CN110156847A - A kind of extracting method of crocin - Google Patents
A kind of extracting method of crocin Download PDFInfo
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- CN110156847A CN110156847A CN201910398366.1A CN201910398366A CN110156847A CN 110156847 A CN110156847 A CN 110156847A CN 201910398366 A CN201910398366 A CN 201910398366A CN 110156847 A CN110156847 A CN 110156847A
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- filtrate
- crocin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
- C07H13/04—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids having the esterifying carboxyl radicals attached to acyclic carbon atoms
- C07H13/06—Fatty acids
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- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of extracting methods of crocin: taking west safflower powder to be dissolved in hot water, dynamic agitation is extracted, and centrifugation takes supernatant to be filtered using glass funnel, collects filtrate；1/5-1/8 times of volume is concentrated the filtrate to, upper large pore resin absorption column separation is first eluted with water removal impurity, then is eluted with volumetric concentration 70-80% ethanol water, collects ethanol eluate；The ethanol eluate of collection is heated to 65 DEG C, adds active carbon decoloring, is filtered, filtrate is further concentrated to no alcohol, then plus acetic acid ethyl ester crystallization, filtering crystal is dry to get crocin.Using extracting method extract output capacity height of the invention up to 7.3%, purity is up to 90%.And construction is low with production investment, easy to operate, and extracting method of the invention is easy to promote and utilize.
Description
Background technique
Crocin is more stable in the natural pigment of yellow system, has fast light, heat-resisting, resistance to metal ion and resistance to
The features such as chemicals, tone variations are not influenced substantially by pH, especially for protein, starch, also have excellent dye
Therefore color has use in terms of the various food based on noodles, cake, candy chestnut.The product are highly-safe, to small
White mouse carries out acute toxicity test, and oral 15g/kg is also without dead example.Subchronic toxicity is carried out with the feed of addition this pigment 2%
Test, as a result also without any exception, this dosage such as converts by human body (in terms of 50kg), is equivalent to and absorbs 200g for each person every day.
Therefore it may be considered under usually using concentration completely harmless.The country to Gardenia Yellow for candy, biscuit, egg roll,
Orange juice, carbonated drink, cold drink, fruit wine are carried out using test, and effect is preferable.But there is micro, extraction in crocin in nature
Enriching step is cumbersome.
Extracting the common method of crocin in the prior art has alcohol solution reflux extraction, supercritical fluid extraction
Method, membrane separation process etc., although these prior arts have attempted a variety of different extractions and purification process, some method and processes are multiple
It is miscellaneous, the special or complicated equipment of some need, but since these prior arts can not completely destroy the constraint of cell wall, most
Effective component is extracted to limits, and sufficiently rationally separation is carried out to active principle, thus products obtained therefrom purity is not high, also not
Easy large-scale production.For this purpose, it is proposed that a kind of extracting method of new crocin.
Summary of the invention
The main purpose of the present invention is to provide a kind of extracting methods of crocin, can effectively solve in background technique
The problem of.
The technical scheme adopted by the invention is as follows:
The present invention provides a kind of extracting method of crocin, and the method is using Chinese medicine west safflower as starting material, packet
Include crushing, extraction, centrifuge separation, elution and purification step, the specific steps are as follows:
(1) west safflower is crushed to 80-100 mesh, obtains west safflower powder；
(2) step (1) west safflower powder is taken to be dissolved in hot water, dynamic agitation is extracted, and centrifugation takes supernatant to leak using glass
Bucket is filtered, and collects filtrate；
(3) step (2) filtrate is concentrated into 1/5-1/8 times of volume, upper large pore resin absorption column separation is first eluted with water
(preferably 1.5 column volumes) remove impurity, then elute (preferably room temperature, with 30ml/ with volumetric concentration 70-80% ethanol water
The speed of min filters 3-4 column volume of elution), collect ethanol eluate；
(4) ethanol eluate that step (3) are collected is heated to 65 DEG C, adding active carbon, (preferably active carbon additional amount is to wash
De- liquid product is calculated as 0.2-0.5g/ml) decoloration, filtering, filtrate is further concentrated to no alcohol, then plus acetic acid ethyl ester crystallization, filtering will be brilliant
Soma dry (preferably 60 DEG C) is to get crocin.
Further, the temperature of step (2) hot water is 60-80 DEG C.
Further, saffron powder weight is calculated as 8-10ml/g to the west of step (2) hot water volumetric usage.
Further, step (2) dynamic agitation extraction conditions are as follows: 60-70r/min stirs 100-120min.
Further, step (2) centrifugal condition are as follows: 2000r/min, 20min.
Further, step (2) extraction 2-3 times, after the completion of extracting every time, 2000r/min is centrifuged 20min, and precipitating is taken to add again
Enter and extracted in 60 DEG C of 800ml of hot water, merge the supernatant extracted after centrifugation every time, filtrate is collected in filtering；It is preferred that 2
Secondary, after the completion of extraction, primary to be centrifuged, 2000r/min, 20min take precipitating to add in 60 DEG C of 800ml of hot water and carry out second
Secondary extraction, secondary centrifuging, 2000r/min, 20min are merged the supernatant being centrifuged twice, are filtered using glass funnel, and filter is collected
Liquid.
Further, step (3) macroreticular resin is one of following: macroreticular resin D941.
Further, step (3) macroreticular resin column volume is the pillar of 500mm*500mm*1000mm.
Compared with prior art, the invention has the following beneficial effects: use extracting method extract output of the invention
Rate height is up to 7.3%, and purity is up to 90%.And construction is low with production investment, easy to operate, and extracting method of the invention is convenient for pushing away
Wide application.
Detailed description of the invention
Fig. 1 is products obtained therefrom Quality Map under the conditions of three kinds, and condition 1 is embodiment 1, and condition 2 is embodiment 2, and condition 3 is real
Apply example 3.
Specific embodiment
Technical solution of the present invention is described further With reference to embodiment.
West safflower used in the embodiment of the present invention is according to " Chinese Pharmacopoeia " 2010 editions acquisition preparations.
Embodiment 1
A kind of extracting method of crocin, is done with Chinese medicine west safflower as starting material, including crushing, extraction, centrifugation
Separation, elution and purification step, the specific steps are as follows:
(1) it weighs west safflower and is crushed to 80 mesh, obtain west safflower powder, it is spare.
(2) step (1) west safflower powder 100g is taken to be dissolved in 60 DEG C of 800ml of hot water, under the conditions of revolving speed 60r/min
Dynamic agitation 100min, primary to be centrifuged, 2000r/min, 20min take precipitating to add in 60 DEG C of 800ml of hot water and carry out the
Second extraction, secondary centrifuging, 2000r/min, 20min are merged the supernatant being centrifuged twice, are filtered using glass funnel, are collected
Filtrate.
(3) step (2) filtrate 750ml is concentrated into 1/5 times of volume, upper large pore resin absorption column (volume 500mm*
The pillar of 100mm*1000mm), using macroreticular resin D941,1.5 column volume removal impurity are first eluted with water, then dense with volume
It spends 70% ethanol water and 3 column volumes is eluted with the speed of 30ml/min, be collected into ethanol eluate 300ml, the amount of collection
For 3 times of amount column volumes.
(4) the ethanol eluate 300ml that step (3) are collected is heated to 65 DEG C, adds 100g activity carbon decoloring, filtered, filter
Liquid is further concentrated to no alcohol, then plus acetic acid ethyl ester crystallization, filtering, by 60 DEG C of dryings of crystal to get product 6.5g, quality recovery rate is
6.5%, purity 85%.
Embodiment 2
A kind of extracting method of crocin, is done with Chinese medicine west safflower as starting material, including crushing, extraction, centrifugation
Separation, elution and purification step, the specific steps are as follows:
(1) it weighs west safflower and is crushed to 90 mesh, obtain west safflower powder, it is spare.
(2) it takes step (1) west safflower powder 100g to be dissolved in 900ml70 DEG C of hot water, is moved under the conditions of revolving speed 65r/min
State stirs 110min, and primary to be centrifuged, 2000r/min, 20min take precipitating to add in 60 DEG C of 800ml of hot water and carry out second
Secondary extraction, secondary centrifuging, 2000r/min, 20min are merged the supernatant being centrifuged twice, are filtered using glass funnel, and filter is collected
Liquid.
(3) step (2) filtrate 760ml is concentrated into 1/6 times of volume, upper large pore resin absorption column (with embodiment 1) is first used
1.5 column volumes of water elution remove impurity, then elute 4 columns with 75% ethanol water of volumetric concentration with the speed of 30ml/min
Volume, is collected into ethanol eluate 400ml, and the amount of collection is 4 times of amount column volumes.
(4) the ethanol eluate 400ml that step (3) are collected is heated to 65 DEG C, adds 150g activity carbon decoloring, filtered, filter
Liquid is further concentrated to no alcohol, then plus acetic acid ethyl ester crystallization, filtering, by 60 DEG C of dryings of crystal to get product 5.8g, quality recovery rate is
5.8%, purity 70%.
Embodiment 3
A kind of extracting method of crocin, is done with Chinese medicine west safflower as starting material, including crushing, extraction, centrifugation
Separation, elution and purification step, the specific steps are as follows:
(1) it weighs west safflower and is crushed to 100 mesh, obtain west safflower powder, it is spare.
(2) step (1) west safflower powder 100g is taken to be dissolved in 1000ml80 DEG C of hot water, under the conditions of revolving speed 70r/min
Dynamic agitation 120min, primary to be centrifuged, 2000r/min, 20min take precipitating to add in 60 DEG C of 800ml of hot water and carry out the
Second extraction, secondary centrifuging, 2000r/min, 20min are merged the supernatant being centrifuged twice, are filtered using glass funnel, are collected
Filtrate.
(3) step (2) filtrate 780ml is concentrated into 1/8 times of volume, upper large pore resin absorption column (with embodiment 1) is first used
1.5 column volumes of water elution remove impurity, then elute 4 columns with 80% ethanol water of volumetric concentration with the speed of 30ml/min
Volume, is collected into ethanol eluate 400ml, and the amount of collection is 4 times of amount column volumes.
(4) the ethanol eluate 400ml that step (3) are collected is heated to 65 DEG C, adds 150g activity carbon decoloring, filtered, filter
Liquid is further concentrated to no alcohol, then plus acetic acid ethyl ester crystallization, filtering, by 60 DEG C of dryings of crystal to get product 7.3g, quality recovery rate is
7.3%, purity 90%.
Claims (9)
1. a kind of extracting method of crocin, it is characterised in that the method:
(1) west safflower is crushed to 80-100 mesh, obtains west safflower powder；
(2) step (1) west safflower powder is taken to be dissolved in hot water, dynamic agitation extract, centrifugation, take supernatant using glass funnel into
Row filtering, collects filtrate；
(3) step (2) filtrate is concentrated into 1/5-1/8 times of volume, removal is first eluted with water in upper large pore resin absorption column separation
Impurity, then eluted with volumetric concentration 70-80% ethanol water, collect ethanol eluate；
(4) ethanol eluate that step (3) are collected is heated to 65 DEG C, adds active carbon decoloring, filtered, filtrate is further concentrated to nothing
Alcohol, then plus acetic acid ethyl ester crystallization, filtering crystal is dry to get crocin.
2. the method as described in claim 1, it is characterised in that the temperature of step (2) hot water is 60-80 DEG C.
3. the method as described in claim 1, it is characterised in that saffron powder weight is calculated as to the west of step (2) hot water volumetric usage
8-10ml/g。
4. the method as described in claim 1, it is characterised in that step (2) dynamic agitation extraction conditions are as follows: 60-70r/min is stirred
Mix 100-120min.
5. the method as described in claim 1, it is characterised in that step (2) centrifugal condition are as follows: 2000r/min, 20min.
6. the method as described in claim 1, it is characterised in that step (2) is extracted 2-3 times, after the completion of extracting every time, 2000r/
Min is centrifuged 20min, takes precipitating to add in 60 DEG C of 800ml of hot water and extracts, and merges the supernatant extracted after centrifugation every time
Filtrate is collected in liquid, filtering.
7. the method as described in claim 1, it is characterised in that step (3) macroreticular resin is one of following: macroreticular resin D941.
8. the method as described in claim 1, it is characterised in that the elution of step (3) ethanol water refers to the speed with 30ml/min
Degree 3-4 column volume of elution.
9. the method as described in claim 1, it is characterised in that step (3) macroreticular resin column volume is 500mm*500mm*
1000mm。
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| CN201910398366.1A CN110156847A (en) | 2019-05-14 | 2019-05-14 | A kind of extracting method of crocin |
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| CN201910398366.1A CN110156847A (en) | 2019-05-14 | 2019-05-14 | A kind of extracting method of crocin |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2130066B1 (en) * | 1997-04-15 | 2000-04-01 | Univ Castilla La Mancha | METHOD OF ISOLATION OF COLORING AND FLAVORING SUBSTANCES OF SAFFRON SPECIES: CROCINAS AND PICROCROCINA. |
| CN101864461A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Process for extracting alpha-crocin from fructus gardeniae |
| CN103387489A (en) * | 2013-07-11 | 2013-11-13 | 苏州大学 | Preparation method of high pure crocin and geniposide |
| CN103665060A (en) * | 2013-12-23 | 2014-03-26 | 成都普思生物科技有限公司 | Separation and purification method of crocin I monomer and crocin II monomer |
| CN105131052A (en) * | 2015-07-24 | 2015-12-09 | 河南中大恒源生物科技股份有限公司 | Extraction method of crocin I |
| CN108553556A (en) * | 2018-04-16 | 2018-09-21 | 湖州耕香生物科技有限公司 | A method of preparing the total glycosides of west safflower from west safflower |
-
2019
- 2019-05-14 CN CN201910398366.1A patent/CN110156847A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2130066B1 (en) * | 1997-04-15 | 2000-04-01 | Univ Castilla La Mancha | METHOD OF ISOLATION OF COLORING AND FLAVORING SUBSTANCES OF SAFFRON SPECIES: CROCINAS AND PICROCROCINA. |
| CN101864461A (en) * | 2010-03-23 | 2010-10-20 | 南京泽朗农业发展有限公司 | Process for extracting alpha-crocin from fructus gardeniae |
| CN103387489A (en) * | 2013-07-11 | 2013-11-13 | 苏州大学 | Preparation method of high pure crocin and geniposide |
| CN103665060A (en) * | 2013-12-23 | 2014-03-26 | 成都普思生物科技有限公司 | Separation and purification method of crocin I monomer and crocin II monomer |
| CN105131052A (en) * | 2015-07-24 | 2015-12-09 | 河南中大恒源生物科技股份有限公司 | Extraction method of crocin I |
| CN108553556A (en) * | 2018-04-16 | 2018-09-21 | 湖州耕香生物科技有限公司 | A method of preparing the total glycosides of west safflower from west safflower |
Non-Patent Citations (3)
| Title |
|---|
| A.BOLHASANI,等: "Separation and purification of some components of Iranian saffron", 《ASIAN JOURNAL OF CHEMISTRY》 * |
| MARCUS LAUTENSCHLÄGER,等: "Effective isolation protocol for secondary metabolites from Saffron：Semi-preparative scale preparation of crocin-1 and trans-crocetin", 《FITOTERAPIA》 * |
| 高丽，等: "HPLC法测定不同产地西红花中西红花苷-I和西红苷-II的含量", 《中华中医药学刊》 * |
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Application publication date: 20190823 |