CN113634011A - Production integrated system of red pruned pine and red pruned refined extract composition, red pruned pine and red pruned refined extract composition and preparation method thereof - Google Patents

Production integrated system of red pruned pine and red pruned refined extract composition, red pruned pine and red pruned refined extract composition and preparation method thereof Download PDF

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CN113634011A
CN113634011A CN202110972305.9A CN202110972305A CN113634011A CN 113634011 A CN113634011 A CN 113634011A CN 202110972305 A CN202110972305 A CN 202110972305A CN 113634011 A CN113634011 A CN 113634011A
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red
extraction
prune
water
extraction tank
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CN113634011B (en
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曹华
陈贤
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Ganeng Biotechnology Shanghai Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0215Solid material in other stationary receptacles
    • B01D11/0219Fixed bed of solid material
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The application relates to the technical field of daily chemicals, and particularly discloses a production integration system of a red prunella pini refined extract composition, the red prunella pini refined extract composition and a preparation method thereof. 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; this application draws through the circulation that the convection current of taking the area is pressed and is drawed, filter and adsorb and go on in step, solves the red plum of pine and mends red essence to extract the composition and prepare inefficiency with traditional technology, and the active is heated the oxidation for a long time in solution, and the alcohol solvent remains the amazing of skin and draws the big drawback of process medicinal material active ingredient residue.

Description

Production integrated system of red pruned pine and red pruned refined extract composition, red pruned pine and red pruned refined extract composition and preparation method thereof
Technical Field
The invention relates to the technical field of daily chemicals, in particular to a production integrated system of a red prunella pini refined extract composition, the red prunella pini refined extract composition, a preparation method and application.
Background
With the wide use of cosmetics and the increasing severity of environmental pollution, modern people have more and more sensitive skin, which is mainly manifested as pruritus, dryness, dandruff, redness, swelling, inflammation and the like, and the medical treatment mode is to use products such as antibiotics and hormones to treat the skin, but the products such as the antibiotics and the hormones 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, the mainly used soothing components are mainly natural plants or traditional Chinese medicine raw materials, but at present, the raw materials mainly have better performance on instant itching relieving, mild anti-inflammation and barrier repair, and the components with good red removing and swelling reducing effects are rare, so 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 daily chemical use process. The traditional plant extraction has many defects, such as low extraction efficiency, long process flow, more impurities, easily oxidized effective components, large adsorption residue of medicinal materials and the like; when the plant extract components are used in the daily chemical field, because the plant extract components are indiscriminately used for long-term external use, 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 on 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 stimulation of methanol or ethanol residues on skin, propylene glycol or 1, 3-butanediol solution is also selected as an extraction solvent, but the two solvents have poor dissolving performance 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 the red prunella pinicola refined extract composition, a preparation method and application.
In a first aspect, the present application provides an integrated system for producing a prune and red essence extract composition, which adopts the following technical scheme:
a production integrated system of a red prune repair and fine extraction composition comprises an extraction tank, a liquid storage tank and a heat exchanger; the extraction tank is an integrated belt pressure extraction tank for extraction and separation integration of 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 to the extraction tank again and then continuously keeps 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 also 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; the heat exchange outlet pipeline of the heat exchanger is provided with a first return pipe and a second return pipe in parallel, the first return pipe is connected with the upper distributor through an upper adsorption residual liquid reflux inlet pipeline through a valve F3, the second return pipe is connected with the lower distributor through a lower adsorption residual liquid reflux inlet pipeline through a valve F4, and the ceramic membrane pipes are vertically and uniformly distributed in the 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 medicinal materials and a solvent (namely adsorption residual liquid) close to the blank is always kept 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 present application provides a red prune refined extract composition, which adopts the following technical scheme:
the red prune refined extract composition 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 the steps of raw material pretreatment, extraction, material carrying, slag discharging and analysis to obtain the red-removed refined extract composition of the red prune; in the extraction process, a production integrated system of the red prune refined extract composition is adopted to carry out convection belt pressure extraction, and the red prune refined extract composition 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 present application provides a preparation method of a prune red-refined extract composition of pinus koraiensis, which adopts the following technical scheme:
a preparation method of a red prune refined extract composition comprises the following steps:
1) pretreatment of raw materials:
pulverizing the medicinal materials of the Pinus koraiensis and the Stephania tetrandra into coarse powder, adding water, and mixing to obtain a 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 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 red prune refined extract composition; wherein the specific requirement of the analysis operation is to continuously feed 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 to the 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 analysis 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 product, namely the malpighia glabra red refined extract composition.
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 distilled liquid 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 tetrandra root and red pine, 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 impurity interception and the water flow speed can be achieved, and the extraction rate 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 composition of the red prune refined extract of the pine, wherein the addition amount of the composition of the red prune refined extract of the pine in the cosmetic is 0.5-10% by weight.
In summary, the present application has the following beneficial effects:
1. the circulation that this application was carried out through taking the area to press convection current to extract, filter and adsorb in step is drawed, solves the preparation inefficiency of the traditional extraction technology of red plum red trimming essence composition of pine, and 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 conduit; 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; 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 red prune refined extract composition. Referring to fig. 1, the integrated production system comprises an extraction tank 3, a liquid storage tank 1 and a heat exchanger 19, and the three parts are communicated through pipelines to form a circulating loop, and the process of extracting and separating alkaloid active ingredients in plants (or the composition of the red prune essential oil) by using deionized water (simply called water) as an extraction solvent and by a circulating convection extraction mode is adopted in the application.
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 on the first sealing cover 25, three tank upper lugs (not marked in the figure) corresponding to the upper cover lugs are welded on 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 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 adsorption residual liquid reflux inlet pipelines 7 are sequentially divided into an upper adsorption residual liquid reflux inlet pipeline 71 and a lower adsorption residual liquid reflux inlet pipeline 72 from top to bottom, a valve F3 is arranged on the upper adsorption residual liquid reflux inlet pipeline 71, and a valve F4 is arranged on the lower adsorption residual liquid reflux inlet pipeline 72. The second vent 28 is installed on the side wall of the extraction tank 3 near and below the upper raffinate reflux inlet line 71, and a valve F7 is also installed on the second vent 28. Two sight glasses 29 adopt transparent glass to make to fix in two relative lateral walls of extracting jar 3 through the ring flange, the operator can see through above-mentioned glass sight glasses 29 that the liquid level height in extracting 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-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 emptying pipe I27 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, in order to penetrate the three regions, 9 openings 13 are formed in the upper and lower closure plates 12, respectively, so as to be opposed to each other. 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 easily indicate the sealing plate 12 having a different orientation, 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 away from the ceramic membrane tube 10, the external threaded pipes 14 are arranged corresponding to the openings 13 on the lower sealing plate one by one, and the upper and lower sealing plates 12 and the external threaded pipes 14 are made of 304 stainless steel metal materials in the 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, the diameter of the through hole 17 is 4/5 of the diameter of the sintered plate 16 in the embodiment, and the inner wall of the externally threaded pipe 14 and the annular rubber gasket on the screw cap 15 are both 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 sealing plates 12, the ceramic membrane tube 10 is cylindrical, a plurality of micropores are densely distributed on the tube wall of the ceramic membrane tube 10, and the pore diameter of the micropores is 100-200 nm. The ceramic membrane tube 10 is filled with resin, and the resin is macroporous adsorption resin in this embodiment, and can be used for adsorbing active ingredients in medicinal materials, so as to reduce the content of the active ingredients in the solvent and make the solvent 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 tube 10 by ceramic membrane tube 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 and 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, the two distributors 11 are arranged oppositely, and the distributor 12 is 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 liquid that adsorbs (being the solvent) can be followed eight shower nozzles 23 and spouted in the cavity 2 of distinguishing the district during this time to the realization has improved the reuse of solvent to adsorbing the residual liquid, and has realized the convection current and has drawed, avoids the area to press and draws the medicinal material and pile up the influence extraction efficiency.
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. A liquid outlet pipeline 20 is arranged at the bottom of the liquid storage tank 1, 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 circulation 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 a reflux line 22.
Referring to fig. 1, the return pipe 22 is composed of a first return pipe and a second return pipe. A first return pipe and a second return pipe are connected in parallel on a heat exchange outlet pipeline of the heat exchanger 19, the first return pipe is connected with the upper distributor through an upper adsorption residual liquid reflux inlet pipeline 71 through a valve F3, the second return pipe is connected with the lower distributor through a lower adsorption residual liquid reflux 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: the red prune refined extract composition 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 the medicinal materials of the Pink red plum and the Stephania tetrandra into coarse powder, adding 4 times of water, uniformly mixing by using a colloid mill, adding the mixture into an extraction tank, adding 6 times of water into a liquid storage tank, heating the mixture to 50 ℃ by using a heat exchanger, then feeding the mixture into an upper distributor and a lower distributor, filling the extraction tank, and adjusting the relative opening degree of a valve F3 and a 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 red prune refined extract composition of the pine red prune.
Example 2: the red prune refined extract composition 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 flos Pinkoraiensis and radix Stephaniae Japonicae 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 relative opening of valve F3 and valve F4 to form convectionAnd (4) extracting. 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 separated liquid of the preparation example 2 is added for elution, and the elution speed is 0.6ml/cm2And s, obtaining the red prune refined extract composition of the pine red prune.
Example 3: the red prune refined extract composition 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 the medicinal materials of the pine red plum and the tetrandra root into coarse powder, adding 5 times of water, uniformly mixing by using a colloid mill, adding the mixture into an extraction tank, adding 5 times of water into a liquid storage tank, heating the mixture to 60 ℃ by using a heat exchanger, then feeding the mixture into an upper distributor and a lower distributor, filling the tank with the mixture, and adjusting the relative opening degree of a valve F3 and a valve F4 to form convection extraction. Extracting at 2.5bar for 75min, discharging, cleaning, adding 3.5 times of the solution of preparation example 3, and eluting at 0.45ml/cm2And s, obtaining the red prune refined extract composition of the pine red prune.
Comparative example
Comparative example 1: a red prune refined extract composition differs from example 1 in that: the amount of the composition used varies.
The red-refined extract composition for repairing red of the 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 the medicinal materials of the pine red plum and the tetrandra root into coarse powder, adding 4 times of water, uniformly mixing by using a colloid mill, adding the mixture into an extraction tank, adding 6 times of water into a liquid storage tank, heating the mixture to 50 ℃ by using a heat exchanger, then feeding the mixture into an upper distributor and a lower distributor, filling the tank with the mixture, and adjusting the relative opening degree of a valve F3 and a 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 red prune refined extract composition of the pine red prune.
Comparative example 2: a red prune refined extract composition differs from example 1 in that: the amount of the composition used varies.
The red-refined extract composition for repairing red of the 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.
The preparation method comprises the following steps: pulverizing the medicinal materials of the pine red plum and the tetrandra root into coarse powder, adding 4 times of water, uniformly mixing by using a colloid mill, adding the mixture into an extraction tank, adding 6 times of water into a liquid storage tank, heating the mixture to 50 ℃ by using a heat exchanger, then feeding the mixture into an upper distributor and a lower distributor, filling the tank with the mixture, and adjusting the relative opening degree of a valve F3 and a 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 red prune refined extract composition of the pine red prune.
Comparative example 3: a prune red-refined extract composition of Pinus koraiensis is different from comparative example 2 in that: the difference of the preparation method is that the conventional stirring extraction is adopted.
The red-refined extract composition for repairing red of the 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.
The preparation method comprises the following steps: pulverizing the medicinal materials of the piny red plum and the tetrandra root into coarse powder, adding 10 times of water, stirring and extracting at 50 ℃ for 1.5h, filtering, and concentrating to obtain the medicinal material with the mass: 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 red prune refined extract composition of the pine red prune.
Comparative example 4: a prune red-refined extract composition of Pinus koraiensis is different from comparative example 2 in that: the difference of the preparation method is that the conventional extraction under pressure is adopted.
The red-repairing and refined-extracting composition for the red 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.
The preparation method comprises the following steps: pulverizing the medicinal materials of the pine red plum and the tetrandra root into coarse powder, adding 10 times of water, extracting for 1.5h at 50 ℃ under pressure, filtering, and concentrating to obtain the medicinal material with the mass: 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 red prune refined extract composition of the pine red prune.
Data analysis
Test one: physical and chemical property detection
Test subjects: the compositions of the red prune extracts prepared in examples 1 to 3 were used as test samples 1 to 3, and the compositions of the red prune extracts 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 a colored complex, the colored complex 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 relative total alkaloid content is 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 alkaloid.
(III) DPPH clearance: the diphenylpicrylphenylhydrazine free radical (2, 2-diphenyl-1-propylhydrazyl, DPPH) is a stable organic free radical, and the stability of the radical is mainly from resonance stabilization and steric hindrance of 3 benzene rings, so that unpaired electrons clamped on nitrogen atoms cannot exert the corresponding electron pairing effect. 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 the absorbance at 517nm of an MD microplate reader after reaction.
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
Figure BDA0003226144860000131
As can be seen by combining examples 1-3 and comparative examples 1-4 with Table 1, 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 those 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 advantageous 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 compositions of the red prune extracts prepared in examples 1 to 3 were used as test samples 1 to 3, and the compositions of the red prune extracts 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 number 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 difference significance analysis is carried out on each group, 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 incubation for 30min, followed by removal, 40. mu.L of SDS solution having a mass concentration of 1.0mg/mL was added, and shaking 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
Figure BDA0003226144860000151
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 equivalent to the positive control in inhibiting trpv1 at a dose of 5%, and is significantly better than that 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
Figure BDA0003226144860000161
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
Figure BDA0003226144860000162
Figure BDA0003226144860000171
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 and homogenizing in vacuum 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
Figure BDA0003226144860000172
Figure BDA0003226144860000181
The preparation method of the pine red plum water comprises the following steps: 1. adding deionized water into the main pot, sequentially adding the 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
Figure BDA0003226144860000182
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, and dissolving.
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 (10)

1. The production integrated system for the red trimming and refined extraction composition of the red prune is characterized by comprising 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);
a distributor (11) and a ceramic membrane tube (10) are arranged in the extraction tank (3), and the end part of the distributor (11) close to the side wall of the extraction tank (3) is connected with an adsorption raffinate reflux 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 integrated system for producing a pruned pine extract composition according to claim 1, wherein said extraction tank (3) is internally provided with an upper distributor and a lower distributor, and the sidewall of the extraction tank (3) is provided with an upper absorption raffinate reflux inlet pipe (71) and a lower absorption raffinate reflux inlet pipe (72); a first return pipe (22) and a second return pipe (22) are arranged on a heat exchange outlet pipeline of the heat exchanger (19) in parallel, the first return pipe (22) is connected to the upper distributor through a valve F3 through an upper adsorption residual liquid reflux inlet pipeline (71), the second return pipe (22) is connected to the lower distributor through a valve F4 through a lower adsorption residual liquid reflux inlet pipeline (72), and a plurality of ceramic membrane pipes (10) are vertically and uniformly distributed in a cavity (2) of the extraction tank (3) between the upper distributor and the lower distributor.
3. The integrated system for producing the prune pini and red essence composition according to claim 1, wherein the top of said extraction tank (3) is further provided with a vent for adjusting the pressure in the extraction tank (3), said vent being provided with a valve F7; an exhaust valve F14 is arranged at the top of the liquid storage tank (1).
4. The red prune refined extract composition 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 comprises the steps of raw material pretreatment, extraction, material carrying, slag discharging and analysis to obtain the red-removed refined extract composition of the red prune; carrying out convection extraction by using the integrated production system of the prune red essence composition of any one of claims 1-3 during the extraction process to obtain the prune red essence composition.
5. The method of claim 4, wherein the method comprises the steps of:
1) pretreatment of raw materials:
pulverizing the medicinal materials of the Pinus koraiensis and the Stephania tetrandra into coarse powder, adding water, and mixing to obtain a 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 suspension of the powder and water obtained in the step 1) into the 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 red prune 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.
6. The method for preparing the composition of refined extract of prune of claim 5, wherein in 1), the amount of water added to the meal is 4-6 times of the weight of the meal, the meal is mixed by a colloid mill after being added with water, and the mixture enters the extraction tank (3) from an inlet pipeline (5) for powder-water suspension.
7. The preparation method of the composition of the red prune and the refining extract of the pine hawthorns as claimed in claim 5, 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.
8. The method for preparing the composition of refined extract of red prune according to claim 5, 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 radix stephaniae tetrandrae and the red prune, the extraction temperature is 50-70 ℃, the pressure is controlled at 2-3 bar, and the extraction time is 1-1.5 h.
9. The method for preparing the composition of refined extract of pruned pine red according to claim 6, wherein the resin is macroporous adsorbent resin, the pore diameter of the ceramic membrane tube (10) is 100-200 nm, and the pore diameter of the sintered plate (16) is 5-10 μm.
10. The use of the composition according to claim 4, wherein the composition is added to the cosmetic in an amount of 0.5 to 10% by weight.
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