CN107011155A - A kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin - Google Patents
A kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin Download PDFInfo
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- CN107011155A CN107011155A CN201710212471.2A CN201710212471A CN107011155A CN 107011155 A CN107011155 A CN 107011155A CN 201710212471 A CN201710212471 A CN 201710212471A CN 107011155 A CN107011155 A CN 107011155A
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- mussel shell
- melanin
- calcium
- pyruvic
- acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/618—Molluscs, e.g. fresh-water molluscs, oysters, clams, squids, octopus, cuttlefish, snails or slugs
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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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Abstract
The present invention relates to a kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin.Described method is by steps such as milling, elutriation processing, acid adding conversion, filtering and purifying.Mussel shell puts into wet process disintegrator milling (below 60 mesh) after scrub, plus appropriate distilled water and conversion of pyruvate；Said mixture is filtered, filter residue is after alkali soluble, the heavy processing of acid, and sediment is again through washing, being drying to obtain mussel shell melanin；Filtrate concentrates in the evaporator that is concentrated under reduced pressure, 4 DEG C of crystallizations, then is drying to obtain CALCIUM PYRUVIC through 100~120 DEG C.The mussel shell melanin that the present invention is separated has to the lung carcinoma cells of A 549 significantly inhibits effect, is expected to be developed to natural antitumor medicine；CALCIUM PYRUVIC is widely used in fields such as medicine, food.This method is easy to operate, it is easy to large-scale production and popularization and application, can the high-valued mussel shell resource for comprehensively utilizing China's abundant.
Description
Technical field：
The invention belongs to the high-valued technical field of comprehensive utilization of shell, and in particular to one kind separates melanin using mussel shell
The method of simultaneously synthesizing CALCIUM PYRUVIC.
Background technology：
Mussel (Mytilus edulis), dried product is then referred to as mussel, is a kind of bivalve, is China's weight
One of cultivated shellfish wanted.Mussel is extremely strong because of vitality, easily propagates artificially on a large scale, China Shandong, Guangdong, Liaoning, Hainan
There is large stretch of marine site to be used for mussel culture Deng province.In the last few years, research of the domestic and foreign scholars to it is concentrated mainly on edible portion,
Research shows mussel meat delicious, and protein content is high, therefore has a laudatory title of " marine egg ", and to the research of its shell relatively
It is few.In fact, mussel shell is rich in natural black pigment and enriches calcareous, can be by higher value application.
Natural black pigment source very wide, physicochemical property is unique and immune with anti-aging, protection illumination damage, regulation
The multiple biological activities such as power, anti-oxidant, protection cardiovascular function, all have in terms of prophylactic treatment, food, cosmetics
Fabulous application prospect, thus all have great importance in terms of theory and practice.At present, consumer can not increasingly connect
The colouring agent and antioxidant synthesized so that natural colorant and antioxidant become more and more popular.On natural black pigment
Research alreadys exceed half a century, because it is often firmly combined with protein and polysaccharide so that melanin dissolubility is poor and does not allow
It is easily separated, thus great difficulty is encountered to its research carried out.
Meanwhile, the discarded object that mussel shell is processed as seashells, content of mineral substances enriches, wherein 95% above is carbonic acid
The trace element such as calcium, also zinc, silicon, iron, magnesium, thus mussel shell can as high-quality green calcium source.Such as using suitable preparation
Technique mussel shell is made the calcium activated agent being easily absorbed by the human body, can higher value application shell, and then solve mussel shell as solid
The problems such as wasting of resources and environmental pollution caused by body rubbish.
National nutrition survey result is shown within 2013, and the shortage of Chinese residents calcium is commonplace.Calcium intake is not enough easily
Guided many illnesss, such as it is regular ache all over, tetany, it is powerless symptom.Calcium is more than constituting bone and tooth
The important element of tooth, the also movable close relation with N＆M, with the activity, blood clotting, hormone of internal enzyme
Of close concern to each other in terms of the normal physiological condition of secretion and cell, calcium deficiency influences whether the every aspect of human body.On the other hand, with
The raising of economic level and the change of dietary structure, fat people is more and more more.Obesity not only influences figure, can also endanger body and be good for
Health.So miscellaneous fat-reducing measure is of common occurrence, but wherein effective and healthy mode is seldom.CALCIUM PYRUVIC is also
A kind of calcium nutritious supplementary pharmaceutical, let it be to the greatest extent, and calcium content is less than 20%, but enters after human body, unlike the acid in other calcium-supplementing preparations
Radical ion increases liver kidney burden.Acetone acid ion, which enters, to be easy to enter mitochondria by osmosis in vivo, participates in fat
The metabolism of acid (mainly long chain type), and produce the energy needed for body.From the point of view of macroscopic view, the fat reduction of body, body weight drop
It is low.The scientific experiment result of Univ. of Pittsburgh's medical research center shows：CALCIUM PYRUVIC can at least increase by 48% fat
Fat is consumed, and reduces the consumption of vivo protein to a certain extent.In addition, CALCIUM PYRUVIC also has increase endurance, improves body
Body function, decline cholesterol and low density cholesterol (LDL) level, mitigate heart injury caused by ischaemic, strengthen
The effect such as function of cardiac muscle, and it is not yet found that obvious side effect, edible safety is high.At present, prepared by CALCIUM PYRUVIC
Method is main by pyruvic acid and Ca (OH)2Emulsion is reacted or Sodium Pyruvate reacts with solvable inorganic calcium salt to be prepared.Existing rank
Seldom, its product is mainly outlet, and expensive for the manufacturer of section China.
The present invention seeks to isolate melanin from mussel shell, simultaneously synthesizing CALCIUM PYRUVIC really realizes mussel shell
High-valued comprehensive utilization.
The content of the invention：
The present invention from mussel shell in order to isolate melanin, the property according to mussel shell melanin insoluble in acid, first will
Mussel shell high concentration acetone acid treatment, melanin separate out, calcium carbonate is converted into CALCIUM PYRUVIC simultaneously,.Specific implementation step
It is rapid as follows：(1) it is milled：Mussel shell puts into wet process disintegrator milling (below 60 mesh) after scrubbing, washing down；(2) elutriation is handled：
Above-mentioned mussel shell powder is added in proper amount of clear water, in the case where being stirred continuously, suspension powder is poured out and is stood drip after 1~2 hour
It is dry to produce calcium source mussel shell powder；(3) acid adding：Plus (addition should be less than based on dry mussel shell powder calcium carbonate content 95% pyruvic acid
Calculate obtained quantity, it is ensured that calcium source mussel shell powder excessive 1~5%) and appropriate distilled water, stirring, 3~4 hours are incubated in 60~70 DEG C；
(4) filter, purify：Said mixture is filtered, 1. filter residue is first washed to neutrality, (filter residue is refiltered after being dissolved with appropriate diluted alkaline
Reclaim), filtrate adds enough hydrochloric acid melanin is refiltered after precipitating completely, and filter residue desalts through washing, removes acid (to neutral), dries
Produce mussel shell melanin；2. filtrate concentrates in the evaporator that is concentrated under reduced pressure, crystallized (4 DEG C), then is through 100~120 DEG C of dryings
Obtain CALCIUM PYRUVIC.
The beneficial effects of the invention are as follows synthesize the acetone of calcium tonic one while mussel melanin is separated from mussel shell
Sour calcium (micro- Huang, soluble in water).Mussel shell melanin activity testing result shows that it has notable suppression to A-549 lung carcinoma cells
Make and use, 38.7% is reached to the inhibiting rate of A-549 cells when concentration is 0.4mg/mL, it is ocean antineoplastic to be expected to exploitation
Thing.
Brief description of the drawings
Fig. 1 is the process chart that mussel shell melanin separates simultaneously synthesizing CALCIUM PYRUVIC.
Embodiment：
Below by example, the present invention is further elaborated：
Example：Input wet process disintegrator milling handles to obtain calcium source (below 60 mesh) with elutriation after 110kg mussel shells are cleaned
Mussel shell powder (dry weight about 100kg).Add the pyruvic acid of 82kg 98% and 20kg distilled water, stirring, after 60 DEG C are incubated 3 hours
Filtering, (1) filter residue is first to be originally washed to after neutrality, to filter (filter residue recovery) after 30 liters of 0.5M sodium hydroxides dissolvings, filtrate
Plus refiltered after 5 liters of 4M hydrochloric acid, filter residue desalts through washing, removes acid (to neutral), is drying to obtain mussel shell melanin 390g；(2)
Filtrate is drying to obtain CALCIUM PYRUVIC [C through being concentrated under reduced pressure, crystallizing (4 DEG C), then through 100~120 DEG C6H6CaO6]97kg。
Claims (3)
1. a kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin, its step is as follows：
(1) it is milled：Mussel shell puts into wet process disintegrator milling (below 60 mesh) after scrubbing, washing down；
(2) elutriation is handled：Above-mentioned mussel shell powder is added in proper amount of clear water, in the case where being stirred continuously, suspension powder is poured out and incites somebody to action
It drains after standing 1~2 hour and produces calcium source mussel shell powder；
(3) acid adding：Pyruvic acid addition, which is less than, presses reaction equation amount of calculation, and adds appropriate distilled water, stirring, 60~70 DEG C of insulations 3
~4 hours；
(4) filter, purify：Said mixture is filtered, 1. filter residue is first washed to neutrality, refiltered after being dissolved with appropriate diluted alkaline
(filter residue recovery), filtrate adds enough hydrochloric acid melanin is filtered after precipitating completely, filter residue desalts through washing, go acid (to neutral),
It is drying to obtain mussel shell melanin；2. filtrate is concentrated in the evaporator that is concentrated under reduced pressure after 4 DEG C of crystallizations, then dry through 100~120 DEG C
It is dry to produce CALCIUM PYRUVIC.
2. a kind of production method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin as claimed in claim 1, it is special
Levy and be that the calcium source mussel shell powder calcium carbonate content is calculated (in terms of butt) by 95%.
3. a kind of production method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin as claimed in claim 1, it is special
Levy and be described mussel shell melanin insoluble in acid, but be dissolved in diluted alkaline, have A-549 lung carcinoma cells compared with strong inhibitory activity.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710212471.2A CN107011155A (en) | 2017-03-22 | 2017-03-22 | A kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin |
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| CN201710212471.2A CN107011155A (en) | 2017-03-22 | 2017-03-22 | A kind of method that simultaneously synthesizing CALCIUM PYRUVIC is separated based on mussel shell melanin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266039A (en) * | 2018-09-21 | 2019-01-25 | 海南大学 | A kind of giant clam outer embrane colorant mixture and its extraction and concentration measuring method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215231A (en) * | 2007-12-26 | 2008-07-09 | 仲恺农业技术学院 | Method for preparing calcium salt by using shell as raw material |
| CN104365515A (en) * | 2014-11-25 | 2015-02-25 | 鲁东大学 | Breeding method of crassostrea gigas with high melanin content in soft parts |
-
2017
- 2017-03-22 CN CN201710212471.2A patent/CN107011155A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215231A (en) * | 2007-12-26 | 2008-07-09 | 仲恺农业技术学院 | Method for preparing calcium salt by using shell as raw material |
| CN104365515A (en) * | 2014-11-25 | 2015-02-25 | 鲁东大学 | Breeding method of crassostrea gigas with high melanin content in soft parts |
Non-Patent Citations (2)
| Title |
|---|
| 郝世鑫等: "紫贻贝贝壳和脉红螺厣中色素的提取与鉴定", 《海洋科学》 * |
| 陈忻 等: "九孔鲍壳的综合利用", 《福建水产》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109266039A (en) * | 2018-09-21 | 2019-01-25 | 海南大学 | A kind of giant clam outer embrane colorant mixture and its extraction and concentration measuring method |
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