CN104087009B - A kind of method extracting safflower red pigment from safflower slag - Google Patents
A kind of method extracting safflower red pigment from safflower slag Download PDFInfo
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Abstract
The invention discloses a kind of method extracting safflower red pigment from safflower slag, be to extract the extra dry red wine flower slag charge of carthamin yellow, use certain density solution of potassium carbonate, soak through stirring at room temperature, filter, obtain safflower red pigment crude extract; Add Microcrystalline Cellulose in crude extract, with vinegar acid for adjusting pH to 3.0-5.0, stir 30 minutes, room temperature leaves standstill 2 hours, filters, and obtains clean having adsorbed the Microcrystalline Cellulose of safflower red pigment; Soak Microcrystalline Cellulose with solution of potassium carbonate, stirring at room temperature 15 minutes, suction filtration, collect filtrate; Filtrate adds lemon acid for adjusting pH to 3.0-5.0, and place 10-12 hour at 5 DEG C, supernatant liquor is removed in siphon, and lyophilize at being deposited in-20 DEG C, namely obtains safflower red pigment, after testing, and average pure pink colour valency?
Description
Technical field
The present invention relates to a kind of extraction preparation method of safflower red pigment, specifically a kind of method extracting safflower red pigment from the safflower slag after extraction carthamin yellow.
Background technology
Extractible natural pigment in safflower, mainly contains yellow pigment and haematochrome two class.Yellow pigment and carthamin yellow are water colo(u)rs, and its content accounts for 20% ~ 30%; And haematochrome and safflower red pigment are fat-soluble pigments, only account for 0.3% ~ 0.6%.Because haematochrome structure contains very little water soluble hydroxy, so haematochrome is almost insoluble in an acidic solution, but diluted alkaline and part organic solvent can be dissolved in, compare and be soluble in acetone and dimethyl formamide.Haematochrome less stable, affect can fade gradually by factors such as high temperature, strong acid, highly basic, metal ion, illumination, organic water solvents, and in leaching process, be subject to yellow pigment interference, therefore, extract from extracting the safflower slag after carthamin yellow purity and the extraction yield that safflower red pigment must find suitable final an obtained safflower red pigment of technique guarantee again.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 high-grade cosmetic coloration 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 disclose in the application of CN102295839 to adopt salting-out process to extract, ethyl acetate and ethanol purification, and uses the nearly step of organic reagent to purify, obtain the method for safflower red pigment, owing to employing organic reagent in the method, inevitably have dissolvent residual, and complicated operation, cycle is longer, chroma loss is comparatively large, and extraction yield is low, is unfavorable for suitability for industrialized production.And China Patent Publication No. is disclose the method adopting pH8-12 borate or phosphate buffered saline buffer to extract in safflower slag in the application of CN102031014, although concentrate through reverse osmosis membrane, but be about 8 ‰ from the red yield of safflower that disclosed data calculate, and the safflower contained in safflower is red only has about 3 ‰, illustrate that the impurity contained in the red product of the safflower obtained 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 extracting safflower red pigment from safflower slag, the method organic solvent-free remain, simple to operate, pigment purity and extraction yield high, be beneficial to suitability for industrialized production, improve the utilization ratio of safflower raw material.
Technological process of the present invention is:
(1) the extraction of safflower red pigment
The flower of the extra dry red wine after carthamin yellow slag charge will be crossed with water extraction, be that 1-3% solution of potassium carbonate soaks 2-6 hour in stirred at ambient temperature with massfraction, filter, obtain filtrate; Slag charge with 5 times of deionization washings, filters, merges above filtrate, obtain safflower red pigment crude extract again; Wherein safflower slag charge is 1:10-20 with the ratio of solution of potassium carbonate weight;
(2) adsorb
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 with deionized water rinsing Microcrystalline Cellulose 2-3 time, namely obtains the Microcrystalline Cellulose having adsorbed safflower red pigment; Wherein crude extract is 400:1-3 with the ratio of Microcrystalline Cellulose weight;
(3) resolve
Soak with the solution of potassium carbonate that massfraction is 1-3% and adsorbed the Microcrystalline Cellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 3-5 time, collects each filtrate; Wherein Microcrystalline Cellulose is 1:10 with the ratio of solution of potassium carbonate weight;
(4) refine
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, and lyophilize at being deposited in-20 DEG C, namely 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 safflower red Flos Carthami Huang.Microcrystalline Cellulose (the Microcrystallinecellulose used in above-mentioned steps; MCC) be natural cellulose through dilute acid hydrolysis to the free flowable imperceptible corynebacterium of levelling-off DP (LOOP) or powdery porous shape particle; color is white or near-white; odorless, tasteless; granular size is generally at 20 ~ 80Lm, and levelling-off DP (LODP) is 15 ~ 375; Do not have a fibering and mobility is extremely strong.Water insoluble, diluted acid, organic solvent and grease, be partly dissolved, moisten and rise, in carboxymethylation, acetylize, esterification process, have higher reactivity worth in dilute alkaline soln.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), and reaching reasonable technique effect, is one of innovative point of the present invention.
Meanwhile, the present invention to vat liquor pH, solid-liquid ratio, the processing parameters such as extraction time carry out preferably, and obtain optimal processing parameter, specific experiment process is as follows:
One, Mierocrystalline cellulose shaker test
When other processing condition are identical, to adsorb respectively with 3 kinds of different cellulose adsorbents (cotton, Microcrystalline Cellulose and lignocellulose) and to resolve safflower red, its recovery rate and look valency 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, the determination of optimum extraction condition
By to vat liquor concentration, solid-liquid ratio, the factors such as extraction time, on the impact of the recovery rate of pigment, determine the top condition of each factor.The results are shown in Table 2, table 3.
Test method: will extract 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; Microcrystalline Cellulose is added in crude extract, 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 and has adsorbed the Microcrystalline Cellulose of safflower red pigment, by Impurity removal, obtain clean having adsorbed the Microcrystalline Cellulose of safflower red pigment; Soak Microcrystalline Cellulose with 2% solution of potassium carbonate, Microcrystalline Cellulose is 1:10 with the ratio of solution of potassium carbonate, stirring at room temperature 15 minutes, suction filtration, and repetitive operation, until resolve clean, collects filtrate; Filtrate adds lemon acid for adjusting pH to 4.0, and low temperature places 12 hours, removes supernatant liquor, and pellet frozen is dry, obtains safflower red pigment product.
Table 2 level of factor table
Listed by table 2, condition is extracted, and calculates 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, the impact order of above Three factors on recovery rate is R
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, the determination of Microcrystalline Cellulose add-on and pH value
In salt of wormwood vat liquor, containing a large amount of impurity and a part of carthamin yellow, in order to obtain purer safflower red pigment, the present invention utilizes Microcrystalline Cellulose to the Selective adsorption of safflower red pigment, isolate safflower red pigment, when rinsing Microcrystalline Cellulose, impurity and yellow pigment are removed, but haematochrome does not lose, therefore use Microcrystalline Cellulose not only can improve recovery rate, the safflower red pigment of High color values can also be obtained.
By adding the Microcrystalline Cellulose of different amount in vat liquor, and the recovery rate detecting safflower red pigment is to determine the optimum amount of Microcrystalline Cellulose.The results are shown in Table 4.
The consumption test of table 4 Microcrystalline Cellulose
As can be seen from above-mentioned table, when Microcrystalline Cellulose is 2:400 with the ratio of vat liquor, obtain higher recovery rate, consider and select Microcrystalline Cellulose to be 2:400 with the ratio of vat liquor.
Next determines the pH value that acetic acid regulates, and is selected, the results are shown in Table 5 by the recovery rate investigating safflower red pigment.
The pH value test of table 5 Microcrystalline Cellulose absorption safflower red pigment
As can be seen from above-mentioned table, when the pH value when Microcrystalline Cellulose adsorbs is 4.0, obtain higher recovery rate, therefore, select acetic acid adjust ph to be 4.0.
Finally carry out die-away test to Microcrystalline Cellulose, it the results are shown in Table 6.
Table 6 Microcrystalline Cellulose absorption decay test
As can be seen from the above table, after the use of Microcrystalline Cellulose is approximately 5 times, adsorptive power declines very fast, therefore uses in producing and just need for 5 times to change Microcrystalline Cellulose.
Four, Microcrystalline Cellulose is resolved
Because of the solution of potassium carbonate lixiviate safflower red pigment of experimental selection 2% before, therefore the solution of potassium carbonate also with 2% when resolving presses 1:10 immersion Microcrystalline Cellulose, stirring at room temperature 15 minutes, suction filtration, and repetitive operation, until resolve clean, collects filtrate.
The present invention compared with prior art, owing to utilizing Microcrystalline Cellulose to the Selective adsorption of safflower red pigment, isolates safflower red pigment, when rinsing Microcrystalline Cellulose again, impurity and yellow pigment are removed, but haematochrome does not lose, and decrease impurity, improve 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, and easy to operate, the cycle is short, and influence factor is few, and cost is low, environmental protection, and Microcrystalline Cellulose reusable edible, is conducive to suitability for industrialized production.
Embodiment
Embodiment 1
(1) the extraction of safflower red pigment
By crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 2 hours with the solution of potassium carbonate 150kg that massfraction is 2% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 5 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract and be about 400kg;
(2) adsorb
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 with deionized water rinsing Microcrystalline Cellulose 3 times, namely obtains the Microcrystalline Cellulose having adsorbed safflower red pigment;
(3) resolve
Soak with the solution of potassium carbonate 20kg that massfraction is 2% and adsorbed the Microcrystalline Cellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
(4) refine
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, lyophilize at being deposited in-20 DEG C, namely 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 crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 6 hours with the solution of potassium carbonate 150kg that massfraction is 1% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 5 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract and be about 400kg;
(2) adsorb
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 with deionized water rinsing Microcrystalline Cellulose 3 times, namely obtains the Microcrystalline Cellulose having adsorbed safflower red pigment;
(3) resolve
Soak with the solution of potassium carbonate 20kg that massfraction is 1% and adsorbed the Microcrystalline Cellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
(4) refine
In filtrate, add lemon acid for adjusting pH to 3.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, lyophilize at being deposited in-20 DEG C, namely 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 crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 4 hours with the solution of potassium carbonate 200kg that massfraction is 3% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 4 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract and be about 400kg;
(2) adsorb
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 with deionized water rinsing Microcrystalline Cellulose 3 times, namely obtains the Microcrystalline Cellulose having adsorbed safflower red pigment;
(3) resolve
Soak with the solution of potassium carbonate 30kg that massfraction is 3% and adsorbed the Microcrystalline Cellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
(4) refine
In filtrate, add lemon acid for adjusting pH to 5.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, lyophilize at being deposited in-20 DEG C, namely 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 crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 2 hours with the solution of potassium carbonate 150kg that massfraction is 2% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 5 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract and be about 400kg;
(2) adsorb
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 with deionized water rinsing cotton 3 times, namely obtains the cotton having adsorbed safflower red pigment;
(3) resolve
Soak with the solution of potassium carbonate 20kg that massfraction is 2% and adsorbed the cotton of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
(4) refine
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, lyophilize at being deposited in-20 DEG C, namely obtains safflower red pigment 3g, after testing, and pure pink colour valency
=70A.
Embodiment 5
(1) the extraction of safflower red pigment
By crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 2 hours with the solution of potassium carbonate 150kg that massfraction is 2% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 5 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract and be about 400kg;
(2) adsorb
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 with deionized water rinsing cotton 3 times, namely obtains the lignocellulose having adsorbed safflower red pigment;
(3) resolve
Soak with the solution of potassium carbonate 20kg that massfraction is 2% and adsorbed the lignocellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
(4) refine
In filtrate, add lemon acid for adjusting pH to 4.0, place 12 hours at 5 DEG C, supernatant liquor is removed in siphon, lyophilize at being deposited in-20 DEG C, namely obtains safflower red pigment 14.4g, after testing, and pure pink colour valency
=123A.
Above-described embodiment 1 owing to have employed optimum process condition of the present invention, therefore, the safflower red pigment yield obtained and purity the highest.
Claims (1)
1. from safflower slag, extract a method for safflower red pigment, it is characterized in that being made up of following step:
the extraction of safflower red pigment
By crossing the flower of the extra dry red wine after carthamin yellow slag charge 10kg with water extraction, soak 2 hours with the solution of potassium carbonate 150kg that massfraction is 2% in stirred at ambient temperature, filter, obtain filtrate; Slag charge washes 5 times with 5 times of deionizations again, filters, merges above filtrate, obtain safflower red pigment crude extract 400kg;
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 with deionized water rinsing Microcrystalline Cellulose 3 times, namely obtains the Microcrystalline Cellulose having adsorbed safflower red pigment;
resolve
Soak with the solution of potassium carbonate 20kg that massfraction is 2% and adsorbed the Microcrystalline Cellulose of safflower red pigment, stirring at room temperature 15 minutes, suction filtration, obtains filtrate; Repetitive operation 5 times, collects each filtrate;
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, lyophilize at being deposited in-20 DEG C, namely obtains safflower red pigment 28g, after testing, and pure pink colour valency
=248A.
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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 |
| 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 |
| CN112521769B (en) * | 2020-11-25 | 2021-11-30 | 清华大学 | Safflower red pigment and preparation method and dyeing method thereof |
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