CN104087009A - Method for extracting red flower haematochrome from red flower residue - Google Patents
Method for extracting red flower haematochrome from red flower residue Download PDFInfo
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- CN104087009A CN104087009A CN201410338257.8A CN201410338257A CN104087009A CN 104087009 A CN104087009 A CN 104087009A CN 201410338257 A CN201410338257 A CN 201410338257A CN 104087009 A CN104087009 A CN 104087009A
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- microcrystalline cellulose
- safflower
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Abstract
The invention discloses a method for extracting red flower haematochrome from red flower residue. The method comprises the steps of stirring and soaking dry red flower residue with red flower uranidin extracted in potassium carbonate liquor of a certain concentration at a room temperature, and filtering to obtain red flower haematochrome crude extracting liquor; adding microcrystalline cellulose into the crude extracting liquor, regulating pH to 3.0-5.0 by acetic acid, stirring for 30 minutes, stewing for 2 hours at the room temperature, and filtering to obtain clean microcrystalline cellulose which is adsorbed with the red flower haematochrome; soaking the microcrystalline cellulose in potassium carbonate liquor, stirring for 15 minutes at the room temperature, carrying out suction filtration, and collecting filtrate; adding citric acid into the filtrate to regulate pH to 3.0-5.0, placing for 10-12 hours at 5 DEG C, carrying out siphon to remove liquid supernatant, freezing and drying precipitates at -20 DEG C to obtain red flower haematochrome, wherein mean pure powder color value is detected to be not smaller than 200. The method disclosed by the invention is free of organic solvent residue, simple to operate, high in pigment purity and extracting efficiency and beneficial to industrial production, so that utilization rate of red flower materials is improved.
Description
Technical field
The present invention relates to a kind of extraction preparation method of safflower red pigment, specifically a kind of method of extracting safflower red pigment from extract the safflower slag carthamin yellow.
Background technology
Extractible natural pigment in safflower, mainly contains yellow pigment and haematochrome two classes.Yellow pigment is that carthamin yellow is water colo(u)r, and its content accounts for 20% ~ 30%; Be fat-soluble pigment and haematochrome is safflower red pigment, only account for 0.3% ~ 0.6%.Because haematochrome structure contains few water soluble hydroxy, so haematochrome is almost insoluble in acidic solution, but can be dissolved in diluted alkaline and part organic solvent, be relatively soluble in acetone and dimethyl formamide.Haematochrome less stable, be subject to the factors such as high temperature, strong acid, highly basic, metal ion, illumination, organic water solvent to affect and can fade gradually, and in leaching process, being subject to yellow pigment disturbs, therefore, from extract the safflower slag carthamin yellow, extract again safflower red pigment and must find purity and the extraction yield of suitable final an obtained safflower red pigment of technique guarantee.Have data to show, safflower red pigment can be made into color and luster scope from rose-red to bright cherry-red fat-soluble staining agent after treatment as natural dyestuff, can be widely used in the dyeing of the cosmetics of super quality such as lipstick, kermes.At present, existing a great deal of makeup use safflower red pigment as staining agent exactly in the world, can greatly reduce the harm of chemical dye to human body.But the research of safflower red pigment report is less, China Patent Publication No. is in the application of CN102295839, to disclose employing salting-out process to extract, ethyl acetate and ethanol purification, and use the nearly step of organic reagent to purify, obtain the method for safflower red pigment, owing to having used organic reagent in the method, inevitably have dissolvent residual, and complicated operation, cycle is longer, chroma loss is larger, and extraction yield is low, is unfavorable for suitability for industrialized production.And the method that adopts pH8-12 borate or phosphate buffered saline buffer to extract in safflower slag disclosed in the application that China Patent Publication No. is CN102031014, although concentrated through reverse osmosis membrane, but the red yield of the safflower calculating from disclosed data is 8 ‰ left and right, only have 3 ‰ left and right and the safflower containing in safflower is red, illustrate that the impurity containing in the red product of the safflower obtaining is more, and do not provide the data such as the red pure pink colour valency of concrete safflower.
Summary of the invention
The object of the invention is to provide a kind of method of extracting safflower red pigment from safflower slag, and the method organic solvent-free is residual, simple to operate, and pigment purity and extraction yield are high, are beneficial to suitability for industrialized production, has improved the utilization ratio of safflower raw material.
Technological process of the present invention is:
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge of crossing with water extraction after carthamin yellow, be that 1-3% solution of potassium carbonate stirs immersion 2-6 hour under room temperature with massfraction, filter, obtain filtrate; Slag charge with 5 times of deionization washings, filters again, merges above filtrate, obtains safflower red pigment crude extract; Wherein safflower slag charge is 1:10-20 with the ratio of solution of potassium carbonate weight;
(2) absorption
In above-mentioned crude extract, add Microcrystalline Cellulose, then use vinegar acid for adjusting pH to 3.0-5.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing Microcrystalline Cellulose 2-3 time, obtains having adsorbed the Microcrystalline Cellulose of safflower red pigment; Wherein crude extract is 400:1-3 with the ratio of Microcrystalline Cellulose weight;
(3) resolve
The solution of potassium carbonate that is 1-3% with massfraction soaks the Microcrystalline Cellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 3-5 time, collects filtrate each time; Wherein Microcrystalline Cellulose is 1:10 with the ratio of solution of potassium carbonate weight;
(4) refining
In filtrate, add lemon acid for adjusting pH to 3.0-5.0, place 10-12 hour at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment; After testing, average pure pink colour valency
>=200.
Mierocrystalline cellulose has Selective adsorption to safflower is red, but different Mierocrystalline celluloses is different with parsing degree to the absorption of the red Flos Carthami Huang of safflower.Microcrystalline Cellulose (the Microcrystalline cellulose using in above-mentioned steps; MCC) be natural cellulose through dilute acid hydrolysis free flowable imperceptible corynebacterium or the Powdered vesicular particle to levelling-off DP (LOOP); color is white or near-white; odorless, tasteless; granular size is generally at 20 ~ 80 Lm, and levelling-off DP (LODP) is 15 ~ 375; Do not have fibering and mobility is extremely strong.Water insoluble, diluted acid, organic solvent and grease are partly dissolved, moisten and rise in dilute alkaline soln, have higher reactivity worth in carboxymethylation, acetylize, esterification process.Owing to having compared with special propertys such as low polymerization degree and larger specific surface areas, Microcrystalline Cellulose is widely used in medicine, food, makeup and light industry industry.The present invention has optimized Microcrystalline Cellulose as the red sorbent material of safflower from 3 kinds of different Mierocrystalline celluloses (cotton, Microcrystalline Cellulose and lignocellulose), has reached reasonable technique effect, is one of innovative point of the present invention.
Meanwhile, the present invention is to vat liquor pH, solid-liquid ratio, and the processing parameters such as extraction time have carried out preferably, having obtained optimal processing parameter, and specific experiment process is as follows:
One, Mierocrystalline cellulose shaker test
In the situation that other processing condition are identical, adsorb respectively and to resolve safflower red with 3 kinds of different cellulose adsorbents (cotton, Microcrystalline Cellulose and lignocellulose), its recovery rate and look valency are as shown in table 1:
Table 1 Mierocrystalline cellulose shaker test
As can be seen from Table 1, adopt Microcrystalline Cellulose as sorbent material, recovery rate and the look valency of gained safflower red pigment are the highest.
Two, determining of optimum extraction condition
By to vat liquor concentration, solid-liquid ratio, the impact of the recovery rate of the factors such as extraction time on pigment, has determined the top condition of each factor.The results are shown in Table 2, table 3.
Test method: by extracting the extra dry red wine flower slag charge of sailor yellow, with the solution of potassium carbonate of certain proportion different concns, soak different time through stirring at room temperature, after filtration, slag charge filters after rinsing with 5 times of clear water, merges above filtrate, obtains safflower red pigment crude extract; In crude extract, add Microcrystalline Cellulose, the ratio 400:2 of extracting solution and Microcrystalline Cellulose, with vinegar acid for adjusting pH to 4.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and rinses the Microcrystalline Cellulose that has adsorbed safflower red pigment, by Impurity removal, the Microcrystalline Cellulose of safflower red pigment that obtained clean absorption; With 2% solution of potassium carbonate immersion Microcrystalline Cellulose, Microcrystalline Cellulose is 1:10 with the ratio of solution of potassium carbonate, stirring at room temperature 15 minutes, and suction filtration, repetitive operation is until resolve totally collection filtrate; Filtrate adds lemon acid for adjusting pH to 4.0, and low temperature is placed 12 hours, removes supernatant liquor, will precipitate lyophilize, obtains safflower red pigment product.
Table 2 level of factor table
Extract according to the listed condition of table 2, calculate safflower red pigment recovery rate.
Recovery rate (%)=
Wherein: G
1---the red charging capacity of safflower, kg;
G
2---the red pure grain weight amount of safflower, kg;
530---safflower clearance permit position look valency;
20000---reference colour valency.
Table 3 orthogonal test table
As can be drawn from Table 3, above three factors are R on the impact order of recovery rate
b>R
c>R
a, i.e. concentration of potassium carbonate > solid-liquid ratio > extraction time.Preferred embodiment is: A
1b
2c
3, i.e. extraction time 2 hours, concentration of potassium carbonate 2%(massfraction), solid-liquid ratio 1:15.
Three, determining of Microcrystalline Cellulose add-on and pH value
In salt of wormwood vat liquor, contain a large amount of impurity and a part of carthamin yellow, in order to obtain purer safflower red pigment, the present invention utilizes the Selective adsorption of Microcrystalline Cellulose to safflower red pigment, isolate safflower red pigment, in the time rinsing Microcrystalline Cellulose, impurity and yellow pigment are removed, but haematochrome does not lose, therefore use Microcrystalline Cellulose not only can improve recovery rate, can also obtain the safflower red pigment of high look valency.
By add the Microcrystalline Celluloses of different amounts in vat liquor, and the recovery rate that detects safflower red pigment is determined the optimum amount of Microcrystalline Cellulose.The results are shown in Table 4.
The consumption test of table 4 Microcrystalline Cellulose
From above-mentioned table, can find out, in the time that Microcrystalline Cellulose is 2:400 with the ratio of vat liquor, obtain higher recovery rate, considering selection Microcrystalline Cellulose is 2:400 with the ratio of vat liquor.
Secondly determine the pH value that acetic acid regulates, select by the recovery rate of investigating safflower red pigment, the results are shown in Table 5.
The pH value test of table 5 Microcrystalline Cellulose absorption safflower red pigment
From above-mentioned table, can find out, when the pH value in the time that Microcrystalline Cellulose adsorbs is 4.0, obtain higher recovery rate, therefore, selecting vinegar acid for adjusting pH value is 4.0.
Finally Microcrystalline Cellulose is carried out to die-away test, it the results are shown in Table 6.
Table 6 Microcrystalline Cellulose absorption decay experiment
As can be seen from the above table, after the use of Microcrystalline Cellulose is approximately 5 times adsorptive power decline very fast, therefore use 5 times just to need to change Microcrystalline Cellulose in producing.
Four, Microcrystalline Cellulose is resolved
The solution of potassium carbonate lixiviate safflower red pigment of the experimental selection 2% before cause, soaks Microcrystalline Cellulose therefore also press 1:10 with 2% solution of potassium carbonate while parsing, stirring at room temperature 15 minutes, and suction filtration, repetitive operation is until parsing totally, is collected filtrate.
The present invention compared with prior art, due to the Selective adsorption that utilizes Microcrystalline Cellulose to safflower red pigment, isolates safflower red pigment, while rinsing Microcrystalline Cellulose again, impurity and yellow pigment are removed, but haematochrome does not lose, and reduce impurity, improved purity; Employing optimal processing parameter is produced, and yield can reach more than 2.5 ‰, obtains average pure pink colour valency
530nm>=200, method is simple, easy to operate, and the cycle is short, and influence factor is few, and cost is low, environmental protection, Microcrystalline Cellulose reusable edible, is conducive to suitability for industrialized production.
Embodiment
Embodiment 1
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge 10kg crossing with water extraction after carthamin yellow, the solution of potassium carbonate 150kg that is 2% with massfraction stirs and soaks 2 hours under room temperature, filters, and obtains filtrate; Slag charge with 5 times of deionization washings 5 times, filters again, merges above filtrate, obtains the about 400kg of safflower red pigment crude extract;
(2) absorption
In above-mentioned crude extract, add Microcrystalline Cellulose 2kg, then use vinegar acid for adjusting pH to 4.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing Microcrystalline Cellulose 3 times, obtains having adsorbed the Microcrystalline Cellulose of safflower red pigment;
(3) resolve
The solution of potassium carbonate 20kg that is 2% with massfraction soaks the Microcrystalline Cellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 5 times, collects filtrate each time;
(4) refining
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment 28g, and yield is 2.8 ‰; After testing, pure pink colour valency
=248A.
Embodiment 2
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge 10kg crossing with water extraction after carthamin yellow, the solution of potassium carbonate 150kg that is 1% with massfraction stirs and soaks 6 hours under room temperature, filters, and obtains filtrate; Slag charge with 5 times of deionization washings 5 times, filters again, merges above filtrate, obtains the about 400kg of safflower red pigment crude extract;
(2) absorption
In above-mentioned crude extract, add Microcrystalline Cellulose 1kg, then use vinegar acid for adjusting pH to 3.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing Microcrystalline Cellulose 3 times, obtains having adsorbed the Microcrystalline Cellulose of safflower red pigment;
(3) resolve
The solution of potassium carbonate 20kg that is 1% with massfraction soaks the Microcrystalline Cellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 5 times, collects filtrate each time;
(4) refining
In filtrate, add lemon acid for adjusting pH to 3.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment 25g, and yield is 2.5 ‰; After testing, pure pink colour valency
=216A.
Embodiment 3
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge 10kg crossing with water extraction after carthamin yellow, the solution of potassium carbonate 200kg that is 3% with massfraction stirs and soaks 4 hours under room temperature, filters, and obtains filtrate; Slag charge with 5 times of deionization washings 4 times, filters again, merges above filtrate, obtains the about 400kg of safflower red pigment crude extract;
(2) absorption
In above-mentioned crude extract, add Microcrystalline Cellulose 3kg, then use vinegar acid for adjusting pH to 5.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing Microcrystalline Cellulose 3 times, obtains having adsorbed the Microcrystalline Cellulose of safflower red pigment;
(3) resolve
The solution of potassium carbonate 30kg that is 3% with massfraction soaks the Microcrystalline Cellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 5 times, collects filtrate each time;
(4) refining
In filtrate, add lemon acid for adjusting pH to 5.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment 27g, and yield is 2.7 ‰; After testing, pure pink colour valency
=233A.
Embodiment 4
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge 10kg crossing with water extraction after carthamin yellow, the solution of potassium carbonate 150kg that is 2% with massfraction stirs and soaks 2 hours under room temperature, filters, and obtains filtrate; Slag charge with 5 times of deionization washings 5 times, filters again, merges above filtrate, obtains the about 400kg of safflower red pigment crude extract;
(2) absorption
In above-mentioned crude extract, add cotton 2kg, then use vinegar acid for adjusting pH to 4.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing cotton 3 times, obtains having adsorbed the cotton of safflower red pigment;
(3) resolve
The solution of potassium carbonate 20kg that is 2% with massfraction soaks the cotton of having adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 5 times, collects filtrate each time;
(4) refining
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment 3g, after testing, and pure pink colour valency
=70A.
Embodiment 5
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge 10kg crossing with water extraction after carthamin yellow, the solution of potassium carbonate 150kg that is 2% with massfraction stirs and soaks 2 hours under room temperature, filters, and obtains filtrate; Slag charge with 5 times of deionization washings 5 times, filters again, merges above filtrate, obtains the about 400kg of safflower red pigment crude extract;
(2) absorption
In above-mentioned crude extract, add lignocellulose 2kg, then use vinegar acid for adjusting pH to 4.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing cotton 3 times, obtains having adsorbed the lignocellulose of safflower red pigment;
(3) resolve
The solution of potassium carbonate 20kg that is 2% with massfraction soaks the lignocellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 5 times, collects filtrate each time;
(4) refining
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment 14.4g, after testing, and pure pink colour valency
=123A.
Above-described embodiment 1 is owing to having adopted optimum process condition of the present invention, and therefore, the safflower red pigment yield and the purity that obtain are the highest.
Claims (1)
1. from safflower slag, extract a method for safflower red pigment, it is characterized in that being formed by following step:
(1) the extraction of safflower red pigment
By the extra dry red wine flower slag charge of crossing with water extraction after carthamin yellow, be that 1-3% solution of potassium carbonate stirs immersion 2-6 hour under room temperature with massfraction, filter, obtain filtrate; Slag charge with 5 times of deionization washings, filters again, merges above filtrate, obtains safflower red pigment crude extract; Wherein safflower slag charge is 1:10-20 with the ratio of solution of potassium carbonate weight;
(2) absorption
In above-mentioned crude extract, add Microcrystalline Cellulose, then use vinegar acid for adjusting pH to 3.0-5.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and uses deionized water rinsing Microcrystalline Cellulose 2-3 time, obtains having adsorbed the Microcrystalline Cellulose of safflower red pigment; Wherein crude extract is 400:1-3 with the ratio of Microcrystalline Cellulose weight;
(3) resolve
The solution of potassium carbonate that is 1-3% with massfraction soaks the Microcrystalline Cellulose that has adsorbed safflower red pigment, stirring at room temperature 15 minutes, and suction filtration, obtains filtrate; Repetitive operation 3-5 time, collects filtrate each time; Wherein Microcrystalline Cellulose is 1:10 with the ratio of solution of potassium carbonate weight;
(4) refining
In filtrate, add lemon acid for adjusting pH to 3.0-5.0, place 10-12 hour at 5 DEG C, supernatant liquor is removed in siphon, will be deposited in lyophilize at-20 DEG C, obtains safflower red pigment; After testing, average pure pink colour valency
>=200.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109577028A (en) * | 2018-11-30 | 2019-04-05 | 泉州市正域数码科技有限公司 | A kind of red jet ink and preparation method thereof |
| CN110229866A (en) * | 2019-06-28 | 2019-09-13 | 江南大学 | The detection method of microorganism in a kind of water environment |
| CN111944329A (en) * | 2020-09-09 | 2020-11-17 | 江西丹霞生物科技股份有限公司 | Preparation process for preparing carthamus red pigment and product thereof |
| CN112521769A (en) * | 2020-11-25 | 2021-03-19 | 清华大学 | Safflower red pigment and preparation method and dyeing method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110229866B (en) * | 2019-06-28 | 2020-08-04 | 江南大学 | Method for detecting microorganisms in water environment |
| CN111944329A (en) * | 2020-09-09 | 2020-11-17 | 江西丹霞生物科技股份有限公司 | Preparation process for preparing carthamus red pigment and product thereof |
| CN112521769A (en) * | 2020-11-25 | 2021-03-19 | 清华大学 | Safflower red pigment and preparation method and dyeing method thereof |
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