CN106699767A - Method for extracting chlorophylls from watermelon peel - Google Patents
Method for extracting chlorophylls from watermelon peel Download PDFInfo
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- CN106699767A CN106699767A CN201510775137.9A CN201510775137A CN106699767A CN 106699767 A CN106699767 A CN 106699767A CN 201510775137 A CN201510775137 A CN 201510775137A CN 106699767 A CN106699767 A CN 106699767A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
- C07D487/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains four or more hetero rings
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention discloses a method for extracting chlorophylls from watermelon peel. The method comprises the following steps: 1, crushing and beating watermelon peel, and freezing obtained slurry to obtain freeze-dried watermelon peel powder; 2, mixing the freeze-dried watermelon peel powder with 95 wt% ethanol, carrying out high-speed pretreatment, carrying out homogenous extraction, and filtering obtained extract; 3, mixing filter residues with 95 wt% ethanol, carrying out homogenous extraction, and filtering obtained extract; 4, centrifuging the obtained filtrate, collecting the obtained supernatant, and concentrating the collected supernatant; and 5, purifying and drying the obtained concentrate to obtain the chlorophylls. The method has the advantages of no heating, less chlorophyll loss, short extraction time, less solvent loss and high extraction efficiency.
Description
Technical field
The invention belongs to the extractive technique field of natural pigment, and in particular to a kind of method that chlorophyll is extracted from watermelon outer peel.
Background technology
China's growth of watermelon technology have developed rapidly in recent years, but majority, to sell based on watermelon, added value of product is low, and economic benefit is not obvious.Contain substantial amounts of natural chlorophyll in the sclerderm of watermelon ragged edge, in can be widely used in the industries such as food, medicine；Phyllins pharmaceutically have many-sided bioactivity such as promotion wound healing, antiulcer, antitumor, antimicrobial, anti-cancer, liver protection, anti-anemia action.
It is good chlorophyll source containing abundant chlorophyll in watermelon outer peel.
The current main extracting mode of chlorophyll is that solvent method heats extraction.Chlorophyll is a kind of liposoluble substance, and thermally labile is shown in that light is decomposed, and with heating leach extraction method, the time is more long, and solvent loss is larger, and heating is easily damaged to chlorophyll, and the extraction efficiency to chlorophyll is relatively low.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method for preparing chlorophyll as raw material with watermelon outer peel, without heating, chlorophyll loss is small, and extraction time is very short for the method, it is to avoid a large amount of losses of solvent, and extraction efficiency is high.
The present invention provide technical scheme be：A kind of method that chlorophyll is extracted from watermelon outer peel, it is characterised in that the method comprises the following steps：
(1) watermelon outer peel is crushed and is beaten, freeze to obtain watermelon outer peel freeze-dried powder；
(2) watermelon outer peel freeze-dried powder is mixed with 95wt% ethanol, at room temperature, is pre-processed at a high speed, homogeneous is extracted, filtering；
(3) filter residue after filtering is mixed with 95wt% ethanol, at room temperature, homogeneous is extracted, filtering；
(4) filtrate of step (2) and (3) is centrifuged, collects supernatant, be concentrated in vacuo to obtain concentrate, solid content reaches more than 30% in concentrate；
(5) purifying is that 75%-95% acetone stirs with concentrate with 4-8 times of volume of concentrate concentration, and .5-2d is set to 0 in 0-4 DEG C of decentralization, and filtering removal filter cake obtains chlorophyll fine work after filtrate concentration and recovery acetone.
Wherein, the high speed pretreatment is to be processed more than 5 minutes with 5000-10000 revs/min；Homogeneous in step (2) or (3) is extracted as being processed more than 10 minutes with 1000-4000 revs/min.
The time of step (2) high speed pretreatment is 5-20 minutes；The time that homogeneous is extracted in step (2) or (3) is 10-60 minutes.
The pretreatment of step (2) high speed is to be processed 5-10 minutes with 9000-10000 revs/min, and the homogeneous described in step (2) and step (3) is extracted as being processed 10-30 minutes with 3000 revs/min.
In step (2), the watermelon outer peel freeze-dried powder is 1g/mL~1g/10mL, preferably 1g/5mL~1g/10mL with the mass volume ratio of the 95wt% ethanol；In step (3), the filter residue is 1g/mL~1g/10mL, preferably 1g/5mL~1g/10mL with the mass volume ratio of the 95wt% ethanol.
In the preferred embodiment of the present invention, described high speed pretreatment is to be processed 5-10 minutes with 9000-10000 revs/min, and the homogeneous described in step (2) and step (3) is extracted as being processed 10-30 minutes with 3000 revs/min.
In the present invention, the high speed pretreatment and the homogeneous are extracted and can carried out in homogenizer.
In step (4), the rotating speed of the centrifugation is preferably 200-2000 revs/min, preferably 1000 revs/min.It is 5-30 minutes that the time of the centrifugation is preferably.
Room temperature of the present invention is that this area is understood the routine of room temperature, refers generally to 5-40 DEG C.
On the basis of common sense in the field is met, above-mentioned each optimum condition can be combined, and obtain final product each preferred embodiment of the invention.
Reagent, raw material and the equipment that the present invention is used are all commercially available, and chemical reagent purity used is at least food-grade.
Positive effect of the invention is：
(1) extraction of watermelon outer peel chlorophyll of the present invention is carried out in two stages under the auxiliary of high-shear homogenizing machine, the high speed pretreatment of first stage is smaller by the little particle change of the leaf of bamboo, make it easier to be distributed evenly in solution, reach extraction effect than more uniform, extraction comparison is thorough；And the stage is extracted compared with the homogeneous under low rate, also relatively standing extraction or other extracting methods has chlorophyll recovery rate higher.
(2) extraction process of the invention is simple, low to production equipment requirement, and extraction efficiency is high, and extraction time is short, hence it is evident that better than traditional solvent extraction method.And described extraction process can be carried out at room temperature, it is not necessary to carry out heating extraction.
(3) the chlorophyll good water solubility that present invention process is extracted, product appearance color and luster is good, proterties stabilization, is adapted as food additives and healthy food material.
(4) present invention realizes the comprehensive utilization to watermelon, substantially increases the economic worth of watermelon, and it is fertilizer that the filter residue produced in preparation process can be used to ferment.
Specific embodiment
The present invention is further illustrated with embodiment below, but the present invention is not intended to be limited thereto, and the raw material in embodiment is conventional commercial product.
Embodiment 1
1) watermelon outer peel is crushed and is beaten, freeze to obtain watermelon outer peel freeze-dried powder, weigh 100 grams of above-mentioned watermelon outer peel freeze-dried powder, it is standby.
2) 95wt% ethanol (watermelon outer peel freeze-dried powder: 95wt% ethanol=1g: 5mL) is added, at room temperature, is pre-processed 5 minutes at a high speed with 10000 revs/min, then filtered after being extracted 30 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 5mL) is added in filter residue, at room temperature, filtered after being extracted 30 minutes with 3000 revs/min of homogeneous.
4) merge filtrate twice, at room temperature, be centrifuged 10 minutes with 1000 revs/min, go precipitation, carry out being concentrated in vacuo to obtain concentrate after collecting supernatant, solid content reaches 30% in concentrate.
(5) with 4 times of volume of concentrate concentration for 95% acetone stirs with concentrate, 2d is placed at 0-4 DEG C, filtering removal filter cake obtains chlorophyll fine work, is dried to obtain 3.6 grams of mulberry leaf chlorophyll, color after filtrate concentration and recovery acetone：Green, colour value 22.8.
Embodiment 2
1) watermelon outer peel is crushed and is beaten, freeze to obtain watermelon outer peel freeze-dried powder, weigh 100 grams of above-mentioned watermelon outer peel freeze-dried powder, it is standby..
2) 95wt% ethanol (watermelon outer peel freeze-dried powder: 95wt% ethanol=1g: 7mL) is added, at room temperature, is pre-processed 10 minutes at a high speed with 10000 revs/min, then filtered after being extracted 20 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 7mL) is added in filter residue, filtered after being extracted 20 minutes with 3000 revs/min of homogeneous at room temperature.
4) merge filtrate twice, at room temperature, be centrifuged 15 minutes with 1000 revs/min, go precipitation, be concentrated in vacuo after collecting supernatant, solid content reaches 35% in concentrate.
5) with 8 times of volume of concentrate concentration for 75% acetone stirs with concentrate .5d is set to 0 in 0-4 DEG C of decentralization, filtering removal filter cake obtains chlorophyll fine work, is dried to obtain 3.7 grams of mulberry leaf chlorophyll, color after filtrate concentration and recovery acetone：Green, colour value 25.4.
Embodiment 3
1) watermelon outer peel is crushed and is beaten, freeze to obtain watermelon outer peel freeze-dried powder, weigh 100 grams of above-mentioned watermelon outer peel freeze-dried powder, it is standby.
2) 95wt% ethanol (watermelon outer peel freeze-dried powder: 95wt% ethanol=1g: 10mL) is added, at room temperature, is pre-processed 10 minutes at a high speed with 10000 revs/min, then filtered after being extracted 10 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 10mL) is added in filter residue, filtered after being extracted 10 minutes with 3000 revs/min of homogeneous at room temperature.
4) merge filtrate twice, at room temperature, be centrifuged 15 minutes with 1000 revs/min, go precipitation, be concentrated in vacuo after collecting supernatant, solid content reaches 40% in concentrate.
5) with 6 times of volume of concentrate concentration for 85% acetone stirs with concentrate .5d is set to 0 in 0-4 DEG C of decentralization, filtering removal filter cake obtains chlorophyll fine work, is dried to obtain 3.9 grams of mulberry leaf chlorophyll, color after filtrate concentration and recovery acetone：Green, colour value 24.6.
Claims (5)
1. a kind of method that chlorophyll is extracted from watermelon outer peel, comprises the following steps：
(1) watermelon outer peel is crushed and is beaten, freeze to obtain watermelon outer peel freeze-dried powder；
(2) watermelon outer peel freeze-dried powder is mixed with 95wt% ethanol, at room temperature, is pre-processed at a high speed, homogeneous is extracted, filtering；
(3) filter residue after filtering is mixed with 95wt% ethanol, at room temperature, homogeneous is extracted, filtering；
(4) filtrate of step (2) and (3) is centrifuged, collects supernatant, be concentrated in vacuo to obtain concentrate, solid content reaches more than 30% in concentrate；
(5) purifying is that 75%-95% acetone stirs with concentrate with 4-8 times of volume of concentrate concentration, and .5-2d is set to 0 in 0-4 DEG C of decentralization, and filtering removal filter cake obtains chlorophyll fine work after filtrate concentration and recovery acetone；
Wherein, the high speed pretreatment is with 5000-10000
Rev/min treatment more than 5 minutes；Homogeneous in step (2) or (3) is extracted as being processed more than 10 minutes with 1000-4000 revs/min.
2. the extraction process as described in claim 1, it is characterised in that：The time of the high speed pretreatment is 5-20 minutes；The time that homogeneous is extracted in step (2) or (3) is 10-60 minutes.
3. the extraction process as described in claim 1, it is characterised in that：Described high speed pretreatment is to be processed 5-10 minutes with 9000-10000 revs/min, and the homogeneous described in step (2) and step (3) is extracted as being processed 10-30 minutes with 3000 revs/min.
4. the extraction process as described in claim 1, it is characterised in that：The size of the watermelon outer peel freeze-dried powder is the sieve that can cross 100 mesh.
5. the extraction process as any one of claim 1~4, it is characterised in that：In step (2), the watermelon outer peel freeze-dried powder is 1g/mL~1g/10mL, preferably 1g/5mL~1g/10mL with the mass volume ratio of the 95wt% ethanol；In step (3), the filter residue is 1g/mL~1g/10mL, preferably 1g/5mL~1g/10mL with the mass volume ratio of the 95wt% ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510775137.9A CN106699767A (en) | 2015-11-15 | 2015-11-15 | Method for extracting chlorophylls from watermelon peel |
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| CN201510775137.9A CN106699767A (en) | 2015-11-15 | 2015-11-15 | Method for extracting chlorophylls from watermelon peel |
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| CN106699767A true CN106699767A (en) | 2017-05-24 |
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| CN201510775137.9A Pending CN106699767A (en) | 2015-11-15 | 2015-11-15 | Method for extracting chlorophylls from watermelon peel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707149A (en) * | 2018-07-12 | 2018-10-26 | 云南茶农生物产业有限责任公司 | A kind of extracting method of berberine |
| CN110393675A (en) * | 2019-08-14 | 2019-11-01 | 广州美蔻生物科技有限公司 | A kind of chlorophyll freeze-dried powder and preparation method thereof |
| CN110585099A (en) * | 2019-10-12 | 2019-12-20 | 福建省梦娇兰日用化学品有限公司 | Baby moisturizing and nourishing shower gel prepared by plant chlorophyll centrifugal extraction technology |
-
2015
- 2015-11-15 CN CN201510775137.9A patent/CN106699767A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707149A (en) * | 2018-07-12 | 2018-10-26 | 云南茶农生物产业有限责任公司 | A kind of extracting method of berberine |
| CN110393675A (en) * | 2019-08-14 | 2019-11-01 | 广州美蔻生物科技有限公司 | A kind of chlorophyll freeze-dried powder and preparation method thereof |
| CN110585099A (en) * | 2019-10-12 | 2019-12-20 | 福建省梦娇兰日用化学品有限公司 | Baby moisturizing and nourishing shower gel prepared by plant chlorophyll centrifugal extraction technology |
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Application publication date: 20170524 |