CN101461513B - Method for preparing water-soluble cochinilin color lake - Google Patents
Method for preparing water-soluble cochinilin color lake Download PDFInfo
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- CN101461513B CN101461513B CN2009100448695A CN200910044869A CN101461513B CN 101461513 B CN101461513 B CN 101461513B CN 2009100448695 A CN2009100448695 A CN 2009100448695A CN 200910044869 A CN200910044869 A CN 200910044869A CN 101461513 B CN101461513 B CN 101461513B
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Abstract
The invention relates to a preparation of water soluble lake of carminic acid, including steps of: (1) preparation of cochineal color acid mother liquor; (2) laking; (3) generation of water soluble lake. The water soluble lake of carminic acid can be widely applied to food product, candy, beverage, medicament and cosmetics.
Description
Technical field
The present invention relates to a kind of carminic acid, be specifically related to a kind of preparation of water soluble lake of carminic.
Background technology
Carminic acid is a kind of anthraquinone class natural colouring matter; It mainly is present in female cochineal (Dactylopiuscoccus costa) (having another name called " Coccus cacti the L. ") body; It is made a living with nopal (Nopaleacoccinellifera), Opuntia ficus (Opuntia fidus indica) and other cactus plant, and these cactuses generally are planted in the desert area like Mexico and Sino-U.S.'s South America.According to the difference of pH value, the color gamut of carminic acid colouring agent can from orange to redness again to purple, general common carminic acid pigment and derivative thereof are referred to as alkermes, this pigment is widely used in food and the medicine field.
The extraction of pigment generally extracts through water or alcohol and obtains in the cochineal stem body.But in the process of extraction carminic acid, the protein in the insect bodies is also taken out of with the material of other water solubles or alcohol, thereby is present in the extract.According to relevant report, contain allergenic impurity protein in the alkermes and itself be the factors affecting the disease [Ann Allergy Asthma, 84 volumes (5), 549-552,2000] in the allergic disease, it is irritated to that is to say that cochineal albumen can cause the part crowd.
In order to solve this anaphylaxis problem; A series of patents of Japan San-Ei Gen F. F. I. INC application; CN1388821A for example; EP1318178A1, US2002/0058016 disclose and have a kind ofly adopted protease hydrolytic and utilize macroreticular resin or macroreticular resin separates purify carminic acid and remove cochineal protein of the method that combines with film.But, therefore limited the application of carminic acid greatly because the maximum wavelength fluctuation range of carminic acid product its color under different pH value conditions is wider.
Cochinilin color lake is a kind of chelating class color lake compound that is combined with aluminium ion and calcium ion by carminic acid, this color lake be under the water condition carminic acid and aluminium and calcium ion reaction and product.Patent CN101061185A discloses a kind of employing 40%～80% carminic acid and 10%～30% non-cochineal insect protein is the method that raw material and aluminium, calcium ion reaction generate water-insoluble cochinilin color lake.The document does not provide other after simple process, directly to generate the content of water-soluble cochinilin color lake about adopting the cochineal extract except the reaction condition that proposes the water-insoluble cochinilin color lake of preparation.
Summary of the invention
Technical scheme to be solved by this invention provides a kind of preparation of water soluble lake of carminic, its process route economy, easy, and the water-soluble carminic acid of preparing does not contain potential anaphylactogen cochineal albumen.
In order to achieve the above object, the present invention adopts following technical scheme to realize:
A kind of preparation of water soluble lake of carminic comprises the steps:
(1) preparation of carmic acid mother liquor
Adding pH is 8.5～9 alkali lye in the cochineal stem body; Carminic acid in the extraction cochineal stem body; Add hydrolysising protease then and carry out proteolysis, filter behind the adjusting pH to 1-2.5, will filtrate then and remove the cochineal protein of molecular weight greater than 6000Da through milipore filter;
(2) color lakeization
When to be concentrated to carminic acid concentration be 2wt%～5wt% with above-mentioned carmic acid mother liquor, be warming up to 60 ℃-100 ℃, add alum solution and calcium chloride solution, regulate pH to 1-3 after insulation reaction 2-4 hour, make the color lake deposition and filter;
(3) generation in water-soluble color lake
It is in 20 ℃-80 ℃ the hot water that the above-mentioned cochinilin color lake filter cake that obtains is dropped into temperature, regulates pH to 7-10, insulated and stirred 0.5-2 hour, and after the filtration, drying.
Alkali lye in the said step (1) is the cushioning liquid of sodium carbonate, sodium acid carbonate or glycine and NaOH; Because leaching process is the dispose procedure of walking unhurriedly that a kind of carminic acid is converted into sodium salt; Adopt pH can accelerate the rate of release of carminic acid, reduce extraction time in 8.5～9 scope; Can make simultaneously carminic acid be in receptive phase in the situation that alkali condition decomposes again, its resolution ratio is less than 1.5%.
Protease in the said step (1) is neutral proteinase or animal proteolytic enzyme, its pH≤9, and the proteolysis condition changes according to the difference of the enzyme of selecting.
Milipore filter in the said step (1) must can molecular cut off greater than the material of 6000Da.
Carmic acid mother liquor in the said step (2) comprises: carmine color acid butt 5wt%-20wt%; With cochineal protein hydrolysate butt 5wt%-20wt%.
The carmic acid in the said step (2) and the mol ratio of alum are 1: 0.5-5, the mol ratio of carmic acid and calcium chloride is 1: 0.5-9.
The cochinilin color lake filter cake in the said step (3) and the weight ratio of water are 1: 1-15.
PH in the said step (3) is preferably 8-9.
The application of said water-soluble cochinilin color lake in food products, candy, beverage, medicine and cosmetics.
Because carminic acid belongs to the hydroxy-anthraquione derivative, according to its molecular structure, belong to madder type hydroxy-anthraquione derivative, can be water-soluble, diluted acid, diluted alkaline, ethanol, propane diols, be insoluble to ether or edible oil, can adopt therefore that alkali is carried, alcohol extracting, supercritical CO
2Extracting three kinds of modes extracts the carminic acid in the cochineal.Supercritical CO wherein
2Extraction just proposed in recent years, and relevant report is fewer, and needed specific laboratory apparatus, therefore was difficult to extensive use.The present invention carries, after alcohol extracting experiment compares, finds that alkali puies forward effect and be superior to the alcohol extracting effect through a series of alkali, considers follow-up color lake chemical industry preface simultaneously, therefore confirms to adopt the alkali lye method for distilling to carry out the extraction of carminic acid.
But for the extraction of carminic acid, its influence factor possibly also have temperature, pH, extraction time, and the present invention has carried out orthogonal experiment to confirm the optimum condition of extraction process to this.Fig. 2 is the pH of carminic acid and the graph of a relation of carminic acid resolution ratio, from figure, can find that after pH was greater than 10, the decomposition rate of carminic acid obviously increased.
The film device that the present invention simultaneously also adopts the membrane molecule interception to be respectively 6000Da, 3000Da, 1000Da experimentizes to the coccinic acid extract, finds directly to adopt membrane separation technique also can effectively remove the potential allergy protein of molecular weight greater than 6000Da; Simultaneously according to experiment also explain pH acid with neutrallty condition under the effect of separating through film better; And under alkali condition owing to there is the decomposition of carminic acid; So the yield of product lower (part is decomposed), the environment for use of therefore explanation the best should be carried out under neutrality or solutions of weak acidity; And three kinds of films that experiment is adopted all can be removed the potential allergy protein of molecular weight greater than 6000Da.
CN1388821A compares with patent, and the preparation process of carmic acid mother liquor of the present invention has been skipped the adsorption treatment process, has simplified preparation technology, has improved the carminic acid product unit output capacity that does not contain potential allergic protein matter greatly; Prepared product is to contain more molecular weight to be lower than the protein of 6000Da and the carminic acid mother liquor of other impurity, and wherein color acid content is 5%～20%, and protein content is 5%～20%.And color lake of the present invention employing is to utilize the carminic acid extract directly through the low content carminic acid mother liquor of ultrafiltration membrane treatment, and patent CN101061185A color lake employing is the high-load carminic acid mother liquor of extract after adsorption treatment and ion-exchange treatment/film processing/acid treatment.The present invention adopts the lower carminic acid mother liquor of color acid content value to carry out the color lake reaction; Reduced ingredient requirement to the carminic acid mother liquor; Thereby cost for purification rising and environmental pollution that source carminic acid mother liquor is caused have been reduced; Along with the simplification of process route, improved the unit output of cochinilin color lake product simultaneously.
CN101061185A compares with patent, and the present invention adopts control color lake reactant concentration, and (weight ratio of cochinilin color lake filter cake and water is 1: 1-15); PH value scope 7～10 is preferably 8～9; Alkali lye is the cushioning liquid of sodium carbonate, sodium acid carbonate, glycine and NaOH.The cushioning liquid (pH is 8.6～9.0) that is preferably glycine and NaOH carries out the production of water-soluble cochinilin color lake.And this patent only has the statement of " it can be used for making cochineal solution and water miscible carmine powder the carmine lake that obtains " in the explanation of embodiment, and pH scope that concrete experiment condition wherein such as water-soluble color lake generate and reactant concentration etc. are all mentioned.
Description of drawings
Further specify the present invention below in conjunction with the accompanying drawing and the specific embodiment.
Fig. 1 is a chemical equation of the present invention.
Fig. 2 is the pH of carminic acid of the present invention and the graph of a relation of carminic acid resolution ratio.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, below in conjunction with concrete diagram, further set forth the present invention.
Embodiment 1
Take by weighing cochineal stem body powder 200g, add the sodium carbonate liquor of 3000mL pH=8.5, be warming up to 95 ℃; Be incubated 1 hour, 100 eye mesh screens are crossed in the cooling back, and regulate pH to 6.7; Add neutral proteinase 12g, after 6 hours, cooling is also regulated pH=1.9 67 ℃ of insulations.Filter and with extract through the AFC milipore filter.Cross coating solution and be evaporated to 1000mL, add 5% alum solution 100g after regulating pH to 5.6 and being warming up to 85 ℃, insulated and stirred adds 5% calcium chloride solution 40g after 2 hours, continue insulation after 1 hour, cooling.Regulate pH to 2.4, make the color lake deposition.After the filtration, filter cake is dropped in the 250mL water, be warming up to 60 ℃; Regulate pH to 9.4 then, be incubated 1 hour, obtaining content behind filtration and the drying under reduced pressure is 53%; Protein content is 12%; Yield is 89.58% water-soluble carminic acid aluminium color lake, and adopts the SDS-PAGE analytical method that it is carried out protein detection, does not have and finds to contain potential allergen protein (molecular weight is higher than 6000Da).
Embodiment 2
Take by weighing cochineal stem body powder 200g, add the glycine of 3000mL pH=8.6 and the cushioning liquid solution of NaOH, be warming up to 100 ℃; Be incubated 1 hour; 100 eye mesh screens are crossed in the cooling back, and regulate pH to 7.9, add animal proteolytic enzyme 10g; After 6 hours, cooling is also regulated pH=2.2 56 ℃ of insulations.Filter and with extract through the AFC milipore filter.Cross coating solution and be evaporated to 1000mL, add 5% alum solution 120g after regulating pH to 5.2 and being warming up to 100 ℃, insulated and stirred adds 5% calcium chloride solution 35g after 2 hours, continue insulation after 1 hour, cooling.Regulate pH to 2.1, make the color lake deposition.After the filtration, filter cake is dropped in the 250mL water, be warming up to 80 ℃; Regulate pH to 8.6 then, be incubated 1 hour, obtaining content behind filtration and the drying under reduced pressure is 59%; Protein content is 16%; Yield is 95.37% water-soluble carminic acid aluminium color lake, and adopts the SDS-PAGE analytical method that it is carried out protein detection, does not have and finds to contain potential allergen protein (molecular weight is higher than 6000Da).
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; The present invention is not restricted to the described embodiments; That describes in the foregoing description and the specification just explains principle of the present invention; Under the prerequisite that does not break away from spirit and scope of the invention, the present invention also has various changes and modifications, and these variations and improvement all fall in the scope of the invention that requires protection.The present invention requires protection domain to be defined by appending claims and equivalent thereof.
Claims (8)
1. a preparation of water soluble lake of carminic is characterized in that, comprises the steps:
(1) preparation of carmic acid mother liquor
Adding pH is 8.5～9 alkali lye in the cochineal stem body; Carminic acid in the extraction cochineal stem body; Add hydrolysising protease then and carry out proteolysis, filter behind the adjusting pH to 1-2.5, will filtrate then and remove the cochineal protein of molecular weight greater than 6000Da through milipore filter;
(2) color lakeization
When to be concentrated to carminic acid concentration be 2wt%～5wt% with above-mentioned carmic acid mother liquor, be warming up to 60 ℃-100 ℃, add alum solution and calcium chloride solution, regulate pH to 1-3 after insulation reaction 2-4 hour, make the color lake deposition and filter;
(3) generation in water-soluble color lake
It is in 20 ℃-80 ℃ the hot water that the above-mentioned cochinilin color lake filter cake that obtains is dropped into temperature, regulates pH to 7-10, insulated and stirred 0.5-2 hour, and after the filtration, drying.
2. preparation method according to claim 1 is characterized in that: the alkali lye in the said step (1) is the cushioning liquid of sodium carbonate, sodium acid carbonate or glycine and NaOH.
3. preparation method according to claim 1 is characterized in that: the protease in the said step (1) is neutral proteinase or animal proteolytic enzyme, its pH≤9.
4. preparation method according to claim 1 is characterized in that: the milipore filter in the said step (1) must can molecular cut off greater than the material of 6000Da.
5. preparation method according to claim 1 is characterized in that: the carmic acid mother liquor in the said step (2) comprises: carmine color acid butt 5wt%-20wt%; With cochineal protein hydrolysate butt 5wt%-20wt%.
6. preparation method according to claim 1 is characterized in that: the carmic acid in the said step (2) and the mol ratio of alum are 1: 0.5-5, the mol ratio of carmic acid and calcium chloride is 1: 0.5-9.
7. preparation method according to claim 1 is characterized in that: the cochinilin color lake filter cake in the said step (3) and the weight ratio of water are 1: 1-15.
8. require each described preparation method of 1-7 according to aforesaid right, it is characterized in that: the pH in the said step (3) is 8-9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100448695A CN101461513B (en) | 2009-01-05 | 2009-01-05 | Method for preparing water-soluble cochinilin color lake |
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| CN2009100448695A CN101461513B (en) | 2009-01-05 | 2009-01-05 | Method for preparing water-soluble cochinilin color lake |
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| CN101461513A CN101461513A (en) | 2009-06-24 |
| CN101461513B true CN101461513B (en) | 2012-07-25 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102702775A (en) * | 2012-01-18 | 2012-10-03 | 天津天康源生物技术有限公司 | High-stability natural compounded haematochrome preparation |
| CN108795096A (en) * | 2018-05-18 | 2018-11-13 | 山东中惠生物科技股份有限公司 | Natural plants color lake and preparation method thereof |
| CN109021615A (en) * | 2018-09-12 | 2018-12-18 | 乐象永续科技（杭州）有限公司 | Preparation method, color lake and the application in color lake |
| CN110183873B (en) * | 2019-06-14 | 2020-10-16 | 北京工商大学 | Preparation method of edible lake based on calcium carbonate |
| CN112831194B (en) * | 2020-12-24 | 2023-03-31 | 赣州华汉生物科技有限公司 | Cochineal red lake without aluminum salt and preparation method thereof |
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Non-Patent Citations (1)
| Title |
|---|
| 余启洪, 吴巧玲.《胭脂虫红色素提取方法的研究进展》.《农产品加工·学刊》.2008,第*卷(第9 期),59-61. * |
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Effective date of registration: 20140321 Address after: 200065 No. 1238, Putuo District, Shanghai, Zhongshan North Road Patentee after: Shanghai Dyestuffs Research Institute Co.,Ltd. Patentee after: SHANGHAI HUAYUAN INDUSTRY & COMMERCE GENERAL Co. Address before: 200065 No. 1238, Putuo District, Shanghai, Zhongshan North Road Patentee before: Shanghai Dyestuffs Research Institute Co.,Ltd. |
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