Patent US4320050A successfully refreshed from Google Patents.
US4320050A
Expired / Lapsed
US
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Process for selectively extracting dyestuffs contained in cyanophyceae algae, the so-extracted dyestuffs and their use, particularly in foodstuffs
Assignee: IFP Energies nouvelles
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Filing: 1980-04-04
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Granted: 1982-03-16
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Expires: 2000-04-04
Abstract
Abstract Process for extracting dyestuffs and particularly a blue pigment, called phycocyanine, from cyanophyceae algae, particularly of the Spirulina species, comprising contacting said algae with a first aqueous phase containing calcium ions, separating therefrom the mass of algae and contacting it with a second aqueous phase of alkaline character, separating the algae therefrom and extracting phycocyanine from said second aqueous phase by subjecting the same to an ultrafiltration step for concentrating the solution and then to a drying step.
Inventors
- 👤 Michel Rebeller
- 👤 Pierre Yout
- 👤 Daniel Lonchamp
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 17:07
CPC Classifications
C; C09; C09B; C09B61/00; A; A23; A23L; A23L17/00; A23L17/60; A23L5/00; A23L5/40; A23L5/42; A23L5/46; C12; C12N; C12N1/00; C12N1/12; C12N1/125; C12P; C12P1/00; C12R; C12R2001/00; C12R2001/89; Y; Y10; Y10S; Y10S435/00; Y10S435/8215; Y10S435/946
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
170 words
A process for extracting phycocyanine from Cyanophycae algae, comprising the steps of: (a) contacting fresh Cyanophycae algae with a first aqueous phase containing calcium ions in an amount of from 0.02 to 0.2 ion-gram per liter, at a temperature, from 15° to 45° C., and under such conditions as to render the phycocyanine in said algae amenable to extraction with an aqueous alkaline solution; (b) separating resultant mass of algae from said first aqueous phase; (c) contacting said separated mass of algae with a second aqueous phase of an alkaline character comprising at least one compound selected from the group consisting of alkali metal carbonates, alkali metal bicarbonates, sodium hydroxide and potassium hydroxide, the normality thereof being from 0.001 normal to 0.1 normal, at a temperature from 15° to 45° C., for a sufficient time to transfer the phycocyanine from the algae to the second aqueous phase, and (d) separating from said second aqueous phase a mass of residual algae, said second aqueous phase containing phycocyanine in a dissolved state.
Claim 2
Dependent Claim
170 words
A process for extracting phycocyanine from Cyanophycae algae, comprising the steps of: (a) contacting fresh Cyanophycae algae with a first aqueous phase containing calcium ions in an amount of from 0.02 to 0.2 ion-gram per liter, at a temperature, from 15° to 45° C., and under such conditions as to render the phycocyanine in said algae amenable to extraction with an aqueous alkaline solution; (b) separating resultant mass of algae from said first aqueous phase; (c) contacting said separated mass of algae with a second aqueous phase of an alkaline character comprising at least one compound selected from the group consisting of alkali metal carbonates, alkali metal bicarbonates, sodium hydroxide and potassium hydroxide, the normality thereof being from 0.001 normal to 0.1 normal, at a temperature from 15° to 45° C., for a sufficient time to transfer the phycocyanine from the algae to the second aqueous phase, and (d) separating from said second aqueous phase a mass of residual algae, said second aqueous phase containing phycocyanine in a dissolved state.
Claim 3
Dependent Claim
25 words
A process according to claim 1, wherein the concentration of calcium ions in said first phase is from 0.045 to 0.09 ion gram per liter.
Claim 4
Dependent Claim
18 words
A process according to claim 1 wherein said aqueous phase containing calcium ions is a calcium chloride solution.
Claim 5
Dependent Claim
32 words
A process according to claim 1 wherein said aqueous phase containing calcium ions is used in a proportion of 5 to 30 kg per kg of algae, estimated in the dry state.
Claim 6
Dependent Claim
20 words
A process according to claim 1 wherein step (a) is performed over a period from 15 minutes to 1 hour.
Claim 7
Dependent Claim
15 words
A process according to claim 1 wherein the separation step (b) is performed by filtration.
Claim 8
Dependent Claim
29 words
A process according to claim 1 wherein said second aqueous phase of alkaline character is used in a proportion from 5 to 30 kg per kilogram of dry algae.
Claim 9
Dependent Claim
22 words
A process according to claim 1 wherein step (d) is followed with a step (e) of concentrating the phycocyanine solution by ultrafiltration.
Claim 10
Dependent Claim
26 words
A process according to claim 1 wherein the final phycocyanine solution is subjected to a subsequent drying step, whereby phycocyanine is obtained in a solid state.
Claim 11
Dependent Claim
15 words
A process according to claim 9, wherein the drying step is conducted by spray drying.
Claim 12
Dependent Claim
14 words
A process according to claim 9, wherein the drying step is performed by lyophilization.
Claim 13
Dependent Claim
71 words
A process according to claim 1 comprising additional steps of extracting carotenoid pigments as follows: one step of drying the mass of residual algae from step (d) and at least one step of extracting carotenoids, wherein resultant dried mass is treated with at least one organic solvent selective for carotenoids and there is separated a liquid solution containing the major portion of the carotenoids and a mass of reduced carotenoid content.
Claim 14
Dependent Claim
30 words
A process according to claim 12, wherein the light organic solvent used for extracting carotenoids is pure methanol, methanol admixed with a small amount of water, acetone or acetone-methanol mixtures.
Claim 15
Dependent Claim
31 words
A process according to claim 12 wherein the liquid solution containing the major portion of the carotenoids is subsequently evaporated to dryness so as to obtain a residue containing said carotenoids.
Claim 16
Dependent Claim
120 words
A process according to claim 14, wherein, from the residue containing the carotenoids there are separated two types of carotenoids: on the one hand β-carotene and free xanthophylls, on the other hand glycosided xanthophylls, by performing the following steps: contacting said residue with a polar organic solvent, and adding to the resultant liquid solution an agent for the fixation of the glycosided xanthophylls, evaporation of resultant mixture of liquid solution and fixation agent to dryness so as to obtain a solid mass, wherefrom are extracted in particular β-carotene and free xanthophylls by means of a non polar or weakly polar solvent, separation from the liquid solution containing β-carotene and the free xanthophylls, of the solid mass containing the glycosided xanthophylls.
Claim 17
Dependent Claim
44 words
A process according to claim 15, wherein the desorption of the glycosided xanthophylls from the solid mass containing them is performed by means of a polar organic solvent, and a solution of glycosided xanthophylls is separated from a solid mass containing said fixation agent.
Claim 18
Dependent Claim
58 words
A process according to claim 15, wherein said organic polar solvent is acetone, said agent for the fixation of glycosided xanthophylls is selected from starch, dextrose, wheat meal, sugars, sodium chloride, powdered cellulose, powdered alumina and powdered silica and said non-polar or weakly polar organic solvent is selected from one or more liquid saturated hydrocarbons, and petroleum ether.
Claim 19
Dependent Claim
18 words
A process according to claim 16, wherein said polar organic solvent is selected from acetone, methanol and ethanol.
Claim 20
Dependent Claim
15 words
A process according to claim 1 wherein the Cyanophyceae algae are of the Spirulina species.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-03-15 | 1985-09-14 | 1986-03-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-03-15 | 1989-09-14 | 1990-03-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-03-15 | 1993-09-14 | 1994-03-16 | $7700.00 | Window Closed / Lapsed |