CN112724703B - Method for extracting gardenia yellow pigment - Google Patents
Method for extracting gardenia yellow pigment Download PDFInfo
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- CN112724703B CN112724703B CN202110243454.1A CN202110243454A CN112724703B CN 112724703 B CN112724703 B CN 112724703B CN 202110243454 A CN202110243454 A CN 202110243454A CN 112724703 B CN112724703 B CN 112724703B
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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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- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
A method for extracting gardenia yellow pigment comprises the following steps: removing peel of fructus Gardeniae, sun drying, grinding into powder, sieving, and extracting with water; performing solid-liquid separation on the leaching liquor to obtain a first extracting solution, then adding water into the residual solid mixture for secondary extraction under ultrasonic waves, and performing solid-liquid separation on the second leaching liquor to obtain a second extracting solution; mixing the two extractive solutions, adding pectase and diatomaceous earth, stirring, standing, filtering with filter membrane, and microfiltering to obtain microfiltrate; purifying the micro-filtrate by using petroleum ether to obtain a purified extracting solution; and (3) performing weight reduction and concentration on the purified extracting solution through a reverse osmosis membrane, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separation solution, and performing vacuum freeze drying. The extraction method can efficiently extract high-price gardenia yellow pigment from gardenia jasminoides fruits, and the extracted gardenia yellow pigment is not easy to generate green change and gray change and has long storage time.
Description
Technical Field
The invention belongs to the technical field of natural pigment extraction, and particularly relates to a method for extracting gardenia yellow pigment.
Background
Natural pigments are widely used in the food industry as good food colorants. Because the natural edible pigment has higher price and is limited by production technology, the application amount of the natural edible pigment in the domestic food manufacturing industry is less. The gardenia yellow pigment is natural edible yellow pigment extracted from mature fruits of gardenia jasminoides ellis of rubiaceae, and has certain nutritional and health-care values. With the increasing environmental awareness of people, the gradual replacement of chemical pigments by natural food pigments has become a necessary trend.
In the traditional gardenia yellow pigment leaching process, about 60 wt.% of ethanol-water is generally selected as a leaching agent. Traditionally, ethanol is used as an extracting agent because the polarity of the ethanol is small, the solubility of other polar macromolecules such as pectin and protein in gardenia jasminoides fruit is small, when 60 wt.% ethanol-water is used as an extracting solvent, the purity of an extracting solution is high, but 2 times of volume of absolute ethanol is added after concentration, and the absolute ethanol is shaken uniformly and then kept stand for observation, and precipitates are also separated out. The obtained gardenia yellow can be greened and grayed after being stored for a period of time, a little of precipitate is generated, the product quality is influenced, and the storage time is short.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides the method for extracting the gardenia yellow pigment, and the prepared gardenia yellow pigment has the advantages of long storage time, high extraction rate, difficult greenness and grayness generation and the like.
The technical scheme is as follows: the preparation method of the gardenia yellow pigment comprises the following steps:
step one, removing peel of gardenia jasminoides fruits, drying in the sun, grinding into powder, sieving with a 30-40-mesh sieve, and leaching for the first time for 30-40 min at room temperature by using water according to the liquid-material ratio of (5-8) to 1;
step two, performing solid-liquid separation on the first leaching solution, taking supernatant as a first leaching solution, adding water into the residual solid mixture according to the liquid-material ratio of (3-4): 1, performing ultrasonic extraction at room temperature of 225-245W for 15-25 min to obtain a second leaching solution, performing solid-liquid separation on the second leaching solution, taking supernatant as a second leaching solution, and performing centrifugation for 10-20 min at the rotation speed of 4000-4500 r/min by adopting a horizontal spiral sedimentation centrifuge for the solid-liquid separation twice;
step three, combining the first extracting solution and the second extracting solution, adding 0.002-0.004 wt.% of pectinase and 2-3 wt.% of diatomite, fully stirring, standing for 40-50 min, filtering by a filtering membrane with the aperture of 0.22 mm, performing microfiltration by a ceramic membrane with the surface flow rate of 1-2 m/s and the aperture of 0.1-0.2 mu m at the surface flow rate of 0.15-0.3 MPa, and taking micro-filtrate;
mixing the micro-filtrate with petroleum ether in a volume ratio of 1:4, shaking, separating, collecting lower layer clear liquid, and then performing vacuum rotary evaporation at 45 ℃ under a vacuum degree of 0.09-0.1 MPa for 25 min to recover the petroleum ether, thereby obtaining a purified extracting solution;
and fifthly, reducing the weight of the purified extracting solution through a reverse osmosis membrane, concentrating the weight of the purified extracting solution to 1/4-1/3 of the weight of the purified extracting solution, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separated liquid, and freeze-drying the separated liquid in a vacuum freeze-drying machine for 8-12 hours at the freezing temperature of-30-20 ℃ to obtain the gardenia yellow pigment.
Preferably, in the first step, the gardenia jasminoides fruit is dried in the sun after peeling, ground into powder, sieved by a 30-mesh sieve, and then leached for the first time by water at room temperature for 35 min at a liquid-to-material ratio of 6: 1.
Preferably, in the second step, the first leaching solution is subjected to solid-liquid separation, a supernatant is taken as a first extracting solution, then water is added into the remaining solid mixture according to a liquid-to-material ratio of 3:1, ultrasonic extraction is performed at room temperature of 230W for 20 min, a second leaching solution is obtained, then solid-liquid separation is performed on the second leaching solution, a supernatant is taken as a second extracting solution, a horizontal spiral sedimentation centrifuge is adopted for the solid-liquid separation twice, the rotating speed is 4200 r/min, and centrifugation is performed for 15 min.
Preferably, in the third step, the first extract and the second extract are combined, 0.002 wt.% of pectinase and 2 wt.% of diatomite are added and fully stirred, then the mixture is kept stand for 45 min, and is filtered by a filter membrane with the pore diameter of 0.22 mm, and then is subjected to microfiltration by a ceramic membrane with the surface flow rate of 1.5 m/s and the pore diameter of 0.1 mu m under the pressure of 0.2 MPa, and micro-filtrate is obtained.
Preferably, the reverse osmosis membrane in the fifth step is a reverse osmosis membrane with a salt permeability of 98%, the working temperature is 20-30 ℃, the working pressure is less than or equal to 2.5MPa, and the molecular weight cutoff is 150 Da; the molecular weight cut-off during membrane separation is 2000-5000 Da, the working temperature is 20-30 ℃, and the working pressure is less than or equal to 0.6 MPa.
Preferably, in the fifth step, the purified extract is subjected to weight reduction and concentration by a reverse osmosis membrane, the concentration weight is 1/4-1/3 of the weight of the purified extract, then the concentrated pigment solution is subjected to membrane separation to separate the geniposide to obtain a separation solution, and the separation solution is freeze-dried in a vacuum freeze-drying machine for 10 hours at the freezing temperature of-30 ℃ to obtain the gardenia yellow pigment.
Has the advantages that: the extraction method can efficiently extract high-price gardenia yellow pigment from gardenia jasminoides fruits, and the extracted gardenia yellow pigment is not easy to generate green change and gray change and has long storage time;
the extraction method can improve the concentration of pigment in the leachate and reduce the production cost by carrying out water extraction on the gardenia fruit powder twice, can break fiber by crushing the gardenia fruit, can disintegrate plant tissues of the gardenia fruit, is favorable for leaching natural pigment of gardenia yellow, can further promote the leaching of the gardenia yellow pigment by carrying out ultrasonic extraction during the second water extraction, and can remove impurities which easily cause greenness and grayness of the gardenia yellow pigment to the maximum extent by adopting pectinase to decompose pectin, using diatomite as a filter aid, carrying out microfiltration after common filtration and finally using membrane separation to remove the gardenia glycoside because more pectin, protein and geniposide are doped in the two leaching, thereby increasing the extraction rate of the gardenia yellow pigment and prolonging the storage time of the gardenia yellow pigment.
Detailed Description
The invention is further described with reference to specific examples. Unless otherwise indicated, all starting materials are commercially available.
Example 1
The preparation method of the gardenia yellow pigment comprises the following steps:
step one, removing peel of gardenia jasminoides fruits, drying in the sun, grinding into powder, sieving with a 30-mesh sieve, and then leaching for the first time for 30 min at room temperature by using water according to a liquid-material ratio of 5: 1;
step two, performing solid-liquid separation on the first leaching solution, taking the supernatant as a first leaching solution, adding water into the residual solid mixture according to the liquid-material ratio of 3:1, performing ultrasonic extraction at room temperature of 225W for 15 min to obtain a second leaching solution, performing solid-liquid separation on the second leaching solution, taking the supernatant as a second leaching solution, performing solid-liquid separation twice by using a horizontal spiral sedimentation centrifuge at the rotating speed of 4000 r/min, and centrifuging for 20 min;
step three, combining the first extracting solution and the second extracting solution, adding 0.002 wt.% of pectinase and 2 wt.% of diatomite, fully stirring, standing for 40 min, filtering by a filter membrane with the aperture of 0.22 mm, performing microfiltration by a ceramic membrane with the surface flow rate of 1 m/s and the aperture of 0.1 mu m at the surface flow rate of 0.15 MPa, and taking a micro-filtrate;
mixing the micro-filtrate with petroleum ether in a volume ratio of 1:4, shaking, separating, collecting lower layer clear liquid, and then performing vacuum rotary evaporation at 45 ℃ under a vacuum degree of 0.09-0.1 MPa for 25 min to recover the petroleum ether, thereby obtaining a purified extracting solution;
and fifthly, reducing the weight of the purified extracting solution through a reverse osmosis membrane, concentrating the weight of the purified extracting solution to 1/4 of the weight of the purified extracting solution, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separation solution, and freeze-drying the separation solution in a vacuum freeze-drying machine for 8 hours at the freezing temperature of-30 ℃ to obtain the gardenia yellow pigment.
Example 2
The preparation method of the gardenia yellow pigment comprises the following steps:
step one, removing peel of gardenia jasminoides fruits, drying in the sun, grinding into powder, sieving with a 40-mesh sieve, and adding water according to a liquid-material ratio of 8:1 to leach for the first time for 40 min at room temperature;
step two, performing solid-liquid separation on the first leaching solution, taking supernatant as a first leaching solution, adding water into the residual solid mixture according to a liquid-material ratio of 4:1, performing ultrasonic extraction at room temperature of 245W for 25 min to obtain a second leaching solution, performing solid-liquid separation on the second leaching solution, taking supernatant as a second leaching solution, performing solid-liquid separation twice by using a horizontal spiral sedimentation centrifuge at the rotating speed of 4500 r/min, and centrifuging for 10 min;
step three, combining the first extracting solution and the second extracting solution, adding 0.004 wt.% of pectinase and 3 wt.% of diatomite, fully stirring, standing for 50 min, filtering by a filter membrane with the aperture of 0.22 mm, performing microfiltration by a ceramic membrane with the surface flow rate of 1 m/s and the aperture of 0.2 mu m at the surface flow rate of 0.3MPa, and taking a micro-filtrate;
mixing the micro-filtrate with petroleum ether in a volume ratio of 1:4, shaking, separating, collecting lower layer clear liquid, and then performing vacuum rotary evaporation at 45 ℃ under a vacuum degree of 0.09-0.1 MPa for 25 min to recover the petroleum ether, thereby obtaining a purified extracting solution;
and fifthly, reducing the weight of the purified extracting solution through a reverse osmosis membrane, concentrating the weight of the purified extracting solution to 1/3 of the weight of the purified extracting solution, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separation solution, and freeze-drying the separation solution in a vacuum freeze-drying machine for 12 hours at the freezing temperature of-20 ℃ to obtain the gardenia yellow pigment.
Example 3
The preparation method of the gardenia yellow pigment comprises the following steps:
step one, removing peel of gardenia jasminoides fruits, drying in the sun, grinding into powder, sieving with a 30-mesh sieve, and then leaching for the first time for 35 min at room temperature by using water according to a liquid-material ratio of 6: 1;
step two, performing solid-liquid separation on the first leaching solution, taking the supernatant as a first leaching solution, adding water into the residual solid mixture according to the liquid-material ratio of 3:1, performing ultrasonic extraction at room temperature of 230W for 20 min to obtain a second leaching solution, performing solid-liquid separation on the second leaching solution, taking the supernatant as a second leaching solution, performing solid-liquid separation twice by adopting a horizontal spiral sedimentation centrifuge at the rotating speed of 4200 r/min, and centrifuging for 15 min;
step three, combining the first extracting solution and the second extracting solution, adding 0.002 wt.% of pectinase and 2 wt.% of diatomite, fully stirring, standing for 45 min, filtering by a filter membrane with the aperture of 0.22 mm, performing microfiltration by a ceramic membrane with the surface flow rate of 1.5 m/s and the aperture of 0.1 mu m under the pressure of 0.2 MPa, and taking a micro-filtrate;
mixing the micro-filtrate with petroleum ether in a volume ratio of 1:4, shaking, separating, collecting lower layer clear liquid, and performing vacuum rotary evaporation at 45 ℃ under a vacuum degree of 0.1 MPa for 25 min to recover the petroleum ether, thereby obtaining a purified extracting solution;
and fifthly, reducing the weight of the purified extracting solution through a reverse osmosis membrane, concentrating the weight of the purified extracting solution to 1/4 of the weight of the purified extracting solution, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separation solution, and freeze-drying the separation solution in a vacuum freeze-drying machine for 10 hours at the freezing temperature of-30 ℃ to obtain the gardenia yellow pigment.
Comparative example 1
The difference from example 3 is that in the second step, the first leaching solution is subjected to solid-liquid separation, and the supernatant is taken as a first extracting solution; in the third step, 0.002 wt.% of pectinase and 2 wt.% of diatomite are added into the first extracting solution, the mixture is fully stirred and then stands for 45 min, and is filtered by a filter membrane with the aperture of 0.22 mm, and then is subjected to microfiltration by a ceramic membrane with the surface flow rate of 1.5 m/s and the aperture of 0.1 mu m under the pressure of 0.2 MPa, and micro-filtrate is obtained.
Comparative example 2
The difference from the example 3 is that the extract purified in the fifth step is lyophilized in a vacuum freeze dryer for 10 h at-30 ℃ to obtain gardenia yellow pigment.
The statistics of the extraction rate and the gardenia yellow value are carried out on the products prepared in the examples 1 to 3 and the comparative examples 1 and 2, and the specific results are as follows:
| extract rate/%) | Color scale | Yield/% | |
| Example 1 | 68.3 | 589 | 56 |
| Example 2 | 69.8 | 612 | 55 |
| Example 3 | 75.2 | 640 | 62 |
| Comparative example 1 | 54.2 | 580 | 45 |
| Comparative example 2 | 64.5 | 516 | 59 |
Claims (6)
1. The method for extracting the gardenia yellow pigment is characterized by comprising the following steps of:
step one, removing peel of gardenia jasminoides fruits, drying in the sun, grinding into powder, sieving with a 30-40-mesh sieve, and leaching for the first time for 30-40 min at room temperature by using water according to the liquid-material ratio of (5-8) to 1;
step two, performing solid-liquid separation on the first leaching solution, taking supernatant as a first leaching solution, adding water into the residual solid mixture according to the liquid-material ratio of (3-4): 1, performing ultrasonic extraction at room temperature of 225-245W for 15-25 min to obtain a second leaching solution, performing solid-liquid separation on the second leaching solution, taking supernatant as a second leaching solution, and performing centrifugation for 10-20 min at the rotation speed of 4000-4500 r/min by adopting a horizontal spiral sedimentation centrifuge for the solid-liquid separation twice;
step three, combining the first extracting solution and the second extracting solution, adding 0.002-0.004 wt.% of pectinase and 2-3 wt.% of diatomite, fully stirring, standing for 40-50 min, filtering by a filtering membrane with the aperture of 0.22 mm, performing microfiltration by a ceramic membrane with the surface flow rate of 1-2 m/s and the aperture of 0.1-0.2 mu m at the pressure of 0.15-0.3 MPa, and taking a micro-filtrate;
mixing the micro-filtrate with petroleum ether in a volume ratio of 1:4, shaking, separating, collecting lower layer clear liquid, and then performing vacuum rotary evaporation at 45 ℃ under a vacuum degree of 0.09-0.1 MPa for 25 min to recover the petroleum ether, thereby obtaining a purified extracting solution;
and fifthly, reducing the weight of the purified extracting solution through a reverse osmosis membrane, concentrating the weight of the purified extracting solution to 1/4-1/3 of the weight of the purified extracting solution, separating the gardenoside from the concentrated pigment solution through membrane separation to obtain a separated liquid, and freeze-drying the separated liquid in a vacuum freeze-drying machine for 8-12 hours at the freezing temperature of-30-20 ℃ to obtain the gardenia yellow pigment.
2. The method for extracting gardenia yellow pigment according to claim 1, wherein in the first step, the gardenia fruit is peeled off, dried in the sun, ground into powder, sieved by a 30-mesh sieve, and then extracted for the first time with water at a liquid-to-material ratio of 6:1 for 35 min at room temperature.
3. The method for extracting gardenia yellow pigment according to claim 1, wherein in the second step, the first leaching solution is subjected to solid-liquid separation, the supernatant is taken as the first leaching solution, then water is added into the remaining solid mixture according to the liquid-to-material ratio of 3:1, ultrasonic extraction is performed at room temperature of 230W for 20 min, the second leaching solution is obtained, solid-liquid separation is performed on the second leaching solution, the supernatant is taken as the second leaching solution, a horizontal spiral sedimentation centrifuge is adopted for both solid-liquid separation, the rotating speed is 4200 r/min, and centrifugation is performed for 15 min.
4. The method for extracting gardenia yellow pigment according to claim 1, wherein the third step is to combine the first extract and the second extract, add 0.002 wt.% of pectinase and 2 wt.% of diatomite, fully stir, stand for 45 min, filter through a filter membrane with a pore size of 0.22 mm, microfilter through a ceramic membrane with a surface flow rate of 1.5 m/s at a surface flow rate of 0.2 MPa and a pore size of 0.1 μm, and take the microfiltrate.
5. The method for extracting gardenia yellow pigment according to claim 1, wherein the reverse osmosis membrane in the fifth step is a reverse osmosis membrane with a salt permeability of 98%, the working temperature is 20-30 ℃, the working pressure is less than or equal to 2.5MPa, and the molecular weight cutoff is 150 Da; the molecular weight cut-off during membrane separation is 2000-5000 Da, the working temperature is 20-30 ℃, and the working pressure is less than or equal to 0.6 MPa.
6. The method for extracting gardenia yellow pigment according to claim 1, wherein in the fifth step, the purified extract is subjected to weight reduction concentration by a reverse osmosis membrane, the concentration weight is 1/4-1/3 of the weight of the purified extract, then the concentrated pigment solution is subjected to membrane separation to separate gardenoside, a separation solution is obtained, and the separation solution is freeze-dried in a vacuum freeze-drying machine for 10 hours at-30 ℃ to obtain the gardenia yellow pigment.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100537586C (en) * | 2006-02-23 | 2009-09-09 | 江南大学 | Method for producing high purity jasminoidin and high color number gardenia yellow pigment |
| CN101659794B (en) * | 2009-09-27 | 2012-08-29 | 广西山云生化科技有限公司 | New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology |
| CN102321385B (en) * | 2011-09-14 | 2014-03-26 | 河南中大生物工程有限公司 | Production method for gardenia yellow pigment |
| CN102911513B (en) * | 2012-08-17 | 2014-03-12 | 江苏久吾高科技股份有限公司 | Extraction method of gardenia yellow pigment |
| CN105037461B (en) * | 2015-07-08 | 2018-06-05 | 邵阳学院 | Multistage aqueous two-phase separated in synchronization Gardenoside and Gardenia Yellow |
| CN105482494B (en) * | 2015-12-30 | 2018-04-06 | 河南中大恒源生物科技股份有限公司 | A kind of Gardenia Yellow production method of high safron cellulose content |
| CN108774407B (en) * | 2018-05-30 | 2019-06-11 | 山东省农业科学院农产品研究所 | A kind of extracting method of gardenia yellow pigment with high color value |
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