CN109924501A - A kind of extraction process of brush-cherry seed for health care - Google Patents
A kind of extraction process of brush-cherry seed for health care Download PDFInfo
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- CN109924501A CN109924501A CN201910273142.8A CN201910273142A CN109924501A CN 109924501 A CN109924501 A CN 109924501A CN 201910273142 A CN201910273142 A CN 201910273142A CN 109924501 A CN109924501 A CN 109924501A
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Abstract
The invention discloses a kind of extraction processes of brush-cherry seed for health care, comprising the following steps: S1, to pretreatment of raw material obtains raw material powder；S2, raw material powder is extracted using ethanol solution reflux extraction, obtains extracting solution；S3, extracting solution is filtered, obtains filtrate；S4, extracting solution is concentrated, obtains condensed cream；The content of amarogentin and prunuside in S5, measurement condensed cream；S6, alcohol precipitation processing is carried out to condensed cream, obtains clear liquid；S7, clear liquid is filtered；S8, filtered clear liquid is dried, obtains brush-cherry seed dry powder；The content of amarogentin and prunuside in S9, measurement brush-cherry seed dry powder；S10, packaging are simultaneously put in storage preservation finished product.The present invention uses reduced-pressure backflow extractive technique, and low temperature, low pressure guarantee the stability of brush-cherry seed；Using shaking screen primary filtration, brush-cherry seed bulky grain residue is removed, then technology is filtered by vacuum using diatomite, removes insoluble substance, and be recycled to brush-cherry seed residue, energy conservation and environmental protection.
Description
Technical field
The present invention relates to brush-cherry seed product manufacture field for health care more particularly to a kind of extraction works of brush-cherry seed for health care
Skill.
Background technique
Brush-cherry seed is the kernel of the rosaceous plants such as strongly fragrant Lee, Ou Li, flowering plum, long stalk almond, alias mountain plum, Xiao Li
Benevolence is distributed in the ground such as Heilungkiang, Jilin, Liaoning, the Inner Mongol, in the summer, when the fruit matures in the fall picks, and removes pulp, breaks nucleocapsid,
Seed is taken out, dries and obtain, main component is amarogentin and prunuside, mild-natured, acrid flavour, hardship, sweet, with moisturizing cunning
The effect of the effect of intestines, lower gas row is stagnant, inducing diuresis for removing edema, be mainly used for treat intestine-dryness due to consumption of fluid, stagnation of QI due to dyspepsia, abdominal distention constipation, oedema,
Tinea pedis etc..
The brush-cherry seed product after extracting is taken in discovery after study, can reach more preferable, faster therapeutic effect, and existing
Brush-cherry seed extraction process recovery rate is not high, so that product purity is lower, both influences therapeutic effect, while also resulting in certain money
Source waste.
Summary of the invention
For solve background technique present in existing brush-cherry seed extraction process recovery rate it is not high so that product purity compared with
Low, the technical issues of both influencing therapeutic effect, while also resulting in certain wasting of resources, the present invention proposes a kind of brush-cherry seed
Extraction process, by using reduced-pressure backflow extractive technique, low temperature, low pressure guarantee the stability of brush-cherry seed；It is preliminary using shaking screen
Filtering removes brush-cherry seed bulky grain residue, then technology is filtered by vacuum using diatomite, removes insoluble substance, and to brush-cherry seed
Residue is recycled, to solve the problems mentioned in the above background technology.
A kind of extraction process of brush-cherry seed for health care proposed by the present invention, comprising the following steps:
S1, brush-cherry seed raw material is pre-processed by washing, peeling, crushing and drying process, obtains raw material powder；
S2, brush-cherry seed raw material powder is extracted using ethanol solution reflux extraction: weighs pretreated strongly fragrant Lee first
100 grams of benevolence raw material, after high temperature destroy the enzyme treatment, using the ethanol solution of 60%-80% concentration as extractant, liquid-to-solid ratio 6:1-
10:1, extraction time 0.5-3.0h, Extracting temperature are 55-80 DEG C, extract to brush-cherry seed raw material, obtain extracting solution；
S3, first filtration treatment is carried out to extracting solution using the filter membrane of 100 mesh, obtains primary filtrate, then takes diatomite mistake
Filter carries out secondary filter, last merging filtrate；
S4, using be evaporated under reduced pressure the filtered brush-cherry seed extracting solution of technical treatment, concentrate it to concentration be 30%-35%, obtain
Brush-cherry seed condensed cream, while recycling ethyl alcohol；Then brush-cherry seed condensed cream is quantitative to 100 grams；
S5, reference substance solution and each 10 μ l of test solution are drawn respectively using sample injector, liquid chromatograph is injected, with efficient liquid
Phase chromatography measures the content of amarogentin and prunuside in condensed cream, and according to production actual needs to amarogentin and strongly fragrant
Li Ren glycosides content is deployed；
S6, alcohol precipitation processing is carried out to the brush-cherry seed condensed cream after allotment: adds the ethyl alcohol that 5-7 times of concentration is 95% into condensed cream
Solution simultaneously stirs, and then handles mixed solution, mixed solution using centrifuge (revolving speed 8000-9000r/min)
There is obvious layering；
S7, the supernatant fraction for taking out mixed solution, and clear liquid is filtered using micropore filtering film；
S8, filtered brush-cherry seed clear liquid is sprayed using spray dryer, forms spraying, spraying rapid-curing cutback fast under high temperature environment
It is dry, form brush-cherry seed dry powder；Wherein 210-220 DEG C of spray drying EAT, 85-90 DEG C of leaving air temp；
S9, the reference substance solution and test solution for preparing amarogentin and prunuside respectively；It is drawn respectively using sample injector
The reference substance solution of amarogentin and prunuside and each 10 μ l of test solution inject liquid chromatograph, use high-efficient liquid phase color
Spectrometry measures the content of amarogentin and prunuside in brush-cherry seed dry powder respectively, to guarantee the up to standard of product quality；
S10, it sterilized, packed to the brush-cherry seed dry powder after up to standard, finally storage saves.
Preferably, in S1, brush-cherry seed raw material is washed first；Then 95-100 DEG C of boiling brush-cherry seed 2- is used
3min is dried after peeling with removing brush-cherry seed crust；Then raw material is handled using micronizer, obtains raw material powder；
It is dried finally, raw material powder is put into drying box, drying temperature is 50-70 DEG C, drying time 20-30h.
Preferably, in S2,100 grams of pretreated brush-cherry seed raw material is weighed first, after high temperature destroy the enzyme treatment, with
The ethanol solution of 75% concentration is extractant, and liquid-to-solid ratio 7:1, extraction time 1.5h, Extracting temperature is 65 DEG C, to brush-cherry seed
Raw material extracts, and obtains extracting solution.
Preferably, before carrying out S6, condensed cream need to be heated under the conditions of 95-100 DEG C 15-20S, then cooled down standby
With.
Preferably, in S5 and S9, using ZORBAX SB-C18 chromatographic column (4.6mm × 250mm), column temperature is 35 DEG C, inspection
Survey wavelength is 264nm, flow velocity 1.0mL/min；0.1 aqueous acetic acid of ethyl alcohol-(52:48) in mobile phase, number of theoretical plate should not
Lower than 3000.
Preferably, in S5 and S9, brush-cherry seed this 0.2-0.6g of dry powder is taken when first prepared by test solution, is then used
It is 75% ethanol solution 20ml that concentration is added into dry powder for sample injector, and weighed weight is heated to reflux 1 hour, weighed heavy again after cooling
Amount, the weight of less loss is supplied with 75% ethanol solution, is finally placed in 50ml measuring bottle, is added using micropore filtering film filtration
75% ethanol solution shakes up spare to scale.
Preferably, in S5 and S9, when prepared by the reference substance solution of amarogentin, take amarogentin reference substance appropriate, essence
Close weighed, the mixed solution that every 1ml contains 20 μ g amarogentins is made in the ethanol solution for being added 75%, shakes up spare.
Preferably, in S5 and S9, when prepared by the reference substance solution of prunuside, take prunuside reference substance appropriate, essence
It is close weighed, 75% ethanol solution is added, the mixed solution that every 1ml contains 125 μ g prunusides is made, shakes up spare.
In the present invention, during carrying out brush-cherry seed extraction, high temperature removal crust is first passed through, high temperature brush-cherry seed is thin
Cell wall is conducive to subsequent extracted；Using reduced-pressure backflow extractive technique, the vacuum degree of extraction is controlled, reduces the temperature in extraction process
Degree guarantees the stability that brush-cherry seed extracts, while energy-saving；The ethanol solution of high concentration is chosen as extractant, is effectively controlled
The growth of microorganism, avoids pollution in extraction process processed；The extracting solution after refluxing extraction is carried out just using the shaking screen of 100 mesh
Step filtering removes brush-cherry seed bulky grain residue, subsequent that technology is filtered by vacuum using diatomite, removes the insoluble object in primary filtrate
Matter, and brush-cherry seed residue is recycled, the brush-cherry seed residue after recycling is dry can be used as fats and oils processing raw material and utilize again, save
It can environmental protection；The precipitating of dissolved impurity formation in condensed cream is made by heating before alcohol precipitation processing, then chooses high concentration ethanol, it is right
Condensed cream after heat treatment carries out alcohol precipitation processing, and removal is mainly dissolved in the substance that water is slightly soluble in ethyl alcohol, and makes these substances
Polymerization generates precipitating, finally cooperation centrifugation and filtering, and removal precipitating further promotes the content of target product, improves brush-cherry seed
The quality of product.
Detailed description of the invention
Fig. 1 is the shadow that Extracting temperature proposes rate to brush-cherry seed in a kind of extraction process of brush-cherry seed for health care proposed by the present invention
Loud schematic diagram.
Fig. 2 is the shadow that extraction time proposes rate to brush-cherry seed in a kind of extraction process of brush-cherry seed for health care proposed by the present invention
Loud schematic diagram.
Fig. 3 is to extract solid-liquid ratio in a kind of extraction process of brush-cherry seed for health care proposed by the present invention to propose rate to brush-cherry seed
The structural schematic diagram of influence.
Fig. 4 is that Extractant concentration proposes rate to brush-cherry seed in a kind of extraction process of brush-cherry seed for health care proposed by the present invention
The schematic diagram of influence.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment and join
According to attached drawing, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit this hair
Bright range.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to avoid this is unnecessarily obscured
The concept of invention.
A kind of extraction process of brush-cherry seed for health care proposed by the present invention, comprising the following steps:
S1, brush-cherry seed raw material is pre-processed by washing, peeling, crushing and drying process, obtains raw material powder；
S2, brush-cherry seed raw material powder is extracted using ethanol solution reflux extraction: weighs pretreated strongly fragrant Lee first
100 grams of benevolence raw material, after high temperature destroy the enzyme treatment, using the ethanol solution of 60%-80% concentration as extractant, liquid-to-solid ratio 6:1-
10:1, extraction time 0.5-3.0h, Extracting temperature are 55-80 DEG C, extract to brush-cherry seed raw material, obtain extracting solution；
S3, first filtration treatment is carried out to extracting solution using the shaking screen of 100 mesh, obtains primary filtrate, then takes diatomite mistake
Filter carries out secondary filter, last merging filtrate；
S4, using be evaporated under reduced pressure the filtered brush-cherry seed extracting solution of technical treatment, concentrate it to concentration be 30%-35%, obtain
Brush-cherry seed condensed cream, while recycling ethyl alcohol；Then brush-cherry seed condensed cream is quantitative to 100 grams；
S5, reference substance solution and each 10 μ l of test solution are drawn respectively using sample injector, liquid chromatograph is injected, with efficient liquid
Phase chromatography measures the content of amarogentin and prunuside in condensed cream, and according to production actual needs to amarogentin and strongly fragrant
Li Ren glycosides content is deployed；
S6, alcohol precipitation processing is carried out to the brush-cherry seed condensed cream after allotment: adds the ethyl alcohol that 5-7 times of concentration is 95% into condensed cream
Solution simultaneously stirs, and then handles mixed solution, mixed solution using centrifuge (revolving speed 8000-9000r/min)
There is obvious layering；
S7, the supernatant fraction for taking out mixed solution, and clear liquid is filtered using micropore filtering film；
S8, filtered brush-cherry seed clear liquid is sprayed using spray dryer, forms spraying, spraying rapid-curing cutback fast under high temperature environment
It is dry, form brush-cherry seed dry powder；Wherein 210-220 DEG C of spray drying EAT, 85-90 DEG C of leaving air temp；
S9, the reference substance solution and test solution for preparing amarogentin and prunuside respectively；It is drawn respectively using sample injector
The reference substance solution of amarogentin and prunuside and each 10 μ l of test solution inject liquid chromatograph, use high-efficient liquid phase color
Spectrometry measures the content of amarogentin and prunuside in brush-cherry seed dry powder respectively, to guarantee the up to standard of product quality；
S10, it sterilized, packed to the brush-cherry seed dry powder after up to standard, finally storage saves.
In S1, brush-cherry seed raw material is washed first；Then 95-100 DEG C of boiling brush-cherry seed 2-3min is used, to remove
Brush-cherry seed crust is dried after peeling；Then raw material is handled using micronizer, obtains raw material powder；Finally, by raw material
Powder is put into drying box and is dried, and drying temperature is 50-70 DEG C, drying time 20-30h.
Before carrying out S6, condensed cream need to be heated under the conditions of 95-100 DEG C 15-20S, then cooled down spare.
In S5 and S9, using ZORBAX SB-C18 chromatographic column (4.6mm × 250mm), column temperature is 35 DEG C, Detection wavelength
For 264nm, flow velocity 1.0mL/min；0.1 aqueous acetic acid of ethyl alcohol-(52:48), number of theoretical plate should be not less than in mobile phase
3000。
In S5 and S9, brush-cherry seed this 0.2-0.6g of dry powder is taken when first prepared by test solution, then uses sample injector
It is 75% ethanol solution 20ml that concentration is added into dry powder, and weighed weight is heated to reflux 1 hour, it is cooling after weighed weight again, use
75% ethanol solution supplies the weight of less loss, is finally placed in 50ml measuring bottle using micropore filtering film filtration, 75% second is added
Alcoholic solution shakes up spare to scale.
In S5 and S9, when prepared by the reference substance solution of amarogentin, take amarogentin reference substance appropriate, it is accurately weighed,
The mixed solution that every 1ml contains 20 μ g amarogentins is made in the ethanol solution for being added 75%, shakes up spare.
In S5 and S9, when prepared by the reference substance solution of prunuside, take prunuside reference substance appropriate, it is accurately weighed,
75% ethanol solution is added, the mixed solution that every 1ml contains 125 μ g prunusides is made, shakes up spare.
During carrying out brush-cherry seed extraction, high temperature removal crust is first passed through, high temperature brush-cherry seed cell wall is conducive to
Subsequent extracted；Using reduced-pressure backflow extractive technique, the vacuum degree of extraction is controlled, reduces the temperature in extraction process, is guaranteed strongly fragrant
The stability that Li Ren is extracted, at the same it is energy-saving；The ethanol solution of high concentration is chosen as extractant, effectively control extraction process
The growth of middle microorganism, avoids pollution；Primary filtration is carried out to the extracting solution after refluxing extraction using the shaking screen of 100 mesh, is gone
It is subsequent that technology is filtered by vacuum using diatomite except brush-cherry seed bulky grain residue, the insoluble substance in primary filtrate is removed, and to strongly fragrant
Li Ren residue is recycled, and the brush-cherry seed residue after recycling is dry can be used as fats and oils processing raw material and utilize again, energy conservation and environmental protection；Alcohol
Processing of sinking is preceding to make the precipitating of dissolved impurity formation in condensed cream by heating, high concentration ethanol is then chosen, to heat treatment
Condensed cream afterwards carries out alcohol precipitation processing, and removal is mainly dissolved in the substance that water is slightly soluble in ethyl alcohol, and generates these polymerizations
Precipitating, finally cooperation centrifugation and filtering, removal precipitating further promote the content of target product, improve the product of brush-cherry seed product
Matter.
A kind of extraction process of brush-cherry seed for health care proposed by the present invention, comprising the following steps:
S1, brush-cherry seed raw material is pre-processed by washing, peeling, crushing and drying process, obtains raw material powder；
S2, brush-cherry seed raw material powder is extracted using ethanol solution reflux extraction: weighs pretreated strongly fragrant Lee first
100 grams of benevolence raw material, after high temperature destroy the enzyme treatment, using the ethanol solution of 75% concentration as extractant, liquid-to-solid ratio 7:1, when extraction
Between be 1.5h, Extracting temperature be 65 DEG C, brush-cherry seed raw material is extracted, extracting solution is obtained；
S3, first filtration treatment is carried out to extracting solution using the filter membrane of 100 mesh, obtains primary filtrate, then takes diatomite mistake
Filter carries out secondary filter, last merging filtrate；
S4, using be evaporated under reduced pressure the filtered brush-cherry seed extracting solution of technical treatment, concentrate it to concentration be 30%-35%, obtain
Brush-cherry seed condensed cream, while recycling ethyl alcohol；Then brush-cherry seed condensed cream is quantitative to 100 grams；
S5, reference substance solution and each 10 μ l of test solution are drawn respectively using sample injector, liquid chromatograph is injected, with efficient liquid
Phase chromatography measures the content of amarogentin and prunuside in condensed cream, and according to production actual needs to amarogentin and strongly fragrant
Li Ren glycosides content is deployed；
S6, alcohol precipitation processing is carried out to the brush-cherry seed condensed cream after allotment: adds the ethyl alcohol that 5-7 times of concentration is 95% into condensed cream
Solution simultaneously stirs, and then handles mixed solution, mixed solution using centrifuge (revolving speed 8000-9000r/min)
There is obvious layering；
S7, the supernatant fraction for taking out mixed solution, and clear liquid is filtered using micropore filtering film；
S8, filtered brush-cherry seed clear liquid is sprayed using spray dryer, forms spraying, spraying rapid-curing cutback fast under high temperature environment
It is dry, form brush-cherry seed dry powder；Wherein 210-220 DEG C of spray drying EAT, 85-90 DEG C of leaving air temp；
S9, the reference substance solution and test solution for preparing amarogentin and prunuside respectively；It is drawn respectively using sample injector
The reference substance solution of amarogentin and prunuside and each 10 μ l of test solution inject liquid chromatograph, use high-efficient liquid phase color
Spectrometry measures the content of amarogentin and prunuside in brush-cherry seed dry powder respectively, to guarantee the up to standard of product quality；
S10, it sterilized, packed to the brush-cherry seed dry powder after up to standard, finally storage saves.
In S1, brush-cherry seed raw material is washed first；Then 95-100 DEG C of boiling brush-cherry seed 2-3min is used, to remove
Brush-cherry seed crust is dried after peeling；Then raw material is handled using micronizer, obtains raw material powder；Finally, by raw material
Powder is put into drying box and is dried, and drying temperature is 50-70 DEG C, drying time 20-30h.
Before carrying out S6, condensed cream need to be heated under the conditions of 95-100 DEG C 15-20S, then cooled down spare.
In S5 and S9, using ZORBAX SB-C18 chromatographic column (4.6mm × 250mm), column temperature is 35 DEG C, Detection wavelength
For 264nm, flow velocity 1.0mL/min；0.1 aqueous acetic acid of ethyl alcohol-(52:48), number of theoretical plate should be not less than in mobile phase
3000。
In S5 and S9, brush-cherry seed this 0.2-0.6g of dry powder is taken when first prepared by test solution, then uses sample injector
It is 75% ethanol solution 20ml that concentration is added into dry powder, and weighed weight is heated to reflux 1 hour, it is cooling after weighed weight again, use
75% ethanol solution supplies the weight of less loss, is finally placed in 50ml measuring bottle using micropore filtering film filtration, 75% second is added
Alcoholic solution shakes up spare to scale.
In S5 and S9, when prepared by the reference substance solution of amarogentin, take amarogentin reference substance appropriate, it is accurately weighed,
The mixed solution that every 1ml contains 20 μ g amarogentins is made in the ethanol solution for being added 75%, shakes up spare.
In S5 and S9, when prepared by the reference substance solution of prunuside, take prunuside reference substance appropriate, it is accurately weighed,
75% ethanol solution is added, the mixed solution that every 1ml contains 125 μ g prunusides is made, shakes up spare.
The influence that Extracting temperature proposes rate to brush-cherry seed is tested, as shown in Figure 1.
Experimental procedure: 6 groups of 100 grams of pretreated brush-cherry seeds are weighed, after high temperature destroy the enzyme treatment, with concentration 65%
Ethanol solution is extractant, and liquid-to-solid ratio 7:1,6 groups of Extracting temperature is respectively 55 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 75 DEG C and 80
DEG C, it extracts at 1.5h, then filters, merging filtrate is suitably concentrated quantitative extremely with 65% ethanol solution again after filtrate
100 grams, take the concentrate, by high performance liquid chromatography measure 6 groups of concentrates in amarogentin and prunuside content, every group
Replication 3 times.
Analysis of experimental results: experimental result is shown in Fig. 1 for influence of the different Extracting temperatures to brush-cherry seed recovery rate, as shown in Figure 1,
When Extracting temperature is less than 75 DEG C, prunuside content gradually increases as the temperature rises, and 75 DEG C of whens reach maximum, and to hardship
The extraction of almond glycosides is then the maximum at 65 DEG C, and as Extracting temperature increases, the recovery rate of amarogentin starts when more than 65 DEG C
Reduce, when more than 75 DEG C the recovery rate of prunuside start the reason of reducing, generating this kind of phenomenon be Extracting temperature it is excessively high, wait mention
Taking the stability of ingredient reduces.
Experiment conclusion: comprehensive production cost and product quality consider, selected in actual production 65 DEG C for optimum extraction temperature
Degree.
The influence that extraction time proposes rate to brush-cherry seed is tested, as shown in Figure 2.
Experimental procedure: weighing 16 groups of 100 grams of pretreated brush-cherry seeds, after high temperature destroy the enzyme treatment, with concentration 65%
Ethanol solution be extractant, liquid-to-solid ratio 7:1,65 DEG C of Extracting temperature, 6 groups of extraction time is respectively 0.5,1.0,1.5,
2.0,2.5 and 3.0h, is then filtered, merging filtrate, appropriate to be concentrated after filtrate again with 65% ethanol solution quantitatively to 100 grams, is taken
The concentrate measures the content of amarogentin and prunuside in 6 groups of concentrates, every group of replication by high performance liquid chromatography
3 times.
Analysis of experimental results: experimental result is shown in Fig. 2 for influence of the different extraction times to brush-cherry seed recovery rate, as shown in Figure 2,
Extraction time is less than 1.5h, and the recovery rate of two main components is gradually increased with the extension of extraction time, when extracting 1.5h
Recovery rate reaches maximum, and when extraction time is greater than 1.5h, the recovery rates of two main components is basic with the extension of extraction time
Change unobvious.
Experiment conclusion: consider save the cost, reduce energy consumption, shorten the production cycle, select in actual production 1.5 h for
The optimum extraction time.
It extracts the influence that solid-liquid ratio proposes rate to brush-cherry seed to test, as shown in Figure 3.
Experimental procedure: 6 groups of 100 grams of pretreated brush-cherry seeds are weighed, after high temperature destroy the enzyme treatment, with concentration 65%
Ethanol solution is extractant, and 6 groups of liquid-to-solid ratios are respectively 5:1,6:1,7:1,8:1,9:1,10:1,65 DEG C of Extracting temperature, when extraction
Between be respectively 1.5h, then filter, merging filtrate, appropriate be concentrated after filtrate is quantified with 65% ethanol solution to 100 grams again, is taken
The concentrate measures the content of amarogentin and prunuside in 6 groups of concentrates, every group of replication by high performance liquid chromatography
3 times.
Analysis of experimental results: difference extracts influence of the solid-liquid ratio to brush-cherry seed recovery rate, and experimental result is shown in Fig. 3, can by Fig. 3
Know, with the increase of liquid-to-solid ratio, two kinds of main component recovery rates of brush-cherry seed are gradually increased, and are reached most when solid-liquid ratio is 7:1
Big value, after solid-liquid ratio is more than 7:1, two kinds of main component recovery rates variation of brush-cherry seed is relatively delayed.
Experiment conclusion: liquid-to-solid ratio is bigger, and longer the time required to the concentration of later period extract, cost is higher, in actual production
Select 7:1 for optimum extraction solid-liquid ratio.
The influence that Extractant concentration proposes rate to brush-cherry seed is tested, as shown in Figure 4.
Experimental procedure: 6 groups of 100 grams of pretreated brush-cherry seeds are weighed, after high temperature destroy the enzyme treatment, 6 groups respectively with dense
Degree is extractant for 60%, 65%, 70%, 75% and 80% ethanol solution, liquid-to-solid ratio 7:1,65 DEG C of Extracting temperature, extraction time
Respectively 1.5h is then filtered, merging filtrate, appropriate to be concentrated after filtrate again with the ethanol solution of same concentrations quantitatively to 100 grams,
The concentrate is taken, the content of amarogentin and prunuside in 6 groups of concentrates is measured by high performance liquid chromatography, every group repeats to survey
It is 3 times fixed.
Analysis of experimental results: experimental result is shown in Fig. 4 for influence of the different Extractant concentrations to brush-cherry seed recovery rate, can by Fig. 4
Know, with the increase of concentration of alcohol, the recovery rate of amarogentin is gradually increased, after ethanol solution concentration is greater than 75%, amarogentin
Recovery rate be held essentially constant, and the recovery rate of prunuside is gradually reduced with the increase of ethanol solution concentration.
Experiment conclusion: comprehensively considering production cost and recovery rate, selects in actual production 65% dense for optimum extraction agent
Degree.
It should be understood that above-mentioned specific embodiment of the invention is used only for exemplary illustration or explains of the invention
Principle, but not to limit the present invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into attached claim scope and boundary or this range and the equivalent form on boundary and is repairing
Change example.
Claims (8)
1. a kind of extraction process of brush-cherry seed for health care, which comprises the following steps:
S1, brush-cherry seed raw material is pre-processed by washing, peeling, crushing and drying process, obtains raw material powder；
S2, brush-cherry seed raw material powder is extracted using ethanol solution reflux extraction: weighs pretreated strongly fragrant Lee first
100 grams of benevolence raw material, after high temperature destroy the enzyme treatment, using the ethanol solution of 60%-80% concentration as extractant, liquid-to-solid ratio 6:1-
10:1, extraction time 0.5-3.0h, Extracting temperature are 55-80 DEG C, extract to brush-cherry seed raw material, obtain extracting solution；
S3, first filtration treatment is carried out to extracting solution using the filter membrane of 100 mesh, obtains primary filtrate, then takes diatomite mistake
Filter carries out secondary filter, last merging filtrate；
S4, using be evaporated under reduced pressure the filtered brush-cherry seed extracting solution of technical treatment, concentrate it to concentration be 30%-35%, obtain
Brush-cherry seed condensed cream, while recycling ethyl alcohol；Then brush-cherry seed condensed cream is quantitative to 100 grams；
S5, reference substance solution and each 10 μ l of test solution are drawn respectively using sample injector, liquid chromatograph is injected, with efficient liquid
Phase chromatography measures the content of amarogentin and prunuside in condensed cream, and according to production actual needs to amarogentin and strongly fragrant
Li Ren glycosides content is deployed；
S6, alcohol precipitation processing is carried out to the brush-cherry seed condensed cream after allotment: adds the ethyl alcohol that 5-7 times of concentration is 95% into condensed cream
Solution simultaneously stirs, and then handles mixed solution, mixed solution using centrifuge (revolving speed 8000-9000r/min)
There is obvious layering；
S7, the supernatant fraction for taking out mixed solution, and clear liquid is filtered using micropore filtering film；
S8, filtered brush-cherry seed clear liquid is sprayed using spray dryer, forms spraying, spraying rapid-curing cutback fast under high temperature environment
It is dry, form brush-cherry seed dry powder；Wherein 210-220 DEG C of spray drying EAT, 85-90 DEG C of leaving air temp；
S9, the reference substance solution and test solution for preparing amarogentin and prunuside respectively；It is drawn respectively using sample injector
The reference substance solution of amarogentin and prunuside and each 10 μ l of test solution inject liquid chromatograph, use high-efficient liquid phase color
Spectrometry measures the content of amarogentin and prunuside in brush-cherry seed dry powder respectively, to guarantee the up to standard of product quality；
S10, it sterilized, packed to the brush-cherry seed dry powder after up to standard, finally storage saves.
2. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that right first in S1
Brush-cherry seed raw material is washed；Then 95-100 DEG C of boiling brush-cherry seed 2-3min is used, to remove brush-cherry seed crust, by it after peeling
It dries；Then raw material is handled using micronizer, obtains raw material powder；Finally, raw material powder is put into drying box dry
Processing, drying temperature are 50-70 DEG C, drying time 20-30h.
3. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that in S2, claim first
100 grams of pretreated brush-cherry seed raw material is taken, after high temperature destroy the enzyme treatment, using the ethanol solution of 75% concentration as extractant, liquid
Material is than being 7:1, and extraction time 1.5h, Extracting temperature is 65 DEG C, extracts to brush-cherry seed raw material, obtains extracting solution.
4. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that before carrying out S6,
Condensed cream need to be heated under the conditions of 95-100 DEG C 15-20S, then cooled down spare.
5. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that in S5 and S9, adopt
With ZORBAX SB-C18 chromatographic column (4.6mm × 250mm), column temperature is 35 DEG C, Detection wavelength 264nm, flow velocity 1.0mL/
min；0.1 aqueous acetic acid of ethyl alcohol-(52:48) in mobile phase, number of theoretical plate should be not less than 3000.
6. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that first in S5 and S9
First test solution takes brush-cherry seed this 0.2-0.6g of dry powder when preparing, and it is 75% that concentration is then added into dry powder using sample injector
Ethanol solution 20ml, weighed weight are heated to reflux 1 hour, it is cooling after weighed weight again, supply less loss with 75% ethanol solution
Weight, finally using micropore filtering film filtration be placed in 50ml measuring bottle, be added 75% ethanol solution to scale, shake up spare.
7. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that bitter in S5 and S9
When the reference substance solution preparation of almond glycosides, take amarogentin reference substance appropriate, it is accurately weighed, 75% ethanol solution is added and is made
Every 1ml contains the mixed solution of 20 μ g amarogentins, shakes up spare.
8. a kind of extraction process of brush-cherry seed for health care according to claim 1, which is characterized in that strongly fragrant in S5 and S9
When the reference substance solution preparation of Li Ren glycosides, take prunuside reference substance appropriate, it is accurately weighed, 75% ethanol solution is added and is made often
1ml contains the mixed solution of 125 μ g prunusides, shakes up spare.
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| CN102000066A (en) * | 2010-09-26 | 2011-04-06 | 中国科学院昆明植物研究所 | Inula helianthus-aquatica extract, anti-tumor medicament using same as active ingredient, preparation method and application thereof |
| CN109276634A (en) * | 2018-11-30 | 2019-01-29 | 广东康之辰药物研发有限公司 | A kind of Chinese medicine composition of relax bowel and defecation and preparation method thereof |
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