) out of the production integrated system, and discharging washing water after the ceramic membrane tube (10) is cleaned by water;

4) and (3) analysis: adding the resolving liquid obtained in the step 1) to resolve the resin in the production integrated system to obtain a composite bougainvillea glabra refined extract composition;

wherein the specific requirement of the analysis operation is to continuously introduce an analysis solution into the production integrated system and elute the active ingredients adsorbed on the resin, and the elution speed of the analysis solution is 0.3-0.6 mL/cm²S, the elution times of the analytic solution are 3-4 times of the volume of the resin;

the production integrated system comprises an extraction tank (3), a liquid storage tank (1) and a heat exchanger (19); the extraction tank (3) is an integrated pressure extraction tank for extracting and separating alkaloid active ingredients;

a washing liquid inlet pipeline (4) is arranged at the top of the extraction tank (3), a powder-water suspension inlet pipeline (5), a medicine residue outlet pipeline (6) and an adsorption residual liquid reflux inlet pipeline (7) are arranged on the side wall of the extraction tank (3), an adsorption residual liquid outlet and a washing liquid outlet pipeline (9) are arranged at the bottom of the extraction tank (3), and a valve F8 is arranged on the washing liquid outlet pipeline (9);

the inner wall of the extraction tank (3) is fixedly connected with two sealing plates (12) arranged in a partition way, and a cavity (2) in the extraction tank (3) is divided into an upper area, a middle area and a lower area, wherein the washing liquid inlet pipeline (4) is communicated with the cavity (2) in the upper area; the powder-water suspension inlet pipeline (5), the medicine residue outlet pipeline (6) and two adsorption residual liquid reflux inlet pipelines (7) are communicated with the cavity (2) in the middle area; an outlet pipeline (8) for the adsorption residual liquid and an outlet pipeline (9) for the washing liquid are communicated with the cavity (2) in the lower area;

the extraction device is characterized in that 9 oppositely-arranged open holes (13) are formed in the upper sealing plate (12) and the lower sealing plate (12), a vertically-arranged ceramic membrane tube (10) is inserted into the two vertically-corresponding open holes (13) of the two sealing plates (12), a distributor (11) is arranged in the extraction tank (3), the distributor (11) is composed of an upper distributor and a lower distributor, a plurality of ceramic membrane tubes (10) are vertically and uniformly distributed in a cavity (2) of the extraction tank (3) between the upper distributor and the lower distributor, and the end part, close to the side wall of the extraction tank (3), of the distributor (11) is connected with a raffinate return inlet pipeline (7); the ceramic membrane tube (10) is filled with resin, the end part of the ceramic membrane tube (10) close to the adsorption raffinate outlet is connected with a screw cap (15) in a threaded manner, a sintering plate (16) is arranged in the screw cap (15), and the sintering plate (16) is abutted against the bottom of the ceramic membrane tube (10);

a liquid inlet pipeline (18) of the liquid storage tank (1) is connected with an outlet of the adsorption residual liquid through a valve F9; a liquid supplementing pipeline is arranged at the top of the liquid storage tank (1), an outlet at the bottom of the liquid storage tank (1) is connected with a heat exchange inlet pipeline of the heat exchanger (19) through a valve F12 and a delivery pump (21), the delivery pump (21) is provided with a control valve F13 in parallel through a delivery pipeline, and the control valve F13 is in electrical signal connection with a pressure detection meter on the extraction tank (3);

and a heat exchange outlet pipeline of the heat exchanger (19) is connected with an adsorption raffinate reflux inlet pipeline (7).

2. The method for preparing a composite refined extract composition of pine and red plum as claimed in claim 1, wherein the side wall of the extraction tank (3) is provided with an upper raffinate reflux inlet pipe (71) and a lower raffinate reflux inlet pipe (72); a first return pipe (221) and a second return pipe (222) are connected in parallel on a heat exchange outlet pipeline of the heat exchanger (19), the first return pipe (221) is connected to the upper distributor through an upper adsorption residual liquid return inlet pipeline (71) through a valve F3, and the second return pipe (222) is connected to the lower distributor through a lower adsorption residual liquid return inlet pipeline (72) through a valve F4.

3. The method for preparing the composite refined extract composition of the pine and red plum as claimed in claim 1, wherein the top of the extraction tank (3) is further provided with a vent pipe for adjusting the pressure in the extraction tank (3), and the vent pipe is provided with a valve F7; an exhaust valve F14 is arranged at the top of the liquid storage tank (1).

4. The method for preparing the composite refined extract composition of the pine and red plum as claimed in claim 1, wherein in 1), the amount of water added into the coarse powder is 4-6 times of the weight of the coarse powder, the coarse powder is mixed by a colloid mill after being added with water, and the mixture enters the extraction tank (3) from an inlet pipeline (5) of powder-water suspension.

5. The preparation method of the composite refined extract composition of the pine and red plum as claimed in claim 1, wherein in 1), the amount of water added into the lotus flowers is 8-10 times of the weight of the lotus flowers, and the distillation is stopped when the weight of the distillate reaches 4-6 times of the weight of the lotus flowers.

6. The preparation method of the composite refined extract composition of the Korean plum as claimed in claim 1, wherein in 2), water is added into the liquid storage tank (1), the amount of the added water is 6-10 times of the weight of the medicinal materials of the Japanese stephania root and the Korean plum leaf, the extraction temperature is 50-70 ℃, the pressure is controlled at 2-3 bar, and the extraction time is 1-1.5 h.

7. The method for preparing the composite refined extract composition of the red plum of claim 4, wherein the resin is a macroporous adsorbent resin, the pore diameter of the ceramic membrane tube (10) is 100-200 nm, and the pore diameter of the sintering plate (16) is 5-10 μm.

8. The composite refined extract composition of the pine and red plum is characterized by being prepared from the following raw materials in parts by weight: 40-50 parts of pine red plum leaves, 25-35 parts of tetrandra root and 15-35 parts of lotus; the preparation method of the composite refined extract composition of the red plum of the pine according to any one of claims 1 to 7, wherein the composite refined extract composition of the red plum of the pine is obtained after raw material pretreatment, extraction, material-carrying slag tapping and resolution; and in the extraction process, the production integrated system is adopted for convection extraction.

9. The use of the composite extract composition of red pine and plum of claim 8, wherein the amount of the composite extract composition of red pine and plum added to cosmetics is 0.5-10% by weight.