CN107602642A - A kind of method of the extraction purification tracheloside from kardiseed - Google Patents
A kind of method of the extraction purification tracheloside from kardiseed Download PDFInfo
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- CN107602642A CN107602642A CN201710952856.2A CN201710952856A CN107602642A CN 107602642 A CN107602642 A CN 107602642A CN 201710952856 A CN201710952856 A CN 201710952856A CN 107602642 A CN107602642 A CN 107602642A
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- tracheloside
- kardiseed
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Abstract
The present invention provides a kind of method of the extraction purification tracheloside from kardiseed, mainly solves the problems, such as that yield is low in the prior art, is not suitable for industrialized production and complex process.This method mainly includes the following steps that:The safflower seed meal obtained after first raw material kardiseed is extracted oil crushes, and is extracted using ethanol;Extract solution is concentrated again, decolourized, filtering, filtrate is purified with resin anion (R.A.), collects absorption efflux;Then using salt acid for adjusting pH to 35, filtering, organic extractant solution is added into filtrate, concentrated, place crystallization, filtering, dry coarse crystallization;Finally coarse crystallization is crushed, using ethanol stirring and dissolving, filtering, precipitation is collected, is drying to obtain tracheloside.It is of the invention effectively to utilize the residual dregs of rice obtained after kardiseed oil expression, therefrom isolate and purify to obtain tracheloside, turn waste into wealth, be comprehensively utilized resource, reduce the cost of expense of raw materials;Whole technique is simple, easy to operate, high income, steady quality.
Description
Technical field
The invention belongs to extraction purification technical field, and in particular to a kind of side of the extraction purification tracheloside from kardiseed
Method.
Background technology
Safflower also known as safflower, chrysanthemum safflower, red orchid, Flos Carthami etc., it is annual dicotyledonous catananche.Safflower
Seed is derived from the seed of safflower, small compared with sunflower seeds, and Chinese medicine is entitled " SEMEN CARTHAMI ".Kardiseed oil-containing 25%-37%, containing crude protein
15%-19%, benevolence oil-containing is up to more than 55%.Essential fatty acid content is especially sub- up to more than 80% in safflower seed oil
Oleic acid is one of two kinds of essential fatty acids, and it has obtained more and more wider to the importance for improving health in medical field
General accreditation.There is the good reputation of " blood vessel scavenger ", the work for having prevention of arterial atherosis, hypercholesterolemia and hyperlipidemia
With.
Past research is concentrated mainly on safflower seed oil, and safflower seed meal so causes generally as cheap feed and fertilizer
A large amount of wastes of resource.Research finds, containing abundant tracheloside in safflower seed meal, there is antagonism, anti-hypertension, blood platelet
The effect of agglutination inhibitor.Therefore, the extraction separation tracheloside from safflower seed meal, turns waste into wealth, resource is obtained sufficient profit
With having far-reaching significance.
At present, tracheloside is mainly derived from caulis trachelospermi.For example disclosed in patent CN100577677C a kind of from caulis trachelospermi
The method of middle extraction lignanoid, raw material are extracted using 95% alcohol reflux, are concentrated to give extract, then molten using 95% ethanol
Solution, adds diatomite to mix thoroughly, petroleum ether degreasing, and residue is extracted with 95% ethanol again, macroreticular resin separation, first with 10% ethanol elution
Removal of impurities, then obtain total lignan with 95% ethanol elution.The patent is separated by macroreticular resin, is united with 95% ethanol and is brushed parsing,
Fail tracheloside being collected separately, therefore what is obtained is total lignanoid, and comparision contents are low.
Document " S.NISHIBE, A.&SAKUSHIMA, S.TRACHELOSIDE FROM THE SEEDS OF
CARTHAMUS TINCTORIUS [J] .Phytochemistr1y, one kind is disclosed in 1972,11,2629. " from kardiseed
The method of extraction separation tracheloside, safflower seed raw material crush, petroleum ether, ethanol heating extraction, concentrate ethanol extract, add
Water dilutes, and chloroform extraction, water layer is condensed into medicinal extract, and ethyl acetate dissolves by heating, silica gel column chromatography, chloroform-ethanol (8:2) parse
Obtain tracheloside.The technique is too complicated, and by silica gel column chromatography, cost is too big, is unfavorable for industrialized production.Using chloroform,
The reagents such as petroleum ether, ethyl acetate, are unfavorable for health and environmental protection.
The content of the invention
The shortcomings that the present invention seeks to overcome above-mentioned prior art and provide one kind from kardiseed extraction purification tracheloside
Method, this method high income, be adapted to industrialized production, and technique is simple, cost is relatively low.
The technical scheme is that:
The method of the extraction purification tracheloside from kardiseed, comprises the following steps:
Step 1 is extracted
The safflower seed meal obtained after raw material kardiseed is extracted oil crushes, and is extracted using ethanol, obtains extract solution;
Step 2 concentrates, decolourized
Extract solution obtained by step 1 is concentrated, decolourized, filtering, obtains filtrate;
Step 3 purifies
Step 2 gained filtrate is purified with resin anion (R.A.), collects absorption efflux;
Step 4 prepares crude product
By the absorption efflux obtained by step 3, using salt acid for adjusting pH to 3-5, filtering, organic solution is added into filtrate
Extraction, concentration, place crystallization, filtering, dry coarse crystallization;
Step 5 prepares fine work
Coarse crystallization obtained by step 4 is crushed, using ethanol stirring and dissolving, filtering, precipitation is collected, is drying to obtain trachelospermum jasminoide
Glycosides.
Further, the preferred scheme of above-mentioned steps 1 is:The safflower seed meal obtained after raw material kardiseed is extracted oil is crushed to
100 mesh, under the conditions of 40 DEG C, use 6 times of amounts of material quality and mass concentration is extracted twice for 90%-95% ethanol, merge
Extract solution.
Further, the preferred scheme of above-mentioned steps 2 is:Extract solution obtained by step 1 is concentrated into the 1.03- of proportion
1.05, decolourized under the conditions of 70 DEG C, filter, obtain filtrate;The decolouring is the activated carbon and raw material using material quality 5%-8%
Quality 3%-5% atlapulgite processing.
Further, above-mentioned activated carbon is using one or more combinations in model 767,320,303, HB-F.
Further, resin anion (R.A.) model LX-T5, D958 or WZ-D814 in above-mentioned steps 3;Resin anion (R.A.)
The ratio of volume and the quality of raw material is 1:3-5.
Further, the preferred scheme of above-mentioned steps 4 is:Absorption efflux obtained by step 3 is used into salt acid for adjusting pH extremely
3-5, filtering, equimultiple organic extractant solution is added into filtrate, concentration, places crystallization, filtering, dry coarse crystallization;It is described
Organic solution is the mixed solution of n-butanol and ethanol, wherein, the volume ratio of n-butanol and ethanol is 7-12:1.
Further, the volume ratio of n-butanol and ethanol is 10 in above-mentioned steps 4:1.
Further, the preferred scheme of above-mentioned steps 5 is:Coarse crystallization obtained by step 4 is crushed to 80 mesh, it is dense using quality
The ethanol stirring and dissolving for 80%-90% is spent, is filtered, precipitation is collected, is drying to obtain tracheloside.
It is an advantage of the invention that:
1. of the invention effectively using the residual dregs of rice obtained after kardiseed oil expression, therefrom isolate and purify to obtain tracheloside, change give up into
Treasured, resource is comprehensively utilized, reduces the cost of expense of raw materials.
2. the present invention first extracts oil raw material, safflower seed oil is both obtained, is eliminated largely for the purifying of follow-up tracheloside again
Liposoluble constituent, then extracted using 90-95% ethanol low temperature, the impurity such as substantial amounts of protein, polysaccharide are removed, then pass through work again
Property charcoal and atlapulgite remove pigment impurity and the liposoluble constituent etc. of residual, for tracheloside be further purified laid it is good
Good basis.
3 present invention can further be inhaled using being purified to resin anion (R.A.) of the tracheloside without adsorptivity by resin
Attached a large amount of impurity, and to tracheloside substantially without adsorptivity, so as to reach the purifying to tracheloside, the resin is with strong points, operation
Simply, cycle period is improved.
4. the present invention in acid condition using tracheloside it is with strong points mix reagent extraction, effective component extracting it is same
When greatly eliminate impurity similar in property;The crystallization obtained after concentration, cleaned using a small amount of hydrous ethanol stirring at normal temperature,
Reduce by recrystallizing the loss of effective components brought.
5. the technique of the present invention is simple, easy to operate, high income, steady quality.
6. the present invention using reagents such as chloroform, petroleum ether, ethyl acetate, will not brought to health and environmental protection
Adverse effect.
Embodiment
Embodiment 1
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 90% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of 320 activated carbon 2.5Kg and atlapulgite 1.5Kg are added, are filtered, filtrate is with 16.7Kg LX-T5 anion trees
Fat purifies, and collects absorption efflux, and with salt acid for adjusting pH to 3-5, filtering, filtrate adds the mixing of isometric n-butanol and ethanol
(volume ratio of n-butanol and ethanol is 9 to solution:1) extract 2 times, merge butanol extraction liquid, be concentrated into 1250ml, place analysis
It is brilliant.Filtration drying obtains coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 200ml 80%,
Filtering, common 203g after precipitation is dried, liquid phase detection level 98.2%, the active ingredient rate of recovery 88.5%.
Embodiment 2
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 90% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of 767 activated carbon 4Kg and atlapulgite 2.5Kg are added, are filtered, filtrate is pure with 10Kg D958 resin anion (R.A.)s
Change, collect absorption efflux, with salt acid for adjusting pH to 3-5, filtering, filtrate adds the mixed solution of isometric n-butanol and ethanol
(volume ratio of n-butanol and ethanol is 7:1) extract 2 times, merge butanol extraction liquid, be concentrated into 750ml, place crystallization.Filtering
It is dried to obtain coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 100ml 90%, is filtered, is sunk
Form sediment common 195g after drying, liquid phase detection level 98.6%, the active ingredient rate of recovery 85.5%.
Embodiment 3
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 90% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of HB-F activated carbons 3Kg and atlapulgite 2Kg are added, filtering, filtrate is with 12.5Kg WZ-D814 resin anion (R.A.)s
Purifying, absorption efflux is collected, with salt acid for adjusting pH to 3-5, filtering, the mixing that filtrate adds isometric n-butanol and ethanol is molten
(volume ratio of n-butanol and ethanol is 8 to liquid:1) extract 2 times, merge butanol extraction liquid, be concentrated into 1000ml, place crystallization.
Filtration drying obtains coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 160ml 85%, mistake
Filter, common 197g after precipitation is dried, liquid phase detection level 98.3%, the active ingredient rate of recovery 86.1%.
Embodiment 4
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 95% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of 320 activated carbon 3.5Kg and atlapulgite 1.75Kg are added, are filtered, filtrate is with 12.5Kg LX-T5 anion trees
Fat purifies, and collects absorption efflux, and with salt acid for adjusting pH to 3-5, filtering, filtrate adds the mixing of isometric n-butanol and ethanol
(volume ratio of n-butanol and ethanol is 10 to solution:1) extract 2 times, merge butanol extraction liquid, be concentrated into 900ml, place analysis
It is brilliant.Filtration drying obtains coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 150ml 85%,
Filtering, common 202g after precipitation is dried, liquid phase detection level 99.2%, the active ingredient rate of recovery 89.1%.
Embodiment 5
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 95% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of 303 activated carbon 3.25Kg and atlapulgite 2.25Kg are added, are filtered, filtrate is with 12.5Kg D958 anion trees
Fat purifies, and collects absorption efflux, with salt acid for adjusting pH to 3-5, filtering, the isometric extracting n-butyl alcohol of filtrate addition 2 times, merges
(volume ratio of n-butanol and ethanol is 11 to the mixed solution of n-butanol and ethanol:1) extract, 800ml is concentrated into, places analysis
It is brilliant.Filtration drying obtains coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 120ml 80%,
Filtering, common 198g after precipitation is dried, liquid phase detection level 98.7%, the active ingredient rate of recovery 86.9%.
Embodiment 6
Safflower seed raw material 50Kg, low temperature oil expression is first passed through, obtain 10Kg and clarify bright safflower seed oil.Obtained after oil expression
The residual dregs of rice are crushed to 100 mesh, add 40 DEG C of 95% ethanol of 235Kg and extract 2 times, merge extract solution, be concentrated into proportion 1.03-1.05,
70 DEG C of decolouring 1h of 767 activated carbon 3.75Kg and atlapulgite 2Kg are added, are filtered, filtrate is with 12.5Kg WZ-D814 anion trees
Fat purifies, and collects absorption efflux, and with salt acid for adjusting pH to 3-5, filtering, filtrate adds the mixing of isometric n-butanol and ethanol
(volume ratio of n-butanol and ethanol is 12 to solution:1) extract 2 times, merge butanol extraction liquid, be concentrated into 1100ml, place analysis
It is brilliant.Filtration drying obtains coarse crystallization.Coarse crystallization is crushed to 80 mesh, adds the alcohol at normal temperature stirring and dissolving 30min of 120ml 90%,
Filtering, common 194g after precipitation is dried, liquid phase detection level 98.7%, the active ingredient rate of recovery 85.1%.
Claims (8)
- A kind of 1. method of the extraction purification tracheloside from kardiseed, it is characterised in that comprise the following steps:Step 1 is extractedThe safflower seed meal obtained after raw material kardiseed is extracted oil crushes, and is extracted using ethanol, obtains extract solution;Step 2 concentrates, decolourizedExtract solution obtained by step 1 is concentrated, decolourized, filtering, obtains filtrate;Step 3 purifiesStep 2 gained filtrate is purified with resin anion (R.A.), collects absorption efflux;Step 4 prepares crude productBy the absorption efflux obtained by step 3, using salt acid for adjusting pH to 3-5, filtering, organic solution extraction is added into filtrate Take, concentrate, place crystallization, filtering, dry coarse crystallization;Step 5 prepares fine workCoarse crystallization obtained by step 4 is crushed, using ethanol stirring and dissolving, filtering, precipitation is collected, is drying to obtain tracheloside.
- 2. the method for the extraction purification tracheloside according to claim 1 from kardiseed, it is characterised in that the step 1 It is:The safflower seed meal obtained after raw material kardiseed is extracted oil is crushed to 100 mesh, under the conditions of 40 DEG C, using 6 times of amounts of material quality And the ethanol extraction that mass concentration is 90%-95% is twice, merges extract solution.
- 3. the method for the extraction purification tracheloside according to claim 2 from kardiseed, it is characterised in that the step 2 It is:Extract solution obtained by step 1 is concentrated into the 1.03-1.05 of proportion, decolourized under the conditions of 70 DEG C, filters, obtains filtrate;It is described Decolouring is the atlapulgite processing using material quality 5%-8% activated carbon and material quality 3%-5%.
- 4. the method for the extraction purification tracheloside according to claim 3 from kardiseed, it is characterised in that:The activated carbon Using one or more combinations in model 767,320,303, HB-F.
- 5. the method for the extraction purification tracheloside according to claim 1 from kardiseed, it is characterised in that the step 3 In resin anion (R.A.) model LX-T5, D958 or WZ-D814;The ratio of resin anion (R.A.) volume and material quality is 1:3-5.
- 6. the method for the extraction purification tracheloside according to any one of claims 1 to 5 from kardiseed, it is characterised in that institute Stating step 4 is:By the absorption efflux obtained by step 3 using salt acid for adjusting pH to 3-5, filtering, equimultiple is added into filtrate Organic extractant solution, concentration, place crystallization, filtering, dry coarse crystallization;The organic solution is the mixing of n-butanol and ethanol Solution, wherein, the volume ratio of n-butanol and ethanol is 7-12:1.
- 7. the method for the extraction purification tracheloside according to claim 6 from kardiseed, it is characterised in that:The step 4 The volume ratio of middle n-butanol and ethanol is 10:1.
- 8. the method for the extraction purification tracheloside according to claim 1 from kardiseed, it is characterised in that the step 5 It is:Coarse crystallization obtained by step 4 is crushed to 80 mesh, uses ethanol stirring and dissolving of the mass concentration for 80%-90%, is filtered, Precipitation is collected, is drying to obtain tracheloside.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114748492A (en) * | 2022-05-13 | 2022-07-15 | 山东大学齐鲁医院(青岛) | Medicine for treating atherosclerosis |
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2017
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114748492A (en) * | 2022-05-13 | 2022-07-15 | 山东大学齐鲁医院(青岛) | Medicine for treating atherosclerosis |
CN114748492B (en) * | 2022-05-13 | 2023-03-10 | 山东大学齐鲁医院(青岛) | Medicine for treating atherosclerosis |
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