CN103833763B - The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast - Google Patents
The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast Download PDFInfo
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- CN103833763B CN103833763B CN201410106726.3A CN201410106726A CN103833763B CN 103833763 B CN103833763 B CN 103833763B CN 201410106726 A CN201410106726 A CN 201410106726A CN 103833763 B CN103833763 B CN 103833763B
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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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- 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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Abstract
The present invention relates to a kind of preparation fast and stablize the chlorophyllous method of Enteromorpha.The method take Enteromorpha as raw material, acetic acid solution is added with certain solid-liquid ratio, add with the solid-liquid ratio of 10:1 the copper-bath that concentration is 20% simultaneously, mix and blend 30 minutes at 100 DEG C, filtration obtains Enteromorpha chlorophyll Acetic Acid Extraction liquid, obtains Enteromorpha chlorophyll finished product through petroleum ether extraction, underpressure distillation, oven drying at low temperature.The method adopt Acetic Acid Extraction have simple to operate, efficiently, feature fast, compared with traditional alcohol or the chlorophyllous method of acetone extraction, extraction yield improves more than 3 times.The Enteromorpha chlorophyll utilizing the method to obtain is deep green sticky mass, slightly has tart flavour.Be dissolved in ether, ethanol, normal hexane, sherwood oil, water insoluble and 50% ethanol, have good photostabilization.
Description
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 be present in vegetable cell, is the essential substance of absorption when carrying out photosynthesis of green plants and algae, conversion and transmission luminous energy.The most ruddiness of Chlorophyll absorption 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 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 class, 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.
Produce chlorophyllous raw material to have a lot, use silkworm excrement the earliest, have people in recent years with the leaf of bamboo, reed, beet leaves, the leaf of spinach etc. as the chlorophyllous raw material of production.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 being extensively present in China's Area of The East China Sea, all there is distribution in sea area, south and north, aboundresources.The particularly East Coastal green tide of Enteromorpha that continues to break out in recent years, creates a large amount of Enteromorpha biomass, becomes the desirable feedstock that chlorophyll is produced.
But, different material source chlorophyll molecule, its structure and existence form 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, the final de-magging that generates takes off phytol chlorophyll, loses original green.On the other hand; compare other marine green algae (as sea lettuce); Enteromorpha is in decline process; the plastid film of cell breaks by under the effect of extraneous promotor, and make free radical attack protein, chlorophyll loses the protection of protein; form FC more unstable; to light, thermo-responsive, cause chlorophyllous degraded, thus Enteromorpha is very easily faded.Therefore be that raw material is prepared in chlorophyllous process with Enteromorpha, needing to carry out modification pre-treatment to Enteromorpha chlorophyll.
The present invention is according to the chlorophyllous constitutional features of Enteromorpha, and provide a kind of preparation fast and stablize the chlorophyllous method of Enteromorpha, 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, not high by traditional Extraction solvent alcohol, acetone extraction rate, and Enteromorpha chlorophyll Character instability, the characteristic of very easily rotten under the impact being 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 take Enteromorpha as raw material, and with acetic acid solution lixiviate Enteromorpha chlorophyll, and according to the feature of its Character instability, in leaching process, carry out synchronous modification to Enteromorpha chlorophyll, by extraction, underpressure distillation obtains stable Enteromorpha chlorophyll finished product fast.
This concrete production craft step is.
Step (1): take Enteromorpha as raw material, add acetic acid solution with the solid-liquid ratio of 1:5 ~ 1:30, simultaneously adds with the solid-liquid ratio of 10:1 the copper-bath that concentration is 20%, and 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 obtained in step (1), stirs the rear stratification of extraction, gets upper layer of extraction liquid.
Step (3): the upper layer of extraction liquid obtained in step (2) is carried out underpressure distillation, obtains paste, namely oven drying at low temperature obtains stable Enteromorpha chlorophyll finished product.
The present invention has following beneficial effect compared with existing chlorophyll production method.
1, the method is 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, and make it to have the advantages that extraction rate is fast, output is high, 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, realize the chlorophyllous lixiviate of Enteromorpha and modification and synchronously carry out, not only improve chlorophyllous stability and quality product, simplify the operation step simultaneously, reaches the object improving Enteromorpha chlorophyll production efficiency.
The Enteromorpha chlorophyll obtained by the method is deep green sticky mass, slightly has tart flavour.Be dissolved in ether, ethanol, normal hexane, sherwood oil, water insoluble and 50% ethanol.There is good photostabilization, easily flowing after heating.
Embodiment
Embodiment is below 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, adds 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 at 50 DEG C and obtain 8.4g Enteromorpha chlorophyll finished product.
Embodiment 2: take waterside lichenin 1kg, adds 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 at 50 DEG C and obtain 8.9g Enteromorpha chlorophyll finished product.
Embodiment 3: take waterside lichenin 1kg, adds 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 at 50 DEG C and obtain 9.2g Enteromorpha chlorophyll finished product.
Claims (2)
1. the chlorophyllous method of Enteromorpha is stablized in a quick preparation, it is characterized in that the method comprises: take Enteromorpha as raw material, the ratio being 1:5 ~ 1:30 in solid-liquid ratio adds acetic acid solution, add with the solid-liquid ratio of 10:1 the copper-bath that concentration is 20% simultaneously, 90 DEG C ~ 100 DEG C stirring and leaching 30 minutes, filtration obtains Enteromorpha chlorophyll Acetic Acid Extraction liquid, equal-volume sherwood oil is added in Enteromorpha chlorophyll Acetic Acid Extraction liquid, stir the rear stratification of extraction, upper layer of extraction liquid is carried out underpressure distillation, obtain paste, namely oven drying at low temperature obtains stable Enteromorpha chlorophyll finished product.
2. prepare the chlorophyllous method of stable Enteromorpha fast by one according to claim 1, it is characterized in that Enteromorpha raw material is 10 ~ 200 object waterside lichenins.
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| CN201410106726.3A CN103833763B (en) | 2014-03-21 | 2014-03-21 | The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast |
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| CN201410106726.3A CN103833763B (en) | 2014-03-21 | 2014-03-21 | The chlorophyllous method of Enteromorpha is stablized in a kind of preparation fast |
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| CN103833763B true CN103833763B (en) | 2015-11-18 |
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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Family Cites Families (2)
| 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 |
| KR101180695B1 (en) * | 2010-08-17 | 2012-09-10 | 동성루맥스 주식회사 | Methods for Preparing high purity chlorophyll and Chlorin e6 from Chlorophyll extracts |
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2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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)
| Title |
|---|
| "植物叶绿素测定方法的再探讨";刘秀丽 等;《江苏农业研究》;19991231;第20卷(第3期);第46-47页 * |
| "浒苔叶绿素铜钠盐的制备研究初探";陈晨 等;《中国海洋药物杂志》;20120229;第31卷(第1期);第20-24页 * |
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