CN103833763A - Method of quickly preparing stable enteromorpha chlorophyll - Google Patents

Method of quickly preparing stable enteromorpha chlorophyll Download PDF

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Publication number
CN103833763A
CN103833763A CN201410106726.3A CN201410106726A CN103833763A CN 103833763 A CN103833763 A CN 103833763A CN 201410106726 A CN201410106726 A CN 201410106726A CN 103833763 A CN103833763 A CN 103833763A
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China
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enteromorpha
chlorophyll
acetic acid
extraction
chlorophyllous
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CN201410106726.3A
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CN103833763B (en
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王鹏
黄志俊
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Ocean University of China
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Ocean University of China
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    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Peptides Or Proteins (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention relates to a method of quickly preparing stable enteromorpha chlorophyll. The method comprises the following steps: by taking enteromorpha as a raw material, adding an acetic acid solution in a certain material-feed ratio; meanwhile, adding a 20% copper sulfate solution in the material-feed ratio of 10:1; mixing and stirring for 30 minutes at 100 DEG C; filtering to obtain enteromorpha chlorophyll acetic acid leach liquor; and extracting by petroleum ether, carrying out reduced pressure distillation and low-temperature drying to obtain an enteromorpha chlorophyll finished product. The method adopting acetic acid leaching has the characteristics of simplicity in operation, efficiency and quick speed. Compared with a conventional method of extracting chlorophyll by alcohol or acetone, the extraction rate is increased by over 3 times. The enteromorpha chlorophyll obtained by the method is a bottle green sticky matter and is slightly sour. The enteromorpha chlorophyll is dissolved in ethyl ether, ethanol, normal hexane and petroleum ether but is not dissolved in water and 50% ethanol. The enteromorpha chlorophyll has better light resistance.

Description

The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast
Technical field
The invention belongs to biological technical field, relate to a kind of preparation fast and stablize the chlorophyllous method of Enteromorpha.
Background technology
Chlorophyll is the epochmaking green pigment of a class being present in vegetable cell, is the essential substance of the absorption while carrying out photosynthesis of green plants and algae, conversion and transmission luminous energy.Chlorophyll absorbs most ruddiness and purple light but reflect green light, so chlorophyll presents green.Chlorophyll and derivative thereof are as green colourant, and the fields such as foodstuff additive, cosmetics additive, food colorant, medicine are done in widespread use.
Chlorophyll molecule is roughly made up of two portions: core is a porphyrin ring, and its function is photoabsorption; Another part is a very long aliphatic hydrocarbon side chain, is called phytol.The existence of phytol makes chlorophyll water insoluble, is dissolved in the organic solvents such as alcohol, acetone and sherwood oil.According to its dissolving properties, the organic solvent extraction chlorophyll such as conventional ethanol, acetone, butanols, methylene dichloride, sherwood oil, Virahol, trieline, extraction temperature is at 50 ~ 85 DEG C, 2~5 hours time.And then after filtration, concentrating under reduced pressure, vacuum-drying, the technological process such as refining obtains the finished product.Chlorophyll class pigment product can be divided into water colo(u)r and fat-soluble pigment two classes, and wherein fat-soluble pigment is used for the painted of cake, beverage, Liquor, jam, jelly, chewy gum etc., is a kind of green colourant.
Producing chlorophyllous raw material has a lot, and what use the earliest is silkworm excrement, has in recent years people to use the leaf of bamboo, reed, beet leaves, the leaf of spinach etc. as producing chlorophyllous raw material.Similar to high green plants, nearly all green alga all has chloroplast(id), and chloroplast(id) content accounts for 1.0 ~ 1.6% of its dry weight.And Enteromorpha is as a kind of large-scale economic green alga that is extensively present in China's Area of The East China Sea, all there is distribution in sea area, south and north, aboundresources.The green tide of Enteromorpha that particularly East Coastal continues to break out in recent years, has produced a large amount of Enteromorpha biomass, becomes the desirable feedstock that chlorophyll is produced.
But, the chlorophyll molecule in different material source, its structure and existence form are different.Compare the high terrestrial plant such as silkworm excrement, spinach, in Enteromorpha frond, chlorophyll and protein bound, its character is unstable, as lipase, proteolytic enzyme etc. can directly or indirectly destroy chlorophyll-lipoprotein complex body, finally generate the de-phytol chlorophyll of de-magging, lose original green.On the other hand; compare other marine green algae (as sea lettuce); Enteromorpha is in decline process; the plastid film of cell is subject to break under the effect of extraneous promotor, makes free radical attack protein, and chlorophyll has lost the protection of protein; form FC more unstable; to light, thermo-responsive, cause chlorophyllous degraded, thereby Enteromorpha is very easily faded.Therefore preparing in chlorophyllous process taking Enteromorpha as raw material, need to carry out modification pre-treatment to Enteromorpha chlorophyll.
The present invention, according to the chlorophyllous constitutional features of Enteromorpha, provides a kind of quick preparation to stablize the chlorophyllous method of Enteromorpha, and this method has no report in existing patent and document.
Summary of the invention
At this, the object of the invention is for Enteromorpha chlorophyll polarity larger, with tradition extract solvent alcohol, acetone extraction rate is not high, and Enteromorpha chlorophyll Character instability, the characteristic of very easily rotten under the impact that is subject to the factors such as illumination, chlorphyllase, temperature, pH, oxygen and metal ion, variable color, provides a kind of simple to operate, efficient, rapid extraction to stablize the chlorophyllous production method of Enteromorpha.
The present invention, taking Enteromorpha as raw material, with acetic acid solution lixiviate Enteromorpha chlorophyll, and according to the feature of its Character instability, carries out synchronous modification to Enteromorpha chlorophyll in leaching process, and by extraction, underpressure distillation obtains and stablizes Enteromorpha chlorophyll finished product fast.
This concrete production craft step is.
Step (1): taking Enteromorpha as raw material, add acetic acid solution with the solid-liquid ratio of 1:5 ~ 1:30, simultaneously add the copper-bath of concentration as 20% taking the solid-liquid ratio of 10:1,90 DEG C ~ 100 DEG C stirring and leaching 30 minutes, filter and obtain Enteromorpha chlorophyll Acetic Acid Extraction liquid.
Step (2): add equal-volume sherwood oil in the Enteromorpha chlorophyll Acetic Acid Extraction liquid obtaining in step (1), stir stratification after extraction, get upper layer of extraction liquid.
Step (3): the upper layer of extraction liquid obtaining in step (2) is carried out to underpressure distillation, obtain paste, oven drying at low temperature obtains stablizes Enteromorpha chlorophyll finished product.
The present invention has following beneficial effect compared with existing chlorophyll production method.
1, the method, mainly according to the specificity of Enteromorpha chlorophyll structure and existence form, provides a kind of simple to operate, efficient, quick preparation to stablize the chlorophyllous method of Enteromorpha.
2, present method adopts the form of Acetic Acid Extraction, makes it to have the advantages that extraction rate is fast, output is high, and compared with traditional alcohol or the chlorophyllous method of acetone extraction, extraction yield improves more than 3 times.
3, present method adds properties-correcting agent copper sulfate in Acetic Acid Extraction process, realizing the chlorophyllous lixiviate of Enteromorpha synchronizes and carries out with modification, not only improve chlorophyllous stability and quality product, the step that simultaneously simplifies the operation, reaches the object that improves Enteromorpha chlorophyll production efficiency.
The Enteromorpha chlorophyll obtaining by the method is the thick material of deep green, slightly with tart flavour.Be dissolved in ether, ethanol, normal hexane, sherwood oil, water insoluble and 50% ethanol.There is good photostabilization, after heating, easily flow.
Embodiment
Embodiment is below in order to make those skilled in the art understand the present invention, but limits the present invention never in any form.
Embodiment 1: take waterside lichenin 1kg, add acetic acid solution 5L, 20% copper-bath 100ml, mix and blend lixiviate 30 minutes at 100 DEG C.Filtration obtains 4.3L filtrate.In filtrate, add 4.3L sherwood oil, stir extraction 10 minutes, stratification, gets upper layer of extraction liquid.By upper layer of extraction liquid underpressure distillation at 50 DEG C, obtain blackish green paste, dry and obtain 8.4g Enteromorpha chlorophyll finished product at 50 DEG C.
Embodiment 2: take waterside lichenin 1kg, add acetic acid solution 8L, 20% copper-bath 100ml, mix and blend lixiviate 30 minutes at 95 DEG C.Filtration obtains 7.2L filtrate.In filtrate, add 7.2L sherwood oil, stir extraction 15 minutes, stratification, gets upper layer of extraction liquid.By upper layer of extraction liquid underpressure distillation at 50 DEG C, obtain blackish green paste, dry and obtain 8.9g Enteromorpha chlorophyll finished product at 50 DEG C.
Embodiment 3: take waterside lichenin 1kg, add acetic acid solution 10L, 20% copper-bath 100ml, stirring and leaching 30 minutes at 90 DEG C.Filtration obtains 8.9L filtrate.In filtrate, add 8.9L sherwood oil, stir extraction 10 minutes, stratification, gets upper layer of extraction liquid.By upper layer of extraction liquid underpressure distillation at 50 DEG C, obtain blackish green paste, dry and obtain 9.2g Enteromorpha chlorophyll finished product at 50 DEG C.

Claims (3)

1. prepare and stablize the chlorophyllous method of Enteromorpha fast for one kind, it is characterized in that the method comprises: taking Enteromorpha as raw material, add by a certain percentage acetic acid solution, simultaneously add the copper-bath of concentration as 20% taking the solid-liquid ratio of 10:1,90 DEG C ~ 100 DEG C stirring and leaching 30 minutes, filtration obtains Enteromorpha chlorophyll Acetic Acid Extraction liquid, in Enteromorpha chlorophyll Acetic Acid Extraction liquid, add equal-volume sherwood oil, stir the rear stratification of extraction, upper layer of extraction liquid is carried out to underpressure distillation, obtain paste, oven drying at low temperature obtains stablizes Enteromorpha chlorophyll finished product.
2. prepare and stablize the chlorophyllous method of Enteromorpha fast by one claimed in claim 1, it is characterized in that Enteromorpha raw material is 10 ~ 200 object waterside lichenins.
3. prepare and stablize the chlorophyllous method of Enteromorpha fast by one claimed in claim 1, it is characterized in that the addition of acetic acid solution adds by solid-liquid ratio 1:5 ~ 1:30.
CN201410106726.3A 2014-03-21 2014-03-21 The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast Active CN103833763B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107253953A (en) * 2017-08-02 2017-10-17 中国科学院海洋研究所 A kind of method that chlorophyll is extracted from Enteromorpha

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05279368A (en) * 1992-03-30 1993-10-26 Masaki Kamata Production of chlorophyll a type compound and feed comprising the same product
CN1230546A (en) * 1998-04-01 1999-10-06 中国科学院长春物理研究所 Extraction process of pheophorbide A from algae
KR20120021798A (en) * 2010-08-17 2012-03-09 주식회사 루맥스바이오 Methods for preparing high purity chlorophyll and chlorin e6 from chlorophyll extracts
CN103012414A (en) * 2012-12-04 2013-04-03 青岛艾华隆生物科技有限公司 Process for enzymatic preparation of enteromorpha chlorophyll

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05279368A (en) * 1992-03-30 1993-10-26 Masaki Kamata Production of chlorophyll a type compound and feed comprising the same product
CN1230546A (en) * 1998-04-01 1999-10-06 中国科学院长春物理研究所 Extraction process of pheophorbide A from algae
KR20120021798A (en) * 2010-08-17 2012-03-09 주식회사 루맥스바이오 Methods for preparing high purity chlorophyll and chlorin e6 from chlorophyll extracts
CN103012414A (en) * 2012-12-04 2013-04-03 青岛艾华隆生物科技有限公司 Process for enzymatic preparation of enteromorpha chlorophyll

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘秀丽 等: ""植物叶绿素测定方法的再探讨"", 《江苏农业研究》 *
陈晨 等: ""浒苔叶绿素铜钠盐的制备研究初探"", 《中国海洋药物杂志》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107253953A (en) * 2017-08-02 2017-10-17 中国科学院海洋研究所 A kind of method that chlorophyll is extracted from Enteromorpha
CN107253953B (en) * 2017-08-02 2019-11-12 中国科学院海洋研究所 A method of extracting chlorophyll from Enteromorpha

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