CN107137261B - Preparation method, purposes and the plant extract device of the rough gentian anti-irritant factor - Google Patents
Preparation method, purposes and the plant extract device of the rough gentian anti-irritant factor Download PDFInfo
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- CN107137261B CN107137261B CN201710183506.4A CN201710183506A CN107137261B CN 107137261 B CN107137261 B CN 107137261B CN 201710183506 A CN201710183506 A CN 201710183506A CN 107137261 B CN107137261 B CN 107137261B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/74—Biological properties of particular ingredients
- A61K2800/75—Anti-irritant
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Abstract
The present invention provides a kind of preparation method of rough gentian anti-irritant factor and plant extract devices, include the following steps：It after felwort pulverizing medicinal materials, puts into plant extract device, after carrying out water extraction, releases aqueous extract and the dregs of a decoction；Solvent is added in, thermal desorption is carried out under the conditions of existing for inert gas, obtains the rough gentian anti-irritant factor.The plant extract device include tank body, head cover and under uncap, the head cover and under uncap and be respectively arranged at the top and bottom of tank body, wherein, the tank body madial wall and under the inside uncapped be equipped with ceramic film and carbon fiber layer that ecto-entad is set gradually.Advantages of the present invention is：Extraction, the synchronous progress of absorption, active constituent is transferred in activated carbon fibre in time during extraction, makes to be always maintained at relatively high concentration difference between extracting solution and medicinal material, and recovery rate is high, and reduces the usage amount of solvent.
Description
Technical field
The present invention relates to a kind of preparation method of rough gentian anti-irritant factor and plant extract devices, belong to natural product extraction
Technical field.
Background technology
Current anti-irritant ingredient used for cosmetic has very big application market, with the getting worse of environmental pollution, people
Skin it is originally more fragile, cosmetics, which are used for a long time, in more and more people can generate stimulation, therefore almost all of be formulated all needs
The ingredient of anti-irritant is added to reduce the adverse reaction of product, and the anti-irritant ingredient of plant origin is most popular, but
The anti-irritant ingredient of plant origin is not often strong there are effect, and unstable, the smell is awful, and color can not be esthetically acceptable to the consumers deeply
Shortcoming.
The rough gentian anti-irritant factor is prepared from felwort, mainly by gentiamarin, Swertiamarin, chiratin, three
The compositions such as leaf glycosides, amarogentin, four acetyl gentiamarins, amaroswerin, gentioflavine, erythricine, cupreol, there has been no right at present
Its report applied in cosmetics.The preparation of analogous components such as CN200410042874.X, CN201510158387.8,
CN200810176032.1, the method detached using solvent extraction resin, process cycle is long, and loss is big, and of high cost, use is organic
Reagent neither safety and environmental protection also easily stimulates skin products；CN201310706467.3 is detached using means of supercritical extraction resin
Method, of high cost, processing capacity is small, and operation difficulty is big；CN201610780013.4 is using stage extraction after solvent extraction
Scheme, obtained product colour is deep, and complex steps, largely uses organic reagent.
Invention content
The present invention obtains the rough gentian anti-irritant factor by special preparation process and equipment from felwort, has after tested
Significant anti-irritant effect, and product colour is shallow, stables, active constituent recovery rate height, process cycle are short, it is at low cost, do not make
With inflammable and explosive or toxic reagent, energy-saving environmental protection safety.And it discloses its certain applications in skin care and cleaning product to match
Side.
The present invention is achieved by the following technical solutions：
In a first aspect, the present invention provides a kind of preparation method of the rough gentian anti-irritant factor, include the following steps：
It after felwort pulverizing medicinal materials, puts into plant extract device, after carrying out water extraction, releases aqueous extract and medicine
Slag；
Solvent is added in, under the conditions of existing for inert gas, thermal desorption is carried out in 70~95 DEG C, obtains the anti-thorn of the rough gentian
Swash the factor.
Preferably, in water extraction, the dosage of water is 3~5 times of felwort medicinal material weight.
Preferably, the dosage of the solvent is 2~4 times of felwort medicinal material weight.
Preferably, the solvent is the aqueous solution of propylene glycol of mass fraction 30~80%.
Preferably, in water extraction, control stir speed (S.S.) is 100~400rpm, cycle rate is 3~5 times/
h。
Preferably, in the thermal desorption, control stir speed (S.S.) is 300~500 turns/min, and cycle rate is 5~8
Secondary/h.
Second aspect, the present invention provides a kind of rough gentian anti-irritant factor obtained such as aforementioned preparation process in cosmetics
Purposes, the cosmetics include lotion, spray water, shampoo etc..
The third aspect, the present invention also provides the plants in a kind of preparation method for the aforementioned rough gentian anti-irritant factor to carry
Take device, including tank body, head cover and under uncap, the head cover and under uncap and be respectively arranged at the top and bottom of tank body, wherein,
The tank body madial wall and under the inside uncapped be equipped with ceramic film and carbon fiber layer that ecto-entad is set gradually, it is described
The section of ceramic film is linear, and the section of the carbon fiber layer is in fold-line-shaped, and the ceramic film is by being attached in tank body
Side wall and be set up in tank base the first porous support layer it is immobilized, the carbon fiber layer is by being set to the first porous support layer
Second porous support layer of inside is immobilized.
Preferably, the bottom uncapped under described is communicated with drain pipe, and the drain pipe is also connected with a circulating pump
Logical, the circulating pump is equipped with return duct, and the return duct is extended at the top of tank body.
Preferably, the lateral wall of the tank body is equipped with heating mantle, and the heating mantle is provided with steam inlet and steaming
Vapor outlet.
Preferably, the head cover be equipped with compressed air inlet, inert gas import, solvent inlet, medicinal material into
Mouth and motor, the bottom of the motor are equipped with the agitating paddle extended in tank body.
Preferably, the end of first porous support layer and the second porous support layer is nested with sealing ring.
Preferably, the source of the carbon fiber is timber or coconut husk, and the aperture of the ceramic membrane is 0.1~0.45
μm。
The plant extract device of the present invention, tank body is interior to be equipped with the liner being made of microporous membrane and activated carbon fibre, carries
When taking the rough gentian anti-irritant factor from medicinal material enter solvent after i.e. by carbon fiber adsorption and catalytic combustion, adsorbed in activated carbon fibre during desorption
The rough gentian anti-irritant factor enters after solvent carries out micro-filtration by cycle, achievees the effect that desorption, filtering, degerming synchronize and carries out.
Compared with prior art, the present invention has following advantageous effect：
1st, it extracts, adsorb synchronous progress, active constituent is transferred in activated carbon fibre in time during extraction, makes extraction
Relatively high concentration difference is always maintained between liquid and medicinal material, recovery rate is high, and reduces the usage amount of solvent；
2nd, active ingredient is retained, and extraction process room temperature carries out, and active ingredient will not decompose variation, be used in desorption process
Inert gas is protected, and reduces the generation of the reactions such as oxidation；
3rd, without using inflammable and explosive or toxic reagent, energy-saving and environmental protection, production safety, while also final products is avoided to carry secretly
Related reagent remains, and endangers skin；
4th, desorption with filtering, degerming it is synchronouss carry out, purification efficiency height；
5th, processing step is short, only needs 3 steps that preparation can be completed, and greatly shortens process cycle, improves production efficiency；
6th, equipment is simple, as long as an equipment is to realize the preparation of product, cost and space is greatly saved；
7th, product is beautiful, and resulting product is of light color, stablizes, and is suitble to add using in cosmetics；
8th, product efficacy is apparent, has significant anti-irritant effect；
9th, the skin care obtained and washing formulation stable, it is beautiful, it is easy to use.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is plant extract apparatus structure schematic diagram in the present invention；
Fig. 2 is the partial enlarged view of a-quadrant in Fig. 1；
In figure：1st, tank body；2nd, head cover；3rd, it uncaps under；4th, ceramic film；5th, carbon fiber layer；61st, the first porous support layer；
62nd, the second porous support layer；7th, drain pipe；8th, conduit；9th, circulating pump；10th, return duct；11st, heating mantle；12nd, sealing ring；111、
Steam inlet；112nd, steam (vapor) outlet；21st, inert gas import；22nd, compressed air inlet；23rd, solvent inlet；24th, motor；
25th, medicinal material import；26th, agitating paddle；71st, liquid outlet.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
For the plant extract device of the preparation method of the aforementioned rough gentian anti-irritant factor in the present invention, including tank body 1, head cover
2 and under uncap 3, head cover 2 and under uncap 3 top and bottom for being respectively arranged at tank body 1, wherein, 1 madial wall of tank body and under open
Ceramic film 4 and the carbon fiber layer 5 that ecto-entad is set gradually are equipped on the inside of lid, the section of ceramic film 4 is linear,
The section of carbon fiber layer 5 is in fold-line-shaped, and ceramic film 4 is by being attached to tank body madial wall and being set up in more than the first of tank base
Hole supporting layer 61 is immobilized, and carbon fiber layer 5 is immobilized by the second porous support layer 62 for being set to 61 inside of the first porous support layer.
Under uncap 3 bottom be communicated with drain pipe 7, drain pipe 7 is also connected with a circulating pump 9 by conduit 8, circulating pump
Return duct 10 is equipped with, return duct 10 is extended in 1 top of tank body, and the end of drain pipe 7 is liquid outlet 71.
The lateral wall of tank body 1 is equipped with heating mantle 11, and heating mantle 11 is provided with steam inlet 111 and steam (vapor) outlet 112.
Head cover 2 be equipped with inert gas import 21, compressed air inlet 22, solvent inlet 23, motor 24 and medicinal material into
Mouth 25, the bottom of motor 24 are equipped with the agitating paddle 26 extended in tank body 1.
The end of first porous support layer 61 and the second porous support layer 62 is nested with sealing ring 12.
There are the gap of 10~20mm between tank body and the first porous support layer, the reflux after being penetrated for feed liquid, first
Porous support layer is made of the stainless steel plate of two pieces of 3~4mm thickness, filled with the microporous membrane that thickness is 5~10mm, is used for
Support and transmission to ceramic film, the second porous support layer are set to the inside of the first porous support layer, are 3 by one piece of thickness
The stainless steel of~4mm folds orifice plate composition, and inner surface is attached with thickness as 2~4mm carbon fiber layers, and stainless steel folds orifice plate can be with
It is laterally folded, it can also be vertically folded.It is used in the sealing ring of the first porous support layer and the second porous support layer end set
Sealing enables feed liquid successively through carbon fiber layer and ceramic film, without passing through from other gaps.
Embodiment 1
The present embodiment is related to a kind of preparation method of the rough gentian anti-irritant factor, includes the following steps：
Felwort is crushed to 80 mesh, is placed in aforementioned plant extract device, 5 times of water is added in and extracts, the time is
1.5h, mixing speed are 400 turns/min, and cycle rate is 5 times/h, and extraction terminates together to release extracting solution and the dregs of a decoction, adds in 4
The aqueous solution of propylene glycol of the 50wt% of amount again desorbs 3h in 95 DEG C, and mixing speed is 500 turns/min, and cycle rate is 8 times/h,
Period is passed through the nitrogen of 2 times of amount of liquid/h, be passed through after desorption process compressed air make extracting solution all outflow to get.
Embodiment 2
The present embodiment is related to a kind of preparation method of the rough gentian anti-irritant factor, includes the following steps：
Felwort is crushed to 20 mesh, is placed in aforementioned plant extract device, 3 times of water is added in and extracts, the time is
3h, mixing speed are 100 turns/min, and cycle rate is 3 times/h, and extraction terminates together to release extracting solution and the dregs of a decoction, adds in 2 times
The aqueous solution of propylene glycol of the 30wt% of amount desorbs 1.5h in 70 DEG C, and mixing speed is 300 turns/min, and cycle rate is 5 times/h,
Period is passed through the helium of 4 times of amount of liquid/h, be passed through after desorption process compressed air make extracting solution all outflow to get.
Embodiment 3
The present embodiment is related to a kind of preparation method of the rough gentian anti-irritant factor, includes the following steps：
Felwort is crushed to 40 mesh, is placed in aforementioned plant extract device, 4 times of water is added in and extracts, the time is
2h, mixing speed are 300 turns/min, and cycle rate is 4 times/h, and extraction terminates together to release extracting solution and the dregs of a decoction, adds in 3 times
80% aqueous solution of propylene glycol of amount desorbs 2h in 80 DEG C, and mixing speed is 400 turns/min, and cycle rate is 6 times/h, during which
Be passed through the nitrogen of 3 times of amount of liquid/h, be passed through after desorption process compressed air make extracting solution all outflow to get.
Comparative example 1
Felwort is crushed to 20 mesh, 6h is extracted with the ethyl alcohol of 5 times of amounts 50%, is repeated 4 times, merges extracting solution, be concentrated into
Gentiopicroside in different morphological 0.6%, cross D101 macroreticular resins, with 30% ethanol elution of 10 times of amount of resin to get.
Comparative example 2
Felwort is crushed to 20 mesh, 3h is extracted in 95 DEG C with the propylene glycol of 5 times of amounts 50%, filters, 4 DEG C of age overnights,
Filtering, sterilize to get.
Table 1：The physical and chemical testing result control of the rough gentian anti-irritant factor prepared by embodiment and comparative example
| Experimental method | Gentiamarin recovery rate % | Gross activity object recovery rate % | Stability * | Process cycle |
| Embodiment 1 | 79.2 | 77.3 | 9 months | 6h |
| Embodiment 2 | 76.0 | 75.9 | 10 months | 6h |
| Embodiment 3 | 77.8 | 75.5 | 10 months | 6h |
| Comparative example 1 | 40.2 | 21.3 | 7 months | 40h |
| Comparative example 2 | 55.4 | 60.6 | 0.5 month | 19h |
* study on the stability condition：4 DEG C, 48 DEG C, normal-temperature light shine, -18~48 DEG C of alternatings, the index of investigation is color, clear and bright
Degree, pH value, smell.
As shown in Table 1, the recovery rate for the raising active ingredient that the preparation method of this programme can be larger, improves stability, greatly
Width shortens process cycle and cost.
Embodiment 4
The present embodiment, which is related to the effect of rough gentian anti-irritant factor, to be tested：
1st, efficacy test method 1 --- guinea pig skin anti-irritant is tested
Using 5%K12 as model group, the sample of experimental group and positive controls mixes respectively with 5%K12, presses《Cosmetics are pacified
Full technical specification》Statistics is smeared and observed to the multiple Skin Irritation Test method of version in 2015, every group of 6 cavys, and male and female are each
Half, the results are shown in Table 2.
2nd, efficacy test method 2 --- human body antihistamine stimulation test
The volunteer 20 of normal skin is chosen, men and women is fifty-fifty, 20~50 one full year of life of age, is persistently smeared in inboard arm
2% histamine solution completes modeling after 30min, smears each experimental group and control sample, when recording the recession of gargalesthesia and inflammation
Between, the results are shown in Table 3.
3rd, efficacy test method 3 --- human body capsazepine stimulation test
The volunteer 20 of normal skin is chosen, men and women is fifty-fifty, 20~50 one full year of life of age, is persistently smeared in inboard arm
2% capsicum aqueous slkali completes modeling after 30min, smears each experimental group and control sample, records disappearing for tingling sensation and inflammation
The time is moved back, the results are shown in Table 4.
Table 2：Efficacy test --- cavy anti-irritant experimental result
3. guinea pig skin stimulus intensity hierarchical table of table
Table 4, efficacy test --- human body antihistamine stimulation test result
Table 5, efficacy test --- human body capsazepine stimulation test result
It is tested as the anti-irritant of cavy and human body it is found that as shown in table 2~5, the rough gentian that the method for the present invention is prepared resists
Stimulating factor has apparent anti-irritant effect, and effect is suitable with hormone drug, can be applied to various doses of skin care and cleaning product
Type.
Embodiment 5
The present embodiment is related to a kind of lotion prepared using the aforementioned rough gentian anti-irritant factor, and formula is as shown in table 6
Table 6
Processing step：
(1) dispersion is stirred at room temperature completely in A phases；
(2) B phase raw materials are sequentially added and adds in A phases, be stirred and heated to 75 DEG C to being completely dissolved；
(3) C phases are added in, stirring is to being uniformly dispersed；
(4) D phase raw materials are sequentially added, stir and are cooled down after mean value 3min；
(5) 65 DEG C are cooled to and sequentially adds E phases, stirring is to being uniformly dispersed；
(6) 45 DEG C are cooled to and sequentially adds F phases, stirring is to being uniformly dispersed to obtain the final product.
Embodiment 6
The present embodiment is related to a kind of spray water prepared using the aforementioned rough gentian anti-irritant factor, and formula is as shown in table 7：
Table 7
Processing step：
(1) A phases raw material in main cooker stir and be warming up to 80 DEG C it is complete to dissolution of raw material dispersion, rear stirring be cooled to 55 DEG C with
Under；
(2) it is uniform that main cooker stirring and dissolving is added in after the predissolve of B phases raw material；
(3) 45 DEG C of next coming in order addition C phase raw materials are cooled to stir to dissolving completely；
(4) moisturizing is stirred evenly to 100% after expecting body cooled to room temperature to obtain the final product.
Embodiment 7
The present embodiment is related to a kind of shampoo prepared using the aforementioned rough gentian anti-irritant factor, and formula is as shown in table 8：
Table 8
Processing step：
(1) deionized water is added in into kettle under room temperature, is added with stirring JR400, it is to be dissolved completely after be warming up to 75 DEG C；
(2) raw material in B phases is sequentially added into kettle, stirring and dissolving is pumped into main cooker afterwards completely, is warming up to 75 DEG C；
(3) by raw material predissolve in C phases；
(4) D phases and C phase raw materials are sequentially added into main cooker under stirring, constant temperature homogeneous 5min after stirring and dissolving；
(5) E phases raw material is added in into main cooker, continues to stir 3min to being uniformly mixed, be down to the slow-speed of revolution and stir and cool down；
(6) F phases are slowly added to main cooker after main cooker temperature is down to 45 DEG C, stirring at low speed is uniform.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (5)
1. a kind of preparation method of the rough gentian anti-irritant factor, which is characterized in that include the following steps：
It after felwort pulverizing medicinal materials, puts into plant extract device, after carrying out water extraction, releases aqueous extract and the dregs of a decoction；
Add in solvent, under the conditions of existing for inert gas, in 70~95 DEG C carry out thermal desorptions, obtain the rough gentian anti-irritant because
Son；
In water extraction, the dosage of water is 3~5 times of felwort medicinal material weight；
The dosage of the solvent is 2~4 times of felwort medicinal material weight；
The solvent is the aqueous solution of propylene glycol of mass fraction 30~80%；
The plant extract device include tank body, head cover and under uncap, the head cover and under uncap and be respectively arranged at the top of tank body
Portion and bottom, which is characterized in that the tank body madial wall and under the inside uncapped be equipped with the pottery that ecto-entad is set gradually
Porcelain film layer and carbon fiber layer, the section of the ceramic film is linear, and the section of the carbon fiber layer is in fold-line-shaped, the pottery
Porcelain film layer by be attached to tank body madial wall and be set up in tank base the first porous support layer it is immobilized, the carbon fiber layer by
The second porous support layer being set on the inside of the first porous support layer is immobilized.
2. the preparation method of the rough gentian anti-irritant factor as described in claim 1, which is characterized in that in the water extraction, control
Stir speed (S.S.) is 100~400rpm, and cycle rate is 3~5 times/h；In the thermal desorption, control stir speed (S.S.) is 300~500
Turn/min, cycle rate is 5~8 times/h.
3. the preparation method of the rough gentian anti-irritant factor as described in claim 1, which is characterized in that the bottom uncapped under described connects
Drain pipe is connected with, the drain pipe is also connected with a circulating pump, and the circulating pump is equipped with return duct, the return duct extension
In at the top of to tank body.
4. the preparation method of the rough gentian anti-irritant factor as described in claim 1, which is characterized in that the head cover is equipped with compression
Air intlet, inert gas import, solvent inlet, medicinal material import and motor, the bottom of the motor, which is equipped with, extends to tank
Internal agitating paddle.
5. the preparation method of the rough gentian anti-irritant factor as described in claim 1, which is characterized in that the source of the carbon fiber is
Timber or coconut husk, the aperture of the ceramic membrane is 0.1~0.45 μm.
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