CN107857792A - A kind of extracting method of gleditschiasaponin - Google Patents
A kind of extracting method of gleditschiasaponin Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J63/00—Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
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- 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
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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
- A61Q19/10—Washing or bathing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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- A61Q5/02—Preparations for cleaning the hair
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Abstract
A kind of extracting method of gleditschiasaponin.The present invention provides one kind and adopts water as solvent, with reference to ultrasound-assisted extraction technology and magnetic water treatment device, expeditiously to extract the method for the natural surfactant gleditschiasaponin in Chinese honey locust, this method is safe and environment-friendly, it is quick, inexpensive, suitable for commercial Application, and the gleditschiasaponin extract solution obtained may be directly applied in personal care product and household care product without purifying concentration.Wherein the power of ultrasonic wave is 300 500W, and the Ultrasonic Radiation time is 6 10 minutes, and Extracting temperature is 80 90 DEG C, and the weight ratio of Chinese honey locust and water is 1:2~1:4, extract 1~3 hour.
Description
Technical field
The present invention relates to a kind of extracting method of gleditschiasaponin, especially with side of the water as solvent extraction gleditschiasaponin
Method.
Background technology
Gleditsia officinalis (Gleditsia Linn) is legume, Caesalpinoidea, shares about 12 kinds.It common are following six
Kind：Gleditsia officinalis (Gleditsia sinensis Lam), Chinese coffeetree fruit tree (Gymnoclabrs chinensis), mountain Gleditsia officinalis
(G.melanacantha), wild Gleditsia officinalis (Gleditisia heterophylla), villus Chinese honey locust tree (G.vestita chun
Ex How), japanese honeylocust tree (Gleditsia.japonica).Wherein Gleditsia officinalis (Gleditsia sinensis Lam) is (again
Claim Chinese Chinese honey locust) be China peculiar kind, growth distribution region accounts for the half of China's area.Gleditsia officinalis is tall for fallen leaves
Wood, trunk is tall and straight, and leaf is luxuriant, and the growth life-span, the period of growth of the crop was up to 200 years up to 600 years.
Gleditsia officinalis whole body may be by.Trunk is wooden good, anticorrosive anti-wear, is fabulous commercial wood.Gleditsia sinensis
Thorn is chinese tradition Chinese medicine, is that treatment breast cancer, lung cancer etc. are more rich in medicinal ingredients such as flavones, saponin, amino acid, phenols
The compatibility Chinese herbal medicine of kind disease.Fructus gleditsiae be Gleditsia officinalis by wound when the lopsided small pod born, there is eliminating the phlegm to have one's ideas straightened out and dissipate
The effect of knot detumescence, it is one of Chinese medicine of Chinese Pharmacopoeia collection.Chinese honey locust fruit includes Gleditsia sinensis Seeds and Chinese honey locust.Gleditsia sinensis Seeds can be with
Chinese honey locust glue is extracted, Chinese honey locust glue can be widely applied to cosmetics, oil exploitation, food medicine, dyeing textile, ore dressing mining etc.
Industry is as thickener, stabilizer, adhesive etc..Contain substantial amounts of natural surfactant gleditschiasaponin in Chinese honey locust, be most ancient
One of old surfactant, it is early to be just used by people to wash clothing, hair, fur etc. in ancient times.In addition, gleditschiasaponin also has
There are desinsection, eliminating the phlegm, have one's ideas straightened out, search wind and other effects.
The well developed root system and resisting drought saving water of Gleditsia officinalis, be ideal ecological seeds, at present countries in the world with China
All in largely plantation Gleditsia officinalis, as farmland, farm shelter-forest, wild fauna and flora protection woods, town and country Landscape Forest and water and soil conservation
Woods etc..But substantial amounts of Chinese honey locust resource is allowed to rot, and is not utilized well, it is extremely valuable natural this has been wasted
Product resource.Substantial amounts of natural surfactant gleditschiasaponin is rich in Chinese honey locust, if the gleditschiasaponin in Chinese honey locust is extracted
Come and successfully apply to personal nursing and household care product in, this is by the plantation for greatly facilitating Gleditsia officinalis and produces downstream
The deep level development of industry chain.It is not only advantageous for afforestation, concedes the land to forestry, promotes the development of Eco-agriculture, and naturally
High-quality plant material, which applies to cosmetics, will promote the upgrading of cosmetic industry, benefit ordinary populace.As can be seen here,
The industrial abstract of gleditschiasaponin and application study, meet the demand of modern society's Green Sustainable.
The molecular structure of gleditschiasaponin is extremely complex, and lipophilic group sapogenin is both contained in molecular structure, and comprising hydrophilic
Group sugar and uronic acid etc., the molecular structure of gleditschiasaponin is shown below.Common sapogenin is pentacyclic triterpenoid,
It is echinocystic acid structure when R1 is OH when R1 is that H is for oleanolic acid structure.Sugar in saponin has glucose, xylose, Arab
Sugar, rhamnose, galactolipin etc., the uronic acid in saponin have galacturonic acid, glucuronic acid etc..
The conventional extracting method of gleditschiasaponin has methanol or ethanol extraction method, percolation, isopropanol dissolving-recrystallization method, returned
Flow extraction method, supercritical fluid extraction, semi-bionic extraction, microwave-assisted, ultrahigh-pressure extraction method, etc..But
Said extracted method is often cumbersome, and solvent usage amount is big, and instrument and equipment is expensive, is not suitable for heavy industrialization operation.
The molecular weight of gleditschiasaponin contains more hydroxyl, carboxyl, ester group isopolarity group in 1600 or so, molecule,
According to the similar principle that mixes, gleditschiasaponin is easily soluble in polar solvent.At present in industry the most frequently used polar solvent have methanol,
Ethanol, water, therefore three of the above solvent is that the most suitable solvent of gleditschiasaponin is extracted in current industry.
(extraction process of mountain gleditschiasaponin and its measure [D] the Jilin Agriculture Universities of surfactant properties are large by Li Yingqiao
Bachelorship paper, 2011) using methanol as solvent, detailed research is carried out to the extracting method of gleditschiasaponin, the results showed that adopt
Extracted 1 hour with 75% methanol, three times, the recovery rate of gleditschiasaponin is 22.39% for extraction altogether.The obvious extracting method Chinese honey locust
The recovery rate of saponin is relatively low, and 77.61% saponin does not extract yet, and the extraction scheme fails sufficiently to utilize Chinese honey locust resource.
Furthermore methanol is severe poisonous chemicals, using methanol as solvent extraction gleditschiasaponin, the methanol remained in product will be to gleditschiasaponin
Use bring potential safety hazard.
Zhang Chunxia etc. (performance of natural surfactant gleditschiasaponin and application [J] Light Engineering Institutes Of Zhengzhou journal,
1993,8(2):Ethanol 56-61) is used as solvent extraction gleditschiasaponin, and its surface-active is studied.Ethanol belongs to
Hazardous chemical, it is inflammable and explosive, and substantial amounts of solvent consumption and cumbersome vacuum distillation program, certainly will greatly it hinder
The commercial Application of gleditschiasaponin.More liposoluble constituent can be contained in the gleditschiasaponin of ethanol extraction, these fat-soluble meetings are tight
The surfactant properties such as the foam of influence gleditschiasaponin of weight, and the color and luster of gleditschiasaponin can be deepened, it is unfavorable for Chinese honey locust
Application of the saponin in personal nursing and household care products.
(gleditschiasaponin Study on extraction [J] Chinese Wild plant resourceses, 2003,22 (6) such as Liang Jingyi:58-61) with
Water is solvent, and orthogonal experiment optimizing research has been carried out to the extraction process of gleditschiasaponin, test result indicates that, carried by solvent of water
The optimum process condition for taking gleditschiasaponin is solid-to-liquid ratio 1:10,45 DEG C of Extracting temperature, 18 hours extraction times, extract three times, soap
The recovery rate of pod saponin is 90.9%.The extraction time of the technique is that (extraction time was to extract three altogether in 18 hours in 54 hours
It is secondary), it is clear that extraction time is too permanent.For Beijing, wherein the content of gleditschiasaponin is 32%, is pressed in the Chinese honey locust place of production used in text
The active matter content that gleditschiasaponin in the extract solution can be then extrapolated according to said extracted technique is about 1%, so low activity
Thing content is obviously not suitable for directly applying in personal nursing and household care products industry.
In summary, the extracting method of gleditschiasaponin is many at present, but often cumbersome, solvent-oil ratio it is big or
Person is not applied to large-scale industrial production and used.So safe and environment-friendly, quick, inexpensive gleditschiasaponin extraction side
The foundation of method seems particularly urgent.
The content of the invention
The present invention uses most abundant cheap water as solvent, is filled with reference to ultrasound-assisted extraction technology and magnetized water treatment
Put, expeditiously to extract the natural surfactant gleditschiasaponin in Chinese honey locust, this method is safe and environment-friendly, it is quick, inexpensive,
Suitable for commercial Application, the gleditschiasaponin of acquisition is high-quality natural material, and obtain gleditschiasaponin extract solution need not purify it is dense
Contracting may be directly applied in personal care product and household care product.
The present invention seeks to what is be achieved through the following technical solutions.
The present invention provides a kind of extracting method of gleditschiasaponin, and it uses Chinese honey locust to make simultaneously as solvent as raw material, water
With magnetic water treatment device and ultrasound-assisted extraction technology.
Magnetized water treatment technology and ultrasound-assisted extraction technology are the new technology, new that recent decades grow up
Skill, the present invention organically combine above-mentioned two technologies, apply in the method for the gleditschiasaponin in extraction Chinese honey locust, to carry
The recovery rate of high gleditschiasaponin, shorten extraction time, possibility is provided for the industrial applications of gleditschiasaponin.
Magnetized water treatment technology utilizes magnetic water treatment device, refers to accompanying drawing 1, and it includes magnetizing reservoir chamber (1), motor
(2), reductor (3), power transmission shaft (4), magnetization impeller (5), the motor (2) connect the reductor (3) and are arranged on described
Magnetize reservoir chamber (1) top, power transmission shaft (4) the connection reductor (3) is simultaneously arranged at magnetization reservoir chamber (1) inside, the magnetic
Change impeller (5) connection power transmission shaft (4)；
Preferably, described magnetization reservoir chamber (1) lower end sets magnetization chamber (12), wherein, magnetic is set inside magnetization chamber (12)
Iron (6)；
Preferably, chuck (7) is set on the outside of the magnetization reservoir chamber (1), chuck (7) one end sets cold water delivery port (8),
The other end sets cold water inlet (9)；
Preferably, the internal magnet (6) of the magnetization chamber (12) is multiple；
Preferably, the magnet (6) is native magnet；
Preferably, the native magnet and the mass ratio of the deionized water are 1:10-20；
Preferably, the native magnet is Fe3O4；
Preferably, the magnetic water treatment device is 200L.
For ultrasound-assisted extraction technology, the efficiency of the power of ultrasonic wave and the radiated time of ultrasonic wave to extraction
All have a great impact.The power of ultrasonic wave is 300-500W, preferably 300W in the present invention；The Ultrasonic Radiation time is 6-10 points
Clock, preferably 6 minutes.
Temperature all has a great impact to the speed of chemical reaction and the balance of chemical reaction.The temperature of extraction is relatively low certainly will
Solubility of the gleditschiasaponin in water can be reduced, the speed of extraction also can be slower.But temperature is too high can cause Chinese honey locust again
The partial hydrolysis of saponin, reduces recovery rate on the contrary.So the Extracting temperature of gleditschiasaponin is very crucial technological parameter.
Solid-to-liquid ratio is the mass ratio of Chinese honey locust and water, it is clear that with the increase of dampening, recovery rate can be correspondingly improved, but water
Increase the concentration of gleditschiasaponin active matter in final extract solution can be caused to reduce.Current personal nursing and household care industry
In standard, shampoo, shower cream, hand cleanser, liquid detergent, the total surfactant content standard of liquid detergent are minimum to be respectively
10%th, 7%, 7%, 15%, 15%.So, after the gleditschiasaponin natural surfactant extract solution of low content must concentrate
Just it can apply in the said goods.The concentration technology of extract solution will necessarily bring the consumption of energy and the increase of human cost etc. no
Good factor.So the selection of solid-to-liquid ratio seems very crucial in extraction process.
Gleditschiasaponin active component is dissolved into the aqueous solution from Chinese honey locust to be needed through Chinese honey locust cell membrane, cell membrane etc., it is clear that
Extension recovery rate over time can be correspondingly improved.But extraction time is oversize, on the one hand because gleditschiasaponin is in the aqueous solution
Middle dissolving reaches saturation, and time lengthening recovery rate does not increase, and is that gleditschiasaponin partial hydrolysis causes recovery rate to reduce on the contrary；Separately
On the one hand, the extension of extraction time can cause the increase that industrial energy consumption, cost of labor etc. all can be at double, be unfavorable for the work of the project
Industry.So extraction of the selection of extraction time to gleditschiasaponin is particularly important.
In the present invention, it is verified by experiments, preferable Extracting temperature is 80-90 DEG C, more preferably 85 DEG C；Chinese honey locust and the weight of water
Amount is than being 1:2~1:4, more preferably 1:3；Extraction 1~3 hour, more preferably 3 hours.
Various Chinese honey locusts can be used in the extracting method of gleditschiasaponin of the present invention, preferably Chinese Chinese honey locust (Gleditsia
sinensis Lam)。
The present invention further provides the gleditschiasaponin extract solution obtained according to the invention described above method.
In another embodiment of the invention, the present invention provides a kind of personal-care supplies, includes Chinese honey locust soap of the present invention
Glucoside extract solution, the personal-care supplies can be shampoo, shower cream, hand cleanser etc..
In another embodiment of the invention, the present invention provides a kind of household care products, includes Chinese honey locust soap of the present invention
Glucoside extract solution, the personal-care supplies can be liquid detergent, liquid detergent etc..
The present invention obtains a kind of gleditschiasaponin natural surfactant of high content by simple water extraction.Live on the surface
Property agent can be widely used in personal-care supplies and household care products, as shampoo, shower cream, hand cleanser, washed
The primary surfactant or cosurfactant of the products such as clothing liquid, liquid detergent.Due to gleditschiasaponin natural surfactant
Lipophilic group is triterpene compound, and hydrophilic radical is the compositions such as polysaccharide, and chemically for the angle of structure, gleditschiasaponin is to skin
The affine degree of skin is necessarily far longer than synthetic surfactant, necessarily active much smaller than synthetic surface to the excitant of skin
Agent.It follows that gleditschiasaponin natural surfactant also can operate with it is high-end wash shield or infant wash and wash one's hair in product.
The present invention intends using most abundant cheap water as solvent, is filled with reference to ultrasound-assisted extraction technology and magnetized water treatment
Put to extract the natural surfactant gleditschiasaponin in Chinese honey locust, in the industrial process conditions found out of the present invention, not only safety,
Environmental protection, quick, cost is low, and the recovery rate of gleditschiasaponin is very high.Such simple, quick operating procedure is transported for large-scale
Practicable operation scheme is provided with Chinese honey locust resource.
In above-mentioned gleditschiasaponin extract solution in addition to containing gleditschiasaponin natural surfactant, also containing a small amount of fiber
The chemical compositions such as element, protein, polysaccharide.Cellulose, protein, polysaccharide etc. are to allow in personal nursing and household care product
The chemical composition used, and said components have thickening, moisturizing and other effects.It is the cellulose that is coexisted in extract solution, protein, more
The impurity such as sugar need not move through separating-purifying.Extraction solvent is water, without by being evaporated under reduced pressure concentration.Therefore, the above method obtains
The gleditschiasaponin extract solution obtained can require no purification ＆ isolation and directly apply in personal nursing and household care products make
For primary surfactant or cosurfactant, the cost of production is greatly reduced.
Brief description of the drawings
Hereinafter, embodiment of the present invention is described in detail with reference to accompanying drawing, wherein：
Fig. 1 is magnetic water treatment device.
The infrared spectrogram of Fig. 2 gleditschiasaponin standard items samples.
Embodiment
The present invention is further described in detail with reference to embodiment, the embodiment provided is only for explaining
The bright present invention, the scope being not intended to be limiting of the invention.
Test method in following embodiments, it is conventional method unless otherwise specified, original used in following embodiments
Material, reagent material etc., unless otherwise specified, it is commercially available products.
Embodiment 1：Preparation, assay and the qualitative reaction of gleditschiasaponin standard items
Gleditsia officinalis (Gleditsia sinensis Lam) of the Chinese honey locust that this experiment uses from the place of production for Henan, Qi Tahua
It is to analyze pure, Chinese medicines group chemical reagents corporation to learn reagent.
(1) measure of the preparation of gleditschiasaponin standard items and gleditschiasaponin content (weight method)：
The 105 DEG C of Chinese honey locust for being dried to weight 2g (being accurate to 0.0001g) are weighed, using ether as solvent soxhlet type 6 hours,
Slough the lipid component in Chinese honey locust.Using methanol as solvent soxhlet type 6 hours, isometric ether is added into methanol extract liquid
The precipitation separated out is collected, is repeated, untill adding ether and no longer separating out precipitation.The precipitation of precipitation is dissolved with water, then
With extracting n-butyl alcohol saponin, repeat, untill n-butanol phase is without gleditschiasaponin, merges butanol extraction liquid, volatilize just
Butanol, residue are put into the measuring cup of weight, and 105 DEG C are dried to weight, can obtain gleditschiasaponin standard items, weigh.This method
The content of gleditschiasaponin in Chinese honey locust can be measured.Calculation formula is as follows：
X-gleditschiasaponin percentage composition, %；
The quality of W1-Chinese honey locust, g；
The quality of the measuring cup of W2-be dried to weight, g；
W3-be dried to the sample of weight and the quality of measuring cup, g.
After measured, the place of production be Henan Chinese honey locust in the content of gleditschiasaponin be 29.8%.
(2) qualitative reaction (aceticanhydride-concentrated sulfuric acid development process) of gleditschiasaponin standard items：
Experimental principle：It is in first yellow that gleditschiasaponin, which meets the concentrated sulfuric acid, is then slowly reddened, then becomes purple, eventually becomes indigo plant
Color.
Experimental method：The gleditschiasaponin standard items sample of a small amount of above-mentioned acquisition is dissolved in the test tube equipped with aceticanhydride, then
The concentrated sulfuric acid-aceticanhydride reagent is added dropwise into test tube, observes the color change in test tube.
Experimental result：Color change order of the gleditschiasaponin standard items sample in test tube is yellow-red-purple-indigo plant
Color.
(3) fusing point of gleditschiasaponin standard items and infrared spectrum analysis：
Fusing point, infrared spectrum, thin-layer chromatography and liquid chromatogram point are carried out to the gleditschiasaponin standard items sample of above-mentioned acquisition
Analysis.
Fusing point：The melting range for measuring gleditschiasaponin is 191~195 DEG C, and literature value is 192~193 DEG C, is coincide substantially.
Infrared spectrum analysis：KBr pressed disc methods.Infrared spectrogram is as shown in Figure 2.
Thin-layer chromatography：Adsorbent uses silica G, and solvent uses ethyl acetate acetic acid-water (8:2:1), with 50% sulphur
Acid is developer.
Liquid chromatogram：ODS-2 C18Reversed-phase column (4.6mm × 250mm, 5 μm), column temperature：40℃；Mobile phase：V (acetonitrile):V
(water)=4:1,0.8mLmin-1；UV-detector, Detection wavelength 454nm.
By checking, the composition for confirming to extract is gleditschiasaponin.
Embodiment 2：Gleditschiasaponin extract solution extraction conditions screen
In the present embodiment, with reference to the method for embodiment 1, the content of gleditschiasaponin in gleditschiasaponin extract solution is surveyed
It is fixed, and accordingly calculate gleditschiasaponin recovery rate.
Embodiment 2-1：The selection of gleditschiasaponin ultrasonic power
In 200L magnetic water treatment devices (referring to Fig. 1), fixed Chinese honey locust:The solid-to-liquid ratio of water is 1:3 (50 kilograms of soaps
Pod：150 kg of water), the ultrasonic wave global radiation time is set as 6 minutes, and extraction time is 2 hours, and Extracting temperature is 85 DEG C.Extraction
After end, filtered acquisition gleditschiasaponin extract solution.Influence of the ultrasonic power to gleditschiasaponin recovery rate is as shown in table 1 below.
Influence of the ultrasonic power of table 1 to recovery rate
As seen from the above table, preferable recovery rate is obtained in 300W-500W scope, when the power of ultrasonic wave is in 300W
When, the recovery rate of gleditschiasaponin is higher, continues to increase ultrasonic power, the recovery rate of gleditschiasaponin has almost no change.
Embodiment 2-2：The selection of Ultrasonic Radiation time
In 200L magnetic water treatment devices (referring to Fig. 1), fixed Chinese honey locust:The solid-to-liquid ratio of water is 1:3 (50 kilograms of soaps
Pod：150 kg of water), the power of ultrasonic wave is set as 300W, and extraction time is 2 hours, and Extracting temperature is 85 DEG C.Extraction terminates
Afterwards, filtered acquisition gleditschiasaponin extract solution.
Influence of the radiated time of ultrasonic wave to gleditschiasaponin recovery rate is as shown in table 2 below.
Influence of the Ultrasonic Radiation time of table 2 to recovery rate
As seen from the above table, the scope in 6-10 minutes obtains preferable recovery rate, when radiated time was at 6 minutes, soap
The recovery rate of pod saponin is higher, continues to increase radiated time, gleditschiasaponin recovery rate has almost no change.
Embodiment 2-3：The selection of Extracting temperature
In 200L magnetic water treatment devices (referring to Fig. 1), fixed Chinese honey locust:The solid-to-liquid ratio of water is 1:3 (50 kilograms of soaps
Pod：150 kg of water), the power of ultrasonic wave is set as 300W, and the Ultrasonic Radiation time is 6 minutes, and extraction time is 2 hours.Carry
After taking end, filtered acquisition gleditschiasaponin extract solution.Influence of the Extracting temperature to gleditschiasaponin recovery rate is as shown in table 3 below.
Influence of the Extracting temperature of table 3 to recovery rate
As seen from the above table, for Extracting temperature at 80~90 DEG C, the recovery rate of gleditschiasaponin is higher.Temperature is below 85 DEG C
When, gradually risen with the rise recovery rate of temperature, when temperature is more than 85 DEG C, recovery rate drops on the contrary with the rise of temperature
It is low.When being probably that temperature is more than 85 DEG C, the hydrolysis of gleditschiasaponin beginning causes.
Embodiment 2-4：The selection of extraction time
In 200L magnetic water treatment devices (referring to Fig. 1), fixed Chinese honey locust:The solid-to-liquid ratio of water is 1:3 (50 kilograms of soaps
Pod：150 kg of water), the power of ultrasonic wave is set as 300W, and the Ultrasonic Radiation time is 6 minutes, and Extracting temperature is 85 DEG C.Carry
After taking end, filtered acquisition gleditschiasaponin extract solution.Influence of the extraction time to gleditschiasaponin is as shown in table 4 below.
Influence of the extraction time of table 4 to recovery rate
As seen from the above table, extraction time, the recovery rate of gleditschiasaponin was higher in 2~4h.It is 2 hours between upon extracting,
The recovery rate of gleditschiasaponin reaches peak.
Embodiment 2-5：The selection of solid-to-liquid ratio
In 200L magnetic water treatment devices (referring to Fig. 1), the power of ultrasonic wave is set as 300W, during Ultrasonic Radiation
Between be 6 minutes, Extracting temperature be 85 DEG C, extraction time be 2 hours.After extraction terminates, filtered acquisition gleditschiasaponin extract solution.
Influence of the solid-to-liquid ratio to gleditschiasaponin recovery rate is as shown in table 5 below.
Influence of the solid-to-liquid ratio of table 5 to recovery rate
| Solid-to-liquid ratio | 1:1 | 1:2 | 1:3 | 1:4 | 1:5 |
| Recovery rate/% | 65.88 | 77.65 | 85.35 | 85.42 | 85.61 |
As seen from the above table, the recovery rate of gleditschiasaponin is with the increase of dampening, recovery rate increase, solid-to-liquid ratio 1:3~1:5
When, the recovery rate of gleditschiasaponin is higher, when solid-to-liquid ratio reaches 1:After 3, the recovery rate of gleditschiasaponin with dampening ratio increase
Change unobvious.
Embodiment 2-6：The orthogonal experiment optimization of extraction conditions
In 200L magnetic water treatment devices (referring to Fig. 1), the power of ultrasonic wave is set as 300W, during Ultrasonic Radiation
Between be 6 minutes.
Utilize the extracting factor of orthogonal experiment, further optimization gleditschiasaponin.When selection and withdrawal temperature (T), extraction
Between (t), the factor that solid-to-liquid ratio (n) is orthogonal test, evaluation criterion is the recovery rate of gleditschiasaponin, and factor level table see the table below 6,
Orthogonal experiments see the table below 7.
The factor level table of table 6
| T (Extracting temperature)/DEG C | T (extraction time)/h | N (solid-to-liquid ratio) | |
| 1 | 80 | 1 | 1:2 |
| 2 | 85 | 2 | 1:3 |
| 3 | 90 | 3 | 1:4 |
The orthogonal experiments of table 7
In upper table, I is that first horizontal gleditschiasaponin recovery rate sum, II corresponding to each factor are each factor
Corresponding second horizontal gleditschiasaponin recovery rate sum, III are the 3rd horizontal gleditschiasaponin corresponding to each factor
Recovery rate sum, I/3 be first horizontal gleditschiasaponin recovery rate corresponding to each factor average value, II/3 for it is each because
The average value of second corresponding to element horizontal gleditschiasaponin recovery rate, III/3 be corresponding to each factor the 3rd it is horizontal
The average value of gleditschiasaponin recovery rate.
As shown in Table 7, gleditschiasaponin yield highest corresponding to sequence number 9 is tested, tests gleditschiasaponin yield corresponding to sequence number 5
Second, the condition tested twice see the table below 8.
The orthogonal test of table 8 analytical table directly perceived
From range analysis, influenceing maximum factor to gleditschiasaponin recovery rate is successively：Extraction time (t) ＞ solid-liquid
Than (n) ＞ Extracting temperatures (T).The optimal extracting factor of gleditschiasaponin is T2t3n2, i.e. Extracting temperature is 85 DEG C, extraction time
For 3 hours, solid-to-liquid ratio 1:3.
3 experimental verifications, as a result as shown in table 9 below, Chinese honey locust soap have been carried out to the Optimal technique process of gleditschiasaponin extraction
The average recoveries of glucoside are 86.56%.
The proving test of table 9
Embodiment 3：The analysis of gleditschiasaponin extract solution physical and chemical index
After measured, the physical and chemical index of liquid mixture is extracted by the experiment 10-12 being performed as described above in example 7 gleditschiasaponins obtained
It is as shown in table 10 below.
The physical and chemical index * of the gleditschiasaponin extract solution of table 10
* method of testing refers to《Cosmetics safety technical specification》(2015 editions)
From the test data in table 10, every physical and chemical index of above-mentioned gleditschiasaponin extract solution meets《Cosmetics
Technical specification of security》Requirement in (2015 editions) to raw material.It follows that the gleditschiasaponin extract solution can be directly as cosmetic
Product raw material is added in cosmetic formulations.
Embodiment 4：The application of gleditschiasaponin extract solution of the present invention
Embodiment 4-1：The preparation of Chinese honey locust shampoo
Weigh following each raw material：Gleditschiasaponin extract solution 4000g of the present invention, EDETATE SODIUM 5g, cocamidopropyl propyl amide sweet tea
Dish alkali 300g, coconut oleoyl amine DEA 100g, silicone emulsion 150g, guar hydroxypropyltrimonium chloride 10g, polyquaternium-
10 5g, citric acid 0.5g, sodium chloride 75g, Kathon CG 4g, essence 17.5g, deionized water 333g.
Guar hydroxypropyltrimonium chloride and 200g water are stirred, obtain melon glue Hydroxyproyl Trimethyl chlorination
Aqueous ammonium.Polyquaternium-10 and 133g water are stirred, obtain the Polyquaternium-10 aqueous solution.
Gleditschiasaponin extract solution of the present invention is added in agitated kettle, is heated to 75 DEG C.Add melon glue hydroxypropyl trimethylammonium
The ammonium chloride aqueous solution, the Polyquaternium-10 aqueous solution, stir；Add EDETATE SODIUM, Cocoamidopropyl betaine, coconut palm
Oleamide DEA, stirs；45 DEG C are cooled to, adds silicone emulsion, citric acid, sodium chloride, Kathon CG, essence, stirs 30 points
Clock, then with 200 mesh filter screen filtrations, produce.
Embodiment 4-2：The preparation of Chinese honey locust shower cream
Weigh following each raw material：Gleditschiasaponin extract solution 2250g of the present invention, EDETATE SODIUM 5g, cocamidopropyl propyl amide sweet tea
Dish alkali 300g, coconut oleoyl amine DEA 100g, citric acid 0.5g, sodium chloride 100g, Kathon CG 4g, essence 17.5g, deionized water
2223g。
Successively by deionized water, gleditschiasaponin extract solution of the present invention, EDETATE SODIUM, Cocoamidopropyl betaine, cocounut oil
Acid amides DEA, citric acid, sodium chloride, Kathon CG, essence are added in agitated kettle, are stirred 60 minutes, then with 200 mesh screen pack mistakes
Filter, is produced.
Embodiment 4-3：The preparation of Chinese honey locust hand cleanser
Weigh following each raw material：Gleditschiasaponin extract solution 1250g of the present invention, laureth sodium sulfovinate 125g,
EDETATE SODIUM 5g, Cocoamidopropyl betaine 300g, coconut oleoyl amine DEA100g, citric acid 0.5g, sodium chloride 100g, Kathon CG
4g, essence 17.5g, deionized water 3098g.
Successively by deionized water, gleditschiasaponin extract solution of the present invention, laureth sodium sulfovinate, EDETATE SODIUM, cocounut oil
Amido propyl betaine, coconut oleoyl amine DEA, citric acid, sodium chloride, Kathon CG, essence are added in agitated kettle, are stirred 60 minutes,
Then with 200 mesh filter screen filtrations, produce.
Embodiment 4-4：The preparation of Chinese honey locust liquid detergent
Weigh following each raw material：Gleditschiasaponin extract solution 500g of the present invention, neopelex 300g, laruyl alcohol
The 200g of polyethers -9, laureth sodium sulfovinate 300g, sodium citrate 25g, hydroxyethyl cellulose 35g, DMDMH
10g, essence 7.5g, deionized water 3622.5g.
Successively by deionized water, gleditschiasaponin extract solution of the present invention, neopelex, laureth -9, the moon
Laureth sodium sulfovinate, sodium citrate, hydroxyethyl cellulose, DMDMH, essence are added in agitated kettle, stirring 60
Minute, then with 200 mesh filter screen filtrations, produce.
Embodiment 4-5：The preparation of Chinese honey locust liquid detergent
Weigh following each raw material：Gleditschiasaponin extract solution 750g of the present invention, neopelex 300g, laruyl alcohol
The 75g of polyethers -9, laureth sodium sulfovinate 500g, sodium citrate 25g, sodium chloride 75g, DMDMH 10g, essence
7.5g, deionized water 3257.5g.
Successively by deionized water, gleditschiasaponin extract solution of the present invention, neopelex, laureth -9, the moon
Laureth sodium sulfovinate, sodium citrate, sodium chloride, DMDMH, essence are added in agitated kettle, are stirred 60 minutes,
Then with 200 mesh filter screen filtrations, produce.
Claims (10)
1. a kind of extracting method of gleditschiasaponin, it is characterised in that using Chinese honey locust as raw material, water uses magnetic as solvent
Water chemical treatment device and ultrasound-assisted extraction technology.
2. the extracting method of gleditschiasaponin according to claim 1, wherein the magnetic water treatment device used includes magnetization
Reservoir chamber (1), motor (2), reductor (3), power transmission shaft (4), magnetization impeller (5), the motor (2) connect the reductor
(3) and described magnetization reservoir chamber (1) top is arranged on, power transmission shaft (4) the connection reductor (3) is simultaneously arranged at magnetization reservoir chamber
(1) it is internal, magnetization impeller (5) the connection power transmission shaft (4)；
Preferably, described magnetization reservoir chamber (1) lower end sets magnetization chamber (12), wherein, magnet is set inside magnetization chamber (12)
(6)；
Preferably, chuck (7) is set on the outside of the magnetization reservoir chamber (1), and chuck (7) one end sets cold water delivery port (8), another
End sets cold water inlet (9)；
Preferably, the internal magnet (6) of the magnetization chamber (12) is multiple；
Preferably, the magnet (6) is native magnet；
Preferably, the native magnet and the mass ratio of the deionized water are 1:10-20；
Preferably, the native magnet is Fe3O4；
Preferably, the magnetic water treatment device is 200L.
3. the power of the extracting method of gleditschiasaponin according to claim 1 or 2, wherein ultrasonic wave is 300-500W, surpass
The acoustic irradiation time is 6-10 minutes.
4. the power of the extracting method of gleditschiasaponin according to claim 3, wherein ultrasonic wave is 300W, Ultrasonic Radiation
Time is 6 minutes.
5. the extracting method of the gleditschiasaponin according to claim any one of 1-4, wherein Extracting temperature are 80-90 DEG C, soap
The weight of pod and water ratio is 1:2~1:4, extract 1~3 hour.
6. the extracting method of gleditschiasaponin according to claim 5, wherein Extracting temperature are 85 DEG C, the weight of Chinese honey locust and water
Than for 1:3, extract 3 hours.
7. the extracting method of the gleditschiasaponin according to claim any one of 1-6, the Chinese honey locust used is Chinese Chinese honey locust
(Gleditsia sinensis Lam)。
8. the gleditschiasaponin extract solution obtained according to any one of claim 1-7 extracting method.
9. a kind of personal-care supplies, the gleditschiasaponin extract solution comprising claim 8, it is preferably shampoo, shower cream, washed
Hand liquid.
10. a kind of household care products, the gleditschiasaponin extract solution comprising claim 8, it is preferably liquid detergent, liquid detergent.
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| CN113549502A (en) * | 2021-08-18 | 2021-10-26 | 中华全国供销合作总社南京野生植物综合利用研究所 | Formula and preparation method of liquid detergent containing gleditschia horrida saponin |
| CN113583766A (en) * | 2021-08-18 | 2021-11-02 | 广州德谷个人护理用品有限公司 | Formula and preparation method of laundry detergent containing gleditschia horrida saponin |
| CN113599323A (en) * | 2021-08-18 | 2021-11-05 | 广州德谷个人护理用品有限公司 | Formula and preparation method of shower gel containing gleditschia horrida saponin |
| CN115595215A (en) * | 2022-09-07 | 2023-01-13 | 江苏雪豹日化有限公司（Cn） | Environment-friendly oil stain purifying agent and preparation method thereof |
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| CN113599323A (en) * | 2021-08-18 | 2021-11-05 | 广州德谷个人护理用品有限公司 | Formula and preparation method of shower gel containing gleditschia horrida saponin |
| CN115595215A (en) * | 2022-09-07 | 2023-01-13 | 江苏雪豹日化有限公司（Cn） | Environment-friendly oil stain purifying agent and preparation method thereof |
| CN115595215B (en) * | 2022-09-07 | 2023-09-15 | 江苏雪豹日化有限公司 | Greasy dirt purifying agent and preparation method thereof |
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