CN106699767A - Method for extracting chlorophylls from watermelon peel - Google Patents

Method for extracting chlorophylls from watermelon peel Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
minutes
extracted
ethanol
freeze
homogeneous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510775137.9A
Other languages
Chinese (zh)
Inventor
曹秀玲
其他发明人请求不公开姓名
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dou Hao Bio Tech Ltd Chongqing
Original Assignee
Dou Hao Bio Tech Ltd Chongqing
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dou Hao Bio Tech Ltd Chongqing filed Critical Dou Hao Bio Tech Ltd Chongqing
Priority to CN201510775137.9A priority Critical patent/CN106699767A/en
Publication of CN106699767A publication Critical patent/CN106699767A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D487/00Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
    • C07D487/22Heterocyclic 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Fruits And Vegetables (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicines Containing Plant Substances (AREA)

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

A kind of method that chlorophyll is extracted from watermelon outer peel
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.
CN201510775137.9A 2015-11-15 2015-11-15 Method for extracting chlorophylls from watermelon peel Pending CN106699767A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510775137.9A CN106699767A (en) 2015-11-15 2015-11-15 Method for extracting chlorophylls from watermelon peel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510775137.9A CN106699767A (en) 2015-11-15 2015-11-15 Method for extracting chlorophylls from watermelon peel

Publications (1)

Publication Number Publication Date
CN106699767A true CN106699767A (en) 2017-05-24

Family

ID=58931831

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510775137.9A Pending CN106699767A (en) 2015-11-15 2015-11-15 Method for extracting chlorophylls from watermelon peel

Country Status (1)

Country Link
CN (1) CN106699767A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN101613418A (en) A kind of method of extracting agaricus lentinan
CN100376684C (en) Process for preparing bacteriostatic peptide by discarded tobacco leaf protein
CN106699767A (en) Method for extracting chlorophylls from watermelon peel
CN102492054B (en) Preparation method of soybean episperm pectin gel polysaccharide
CN102040579A (en) Method for extracting luteolin from peanut roots, stems, leaves and shells
CN107337934A (en) A kind of extracting method of vaccinium bracteatum thunb leaf pigment
CN104231097A (en) Preparation method of lyceum barbarum polysaccharide
CN105385188A (en) Preparation method of mulberry red pigment
CN106188181B (en) A method of extracting aurantiin from pomelo peel
CN112661767B (en) Method for synchronously preparing sesame concentrated protein, sesame oil and sesamin from sesame cake meal
CN104448902A (en) Grape skin pigment extraction technology
CN104448907A (en) Natural pigment extraction technology
EP3505525A1 (en) Method for preparing rubusoside
CN106699769A (en) Method for extracting chlorophylls from mulberry leaves
CN103819572A (en) Extraction technology for production of polysaccharide from mulberry leaf
CN103254321B (en) The method for extraction and purification of medicinal fungi Phellinus vaninii polysaccharide
CN112442136A (en) Method for extracting functional components from tremella
CN101433322B (en) Functional food rich in anthocyanidin and preparation method thereof
CN106188183A (en) A kind of combined extracting naringin and method of pectin from pomelo peel
CN115463181B (en) Preparation method of agilawood leaf extract
CN108101980A (en) A kind of preparation method of high-purity algae blue pigment
CN106699768A (en) Method of extracting chlorophyll from bamboo leaves
CN104546998B (en) The production method of high genistin content isoflavones
CN101898989B (en) Method for extracting carotenoid from Chinese wolfberry by microwaves
CN102433013A (en) Method for extracting betalain from phytolaccic berry

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170524