CN107137261A - 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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- CN107137261A CN107137261A CN201710183506.4A CN201710183506A CN107137261A CN 107137261 A CN107137261 A CN 107137261A CN 201710183506 A CN201710183506 A CN 201710183506A CN 107137261 A CN107137261 A CN 107137261A
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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 invention provides a kind of preparation method of rough gentian anti-irritant factor and plant extract device, it comprises the following steps：After felwort pulverizing medicinal materials, in input plant extract device, carry out after water extraction, release aqueous extract and the dregs of a decoction；Solvent is added, thermal desorption is carried out under conditions of inert gas presence, obtains the rough gentian anti-irritant factor.The plant extract device include tank body, top cover and under uncap, the top 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 inner side uncapped be equipped with ceramic film and carbon fiber layer that ecto-entad is set gradually.Advantages of the present invention is：Extract, absorption is synchronously carried out, active component is transferred in NACF in time during extraction, makes to be always maintained at of a relatively high concentration difference between extract 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 device, belong to natural product extraction
Technical field.
Background technology
Current anti-irritant composition used for cosmetic has very big application market, with increasingly serious, the people of environmental pollution
Skin it is original more fragile, cosmetics, which are used for a long time, in increasing people can produce stimulations, therefore almost all of be formulated all needs
The composition of anti-irritant is added to reduce the adverse reaction of product, and the anti-irritant composition of plant origin is most popular, but
The anti-irritant composition of plant origin often has that effect is not strong, 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
Leaf glycosides, amarogentin, four acetyl gentiamarins, amaroswerin, gentioflavine, erythricine, cupreol etc. are constituted, and are not yet had at present pair
Its report applied in cosmetics.The preparation of analogous components such as CN200410042874.X, CN201510158387.8,
CN200810176032.1, the method separated using solvent extraction resin, process cycle is long, and loss is big, and cost is high, using organic
Skin products are also easily stimulated by reagent neither safety and environmental protection；CN201310706467.3 is separated using means of supercritical extraction resin
Method, cost is high, and disposal ability is small, and operation difficulty is big；CN201610780013.4 uses stage extraction after solvent extraction
Scheme, obtained product colour is deep, and complex steps, largely uses organic reagent.
The content of the invention
The present invention obtains the rough gentian anti-irritant factor by special preparation technology and equipment from felwort, has after tested
Significant anti-irritant effect, and product colour it is shallow, stably, active component recovery rate is high, process cycle is short, cost is low, do not make
With inflammable and explosive or toxic reagent, energy-saving environmental protection safety.And its certain applications in skin care and cleaning product is disclosed to match somebody with somebody
Side.
The present invention is achieved by the following technical solutions：
In a first aspect, the invention provides a kind of preparation method of the rough gentian anti-irritant factor, it comprises the following steps：
After felwort pulverizing medicinal materials, in input plant extract device, carry out after water extraction, release aqueous extract and medicine
Slag；
Solvent is added, under conditions of inert gas presence, 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, during the water is extracted, it is 100~400rpm control stir speed (S.S.), cycle rate for 3~5 times/
h。
Preferably, in the thermal desorption, it is 300~500 turns/min to control stir speed (S.S.), and cycle rate is 5~8
Secondary/h.
Second aspect, the invention provides a kind of rough gentian anti-irritant factor obtained such as aforementioned preparation process in cosmetics
Purposes, the cosmetics include emulsion, spray water, shampoo etc..
The third aspect, is carried present invention also offers the plant in a kind of preparation method for the foregoing rough gentian anti-irritant factor
Take device, including tank body, top cover and under uncap, the top 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 inner side 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 arranged at the first porous support layer
Second porous support layer of inner side is immobilized.
Preferably, the bottom uncapped under described is communicated with discharging tube, and the discharging tube is also connected with a circulating pump
Logical, the circulating pump is provided with return duct, and the return duct is extended at the top of tank body.
Preferably, the lateral wall of the tank body is provided with heating mantle, and the heating mantle is provided with steam inlet and steaming
Vapor outlet.
Preferably, the top cover enters provided with compressed air inlet, inert gas import, solvent inlet, medicinal material
Mouth and motor, the bottom of the motor are provided 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。
Provided with the liner being made up of microporous membrane and NACF in the plant extract device of the present invention, tank body, carry
The rough gentian anti-irritant factor enters after solvent i.e. by carbon fiber adsorption and catalytic combustion from medicinal material when taking, and is adsorbed during desorption in NACF
The rough gentian anti-irritant factor enters after solvent by circulating progress micro-filtration, reaches desorption, filtering, the degerming synchronous effect carried out.
Compared with prior art, the present invention has following beneficial effect：
1st, extract, adsorb synchronous progress, active component is transferred in NACF in time during extraction, makes extraction
Of a 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 normal temperature is carried out, and active ingredient will not be decomposed uses in change, 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 avoiding final products from carrying secretly
Related reagent is remained, and endangers skin；
4th, desorb and filtering, degerming synchronous progress, purification efficiency is high；
5th, processing step is short, only needs 3 steps to complete to prepare, greatly shortens process cycle, improves production efficiency；
6th, equipment is simple, as long as an equipment is to realize the preparation of product, greatlys save cost and space；
7th, product is attractive in appearance, and the product colour of gained is shallow, stable, is adapted to add using in cosmetics；
8th, product efficacy is obvious, with significant anti-irritant effect；
9th, the skin care obtained and washing formulation stable are attractive in appearance, it is easy to use.
Brief description of the drawings
By reading the detailed description made with reference to the following drawings to non-limiting example, further 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 drawing of a-quadrant in Fig. 1；
In figure：1st, tank body；2nd, top cover；3rd, uncapped under；4th, ceramic film；5th, carbon fiber layer；61st, the first porous support layer；
62nd, the second porous support layer；7th, discharging tube；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.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
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.
It is used for the plant extract device of the preparation method of the foregoing rough gentian anti-irritant factor, including tank body 1, top cover in the present invention
2 and under uncap 3, top cover 2 and under uncap 3 top and bottom for being respectively arranged at tank body 1, wherein, the madial wall of tank body 1 and under open
Ceramic film 4 and carbon fiber layer 5 that ecto-entad is set gradually are equipped with 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 arranged at the inner side of the first porous support layer 61.
Under uncap 3 bottom be communicated with discharging tube 7, discharging tube 7 is also connected with a circulating pump 9 by conduit 8, circulating pump
Return duct 10 is provided with, return duct 10 is extended in the top of tank body 1, the end of discharging tube 7 is liquid outlet 71.
The lateral wall of tank body 1 is provided with heating mantle 11, and heating mantle 11 is provided with steam inlet 111 and steam (vapor) outlet 112.
Top cover 2 enters provided with inert gas import 21, compressed air inlet 22, solvent inlet 23, motor 24 and medicinal material
Mouth 25, the bottom of motor 24 is provided 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.
10~20mm gap is left between tank body and the first porous support layer, the backflow after being passed through for feed liquid, first
Porous support layer is made up of the thick stainless steel plates of two pieces of 3~4mm, 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 arranged at the inner side of the first porous support layer, are 3 by one piece of thickness
~4mm stainless steel folds orifice plate composition, and inner surface is attached with thickness for 2~4mm carbon fiber layers, and stainless steel folds orifice plate can be with
It is laterally folded, can also be vertically folded.The sealing ring set in the first porous support layer and the second porous support layer end is used for
Sealing, enables feed liquid to pass through carbon fiber layer and ceramic film successively, 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, comprises the following steps：
Felwort is crushed to 80 mesh, is placed in foregoing plant extract device, 5 times of water is added and is extracted, the time is
1.5h, mixing speed is 400 turns/min, and cycle rate is 5 times/h, and extraction terminates in the lump to release extract solution and the dregs of a decoction, adds 4
The 50wt% of amount aqueous solution of propylene glycol, 3h are desorbed in 95 DEG C again, and mixing speed is 500 turns/min, and cycle rate is 8 times/h,
Period is passed through 2 times of amount of liquid/h nitrogen, and desorption process is passed through compressed air after terminating make extract solution all outflows, produces.
Embodiment 2
The present embodiment is related to a kind of preparation method of the rough gentian anti-irritant factor, comprises the following steps：
Felwort is crushed to 20 mesh, is placed in foregoing plant extract device, 3 times of water is added and is extracted, the time is
3h, mixing speed is 100 turns/min, and cycle rate is 3 times/h, and extraction terminates in the lump to release extract solution and the dregs of a decoction, adds 2 times
The 30wt% of amount aqueous solution of propylene glycol, 1.5h is desorbed in 70 DEG C, and mixing speed is 300 turns/min, and cycle rate is 5 times/h,
Period is passed through 4 times of amount of liquid/h helium, and desorption process is passed through compressed air after terminating make extract solution all outflows, produces.
Embodiment 3
The present embodiment is related to a kind of preparation method of the rough gentian anti-irritant factor, comprises the following steps：
Felwort is crushed to 40 mesh, is placed in foregoing plant extract device, 4 times of water is added and is extracted, the time is
2h, mixing speed is 300 turns/min, and cycle rate is 4 times/h, and extraction terminates in the lump to release extract solution and the dregs of a decoction, adds 3 times
80% aqueous solution of propylene glycol of amount, 2h is desorbed in 80 DEG C, and mixing speed is 400 turns/min, and cycle rate is 6 times/h, during which
3 times of amount of liquid/h nitrogen is passed through, desorption process is passed through compressed air after terminating make extract solution all outflows, produces.
Comparative example 1
Felwort is crushed to 20 mesh, 6h is extracted with the ethanol of 5 times of amounts 50%, is repeated 4 times, merge extract solution, be concentrated into
Gentiopicroside in different morphological 0.6%, crosses D101 macroreticular resins, with 30% ethanol elution of 10 times of amount of resin, produces.
Comparative example 2
Felwort is crushed to 20 mesh, 3h is extracted in 95 DEG C with the propane diols of 5 times of amounts 50%, filters, 4 DEG C of age overnights,
Filtering, sterilizing, is produced.
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 thing 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 is related to the efficacy test of the rough gentian anti-irritant factor：
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 is mixed with 5%K12 respectively, is pressed《Cosmetics are pacified
Full technical specification》Statistics is smeared and observed to the multiple Skin Irritation Test method of version in 2015, and every group of 6 cavys, male and female are each
Half, as a result as 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 half and half, one full year of life at age 20~50, is persistently smeared in inboard arm
Complete modeling after 2% histamine solution, 30min, smear each experimental group and control sample, during the regression of record gargalesthesia and inflammation
Between, as a result as 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 half and half, one full year of life at age 20~50, is persistently smeared in inboard arm
Complete modeling after 2% capsicum aqueous slkali, 30min, smear each experimental group and control sample, record tingling sensation and inflammation disappear
Move back the time, as a result as shown in table 4.
Table 2：Efficacy test --- cavy anti-irritant experimental result
The guinea pig skin stimulus intensity hierarchical table of table 3.
Table 4, efficacy test --- human body antihistamine stimulation test result
Table 5, efficacy test --- human body capsazepine stimulation test result
Tested from the anti-irritant of cavy and human body, as shown in table 2~5, the rough gentian that the inventive method is prepared resists
Stimulating factor has obvious 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 emulsion prepared using the foregoing rough gentian anti-irritant factor, and it is formulated as shown in table 6
Table 6
Processing step：
(1) A phases are stirred at room temperature scattered complete；
(2) B phase raw materials are sequentially added into addition A phases, is stirred and heated to 75 DEG C to being completely dissolved；
(3) C phases are added, stirring is to being uniformly dispersed；
(4) D phase raw materials are sequentially added, stirs and cools after average 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 produced to being uniformly dispersed.
Embodiment 6
The present embodiment is related to a kind of spray water prepared using the foregoing rough gentian anti-irritant factor, and it is formulated 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 scattered complete to dissolution of raw material, rear stirring be cooled to 55 DEG C with
Under；
(2) main cooker stirring and dissolving is added after the predissolve of B phases raw material uniform；
(3) 45 DEG C of next coming in order addition C phase raw materials are cooled to stir to dissolving completely；
(4) material body naturally cools to moisturizing after room temperature and, to 100%, stirs and produce.
Embodiment 7
The present embodiment is related to a kind of shampoo prepared using the foregoing rough gentian anti-irritant factor, and it is formulated as shown in table 8：
Table 8
Processing step：
(1) deionized water is added into kettle under normal temperature, stirring is lower to add 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 are sequentially added into constant temperature homogeneous 5min after main cooker, stirring and dissolving with C phase raw materials under stirring；
(5) E phases raw material is added into main cooker, continues to stir 3min to well mixed, be down to the slow-speed of revolution and stir and cool；
(6) main cooker temperature is down to after 45 DEG C is slowly added to main cooker by F phases, and stirring at low speed is uniform.
The specific embodiment of the present invention is 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 (10)
1. a kind of preparation method of the rough gentian anti-irritant factor, it is characterised in that comprise the following steps：
After felwort pulverizing medicinal materials, in input plant extract device, carry out after water extraction, release aqueous extract and the dregs of a decoction；
Add solvent, inert gas presence under conditions of, in 70~95 DEG C carry out thermal desorptions, obtain the rough gentian anti-irritant because
Son.
2. the preparation method of the rough gentian anti-irritant factor as claimed in claim 1, it is characterised in that in water extraction, water
Dosage be 3~5 times of felwort medicinal material weight.
3. the preparation method of the rough gentian anti-irritant factor as claimed in claim 1, it is characterised in that the dosage of the solvent is dragon
2~4 times of courage herbal medicine material weight.
4. the preparation method of the rough gentian anti-irritant factor as described in claim 1 or 3, it is characterised in that the solvent is quality
The aqueous solution of propylene glycol of fraction 30~80%.
5. the preparation method of the rough gentian anti-irritant factor as claimed in claim 1, it is characterised in that during the water is extracted, control
Stir speed (S.S.) is 100~400rpm, and cycle rate is 3~5 times/h；In the thermal desorption, it is 300~500 to control stir speed (S.S.)
Turn/min, cycle rate is 5~8 times/h.
6. the rough gentian anti-irritant factor that a kind of preparation method as described in any one in Claims 1 to 5 is obtained is as anti-irritant
Purposes of the active component in household chemicals field.
7. a kind of plant extract device being used in the preparation method of the rough gentian anti-irritant factor described in claim 1, including tank body,
Top cover is uncapped with, and the top cover is uncapped with and is respectively arranged at the top and bottom of tank body, it is characterised in that in the tank body
Side wall and under the inner side uncapped be equipped with ceramic film and carbon fiber layer that ecto-entad is set gradually, the ceramic film
Section is linear, and the section of the carbon fiber layer is in fold-line-shaped, and the ceramic film is by being attached to tank body madial wall and frame
The first porous support layer located at tank base is immobilized, the carbon fiber layer by be arranged on the inside of the first porous support layer second
Porous support layer is immobilized.
8. plant extract device as claimed in claim 7, it is characterised in that the bottom uncapped under described is communicated with discharging tube,
The discharging tube is also connected with a circulating pump, and the circulating pump is provided with return duct, and the return duct is extended at the top of tank body
It is interior.
9. plant extract device as claimed in claim 7, it is characterised in that the top cover is provided with compressed air inlet, lazy
Property gas feed, solvent inlet, medicinal material import and motor, the bottom of the motor is provided with the stirring extended in tank body
Oar.
10. plant extract device as claimed in claim 7, it is characterised 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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| CN112915580A (en) * | 2021-01-12 | 2021-06-08 | 曹洪亮 | Supercritical extraction method for effective components of Chinese herbal medicine |
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| CN112915580B (en) * | 2021-01-12 | 2022-04-01 | 深圳太阳生物科技股份有限公司 | Supercritical extraction method for effective components of Chinese herbal medicine |
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