CN115109431A - Preparation method of radish red pigment extract - Google Patents
Preparation method of radish red pigment extract Download PDFInfo
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- CN115109431A CN115109431A CN202110293625.1A CN202110293625A CN115109431A CN 115109431 A CN115109431 A CN 115109431A CN 202110293625 A CN202110293625 A CN 202110293625A CN 115109431 A CN115109431 A CN 115109431A
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- 241000220259 Raphanus Species 0.000 title claims abstract description 51
- 235000006140 Raphanus sativus var sativus Nutrition 0.000 title claims abstract description 50
- 239000000284 extract Substances 0.000 title claims abstract description 41
- 239000001054 red pigment Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000605 extraction Methods 0.000 claims abstract description 162
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000003809 water extraction Methods 0.000 claims abstract description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 126
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 80
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 74
- 238000005406 washing Methods 0.000 claims description 57
- 239000007788 liquid Substances 0.000 claims description 48
- 239000000725 suspension Substances 0.000 claims description 37
- 238000003795 desorption Methods 0.000 claims description 23
- 238000003756 stirring Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 235000013399 edible fruits Nutrition 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000011068 loading method Methods 0.000 claims description 14
- 238000005070 sampling Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000003480 eluent Substances 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 238000004440 column chromatography Methods 0.000 claims description 9
- 238000010828 elution Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000008213 purified water Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 7
- 241000196324 Embryophyta Species 0.000 abstract description 3
- 210000002421 cell wall Anatomy 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000419 plant extract Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000003929 acidic solution Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000004064 recycling Methods 0.000 description 3
- 229930002877 anthocyanin Natural products 0.000 description 2
- 235000010208 anthocyanin Nutrition 0.000 description 2
- 239000004410 anthocyanin Substances 0.000 description 2
- 150000004636 anthocyanins Chemical class 0.000 description 2
- 235000019057 Raphanus caudatus Nutrition 0.000 description 1
- 244000088415 Raphanus sativus Species 0.000 description 1
- 235000011380 Raphanus sativus Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 210000002615 epidermis Anatomy 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 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
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation method of a radish red pigment extract, solves the problem that the radish red pigment cannot be extracted and purified to a higher level in the prior art, and relates to the technical field of plant extract preparation. The radish red pigment extract is obtained by acid water extraction, filtration, concentration and drying. The acidic solution is adopted during extraction, the plant cell walls can be destroyed during extraction, the dissolution and precipitation efficiency of the main component radish red pigment is increased, and the stability protection effect during the extraction process is achieved.
Description
Technical Field
The invention relates to the technical field of plant extract preparation, in particular to a preparation method of a radish red pigment extract.
Background
Radish (Raphanus sativus L.) belongs to a brassicaceae radish genus common cross-pollinated plant, is generally planted in low-altitude areas of China, has more varieties, and is one of black radishes. The black radish is a new germplasm resource introduced in recent years, the epidermis is purple black, the meat is crisp, the nutritive value is higher than that of the white radish, and the black radish has a better health-care effect and a good medicinal and edible value.
The natural haematochrome contained in the black radish fruits contains anthocyanin as a main chemical component, has the advantages of natural color, safe performance, no side effect and the like, and can be widely applied to the fields of foods, cakes, wine blending and the like. In the prior art, the extraction of haematochrome from black radish is generally the extraction of drinking water; the yield of the water extraction process is low, and the utilization rate of raw materials is insufficient; the ethanol extraction process has relatively high production cost; and the radish red pigment in the prior art cannot be extracted and purified to a higher level.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art: provides a preparation method which not only ensures the low cost of the extraction solvent, but also improves the yield of the extraction process and can improve the anthocyanin content of the radish red pigment extract.
The technical solution of the invention is as follows: a preparation method of a radish red pigment extract comprises the following steps:
1) acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 28-32 ℃, adding the chopped black radish fruits, crushing to form a feed liquid, introducing the feed liquid into an extraction tank, adding water and citric acid, and stirring and extracting to obtain a primary extracting solution;
second, the method comprises the following steps: performing secondary extraction on the extraction residues in the extraction tank, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28-32 ℃, adding the extraction residues to obtain suspension, and stirring and extracting to obtain a secondary extraction solution;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28-32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting to obtain three-time extraction liquid, and temporarily storing the third-time extraction liquid in a storage tank to serve as an extraction solvent for the second batch of first extraction;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a plate frame to obtain a fine filtrate, and performing column chromatography;
3) concentrating, drying, and collecting ethanol desorption solution to obtain radix Raphani red pigment extract.
Preferably, the column chromatography in step 2) comprises the following steps:
sampling: controlling the flow rate of the fine filtrate to be 2-4 BV during sample loading Column Stopping sampling when the content of the red pigment in the effluent is 0.0007 percent, and performing the next washing procedure;
washing with water: after the sample loading is finished, using purified water to wash the column, and when the water washing liquid flows out, controlling the flow rate of the water washing liquid to be 2-4 BV by using an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.2-2.7, and starting ethanol desorption;
washing and desorbing: after the water washing is finished, the valve is switched to ethanol for desorption, and 0.5-1.0 BV is firstly used Column Ethanol with the volume fraction of 30-70 percent is used for 2-4 BV Column Washing at a flow rate of/h, recovering eluent, and then using 6-8 BV Column The volume fraction of the additive is 70-85 percent and is 2-4 BV Column And h, analyzing the flow rate, and ending the elution when the concentration of the haematochrome in the eluent is less than 0.002 percent.
Preferably, the weight ratio of the black radish fruits to the water in the first extraction in the step 1) is 1: 10-12.
Preferably, the weight ratio of the black radish fruits to the water in the first extraction in the step 1) is 1: 10.
Preferably, the concentration of the citric acid in the feed liquid in the first extraction in the step 1) is 3.5-6.5 per mill.
Preferably, the concentration of the citric acid in the feed liquid in the first extraction in the step 1) is 5.5 per mill.
Preferably, the stirring extraction time in the first extraction, the second extraction and the third extraction in the step 1) is 2-3 h.
Preferably, the weight ratio of the extraction residues in the second extraction and the third extraction in the step 1) is 1: 10-12, and the concentration of citric acid in the suspension is 3.5-6.5 per thousand.
Preferably, the concentration in the step 3) is vacuum concentration, and the specific concentration temperature is controlled to be 50-60 ℃ and the vacuum degree is more than 0.06 MPa.
Preferably, the drying in the step 3) is vacuum drying, the vacuum drying temperature is 45-55 ℃, and the vacuum degree is-0.090-0.100 MPa.
The invention has the beneficial effects that: the invention adopts an acid water process, and because the haematochrome is difficult to extract and is unstable under alkalescence or neutral conditions, an acid solution is usually adopted during extraction, and the acid solution can damage plant cell walls during extraction, increase the dissolution and precipitation efficiency of the haematochrome and play a role in stability protection during extraction.
The preparation method of the radish red pigment extract comprises the steps of acid water extraction, filtration, concentration, drying, collection and the like, the dosage of an extraction solvent is small, and other organic solvents except edible ethanol are not introduced in the whole process. And an extraction mode is adopted, namely the first three-extract filtrate is used as the first extract of the second batch as the extraction solvent of the second batch, so that the investment of the solvent is effectively reduced, the extraction and concentration time is shortened, the energy consumption and the cost are saved, the whole preparation method is simple in process, convenient to operate and easy to realize industrialization, the color value of the radish red pigment can reach 120-150, and the radish red pigment meets the requirements of foreign trade customers in Europe and America.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the present invention is not limited to the following examples.
Example one
1) Acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 28 ℃, adding chopped black radish fruits, wherein the weight ratio of the water to the black radish fruits is 10:1, introducing the crushed raw materials into an extraction tank, adding water and citric acid, stirring, and carrying out primary extraction for 2 hours to obtain a primary extraction solution, wherein the concentration of the citric acid in the material liquid is controlled to be 6.5 per thousand;
II, extracting: performing secondary extraction on extraction residues in the extraction pool, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 2 hours to obtain a secondary extraction solution, wherein the weight ratio of the extraction residues in the suspension is 1:10, and the concentration of the citric acid in the suspension is 6.5 per thousand;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28 ℃, adding the extraction residues to obtain a suspension, and stirring and extracting for 2 hours to obtain three-time extraction liquid, wherein the weight ratio of the extraction residues in the suspension is 1:10, and the concentration of the citric acid in the suspension is 6.5 per thousand; temporarily storing the third extracting solution in a storage tank to be used as an extracting solvent for the second batch of first extraction;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a 250-mesh plate frame to obtain a fine filtrate, and performing column chromatography:
sampling: controlling the flow rate of the fine filtrate to be 2BV during sample loading Column Stopping sampling when the effluent is close to the liquid with the content of 0.0007%, and performing the next washing process;
washing: after the sample loading is finished, the column is washed by purified water, and when the water washing liquid flows out, the flow rate of the water washing liquid is controlled to be 2BV by an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.7, and starting ethanol desorption;
thirdly, alcohol washing and desorption: after the water washing is finished, the valve is switched to ethanol for desorption, and 0.5BV is used firstly Column Ethanol with volume fraction of 30% in 2BV Column Eluting at flow rate of/h, recovering eluate, and recycling 6BV Column Ethanol with volume fraction of 70 percent in 2BV Column Desorbing at the flow rate of/h, and finishing elution when the concentration of the eluent is less than 0.002%;
3) concentrating, drying, and collecting the ethanol desorption solution to obtain the radish red pigment extract.
The concentration is vacuum concentration, and the concentration temperature is controlled at 50 deg.C and the vacuum degree is greater than 0.06 Mpa.
The drying is vacuum drying, in particular to vacuum drying at the temperature of 55 ℃ and the vacuum degree of-0.090 MPa.
Example two
1) Acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 32 ℃, adding chopped black radish fruits, wherein the weight ratio of the water to the black radish fruits is 12:1, introducing the crushed raw materials into an extraction tank, adding water and citric acid, stirring, and carrying out primary extraction for 3 hours to obtain a primary extraction solution, wherein the concentration of the citric acid in the material liquid is controlled to be 3.5 per thousand;
II, extracting: performing secondary extraction on extraction residues in the extraction pool, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 3 hours to obtain a secondary extraction solution, wherein the weight ratio of the extraction residues in the suspension is 1:12, and the concentration of the citric acid in the suspension is 3.5 per thousand;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 3 hours to obtain three-time extraction liquid, wherein the weight ratio of the extraction residues in the suspension is 1:12, and the concentration of the citric acid in the suspension is 3.5 per thousand; temporarily storing the third extracting solution in a storage tank to serve as the extracting solvent for the first extraction of the second batch;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a 250-mesh plate frame to obtain a fine filter, and performing column chromatography:
sampling: controlling the flow rate of the fine filtrate to be 4BV during sample loading Column Stopping sampling when the effluent is close to the liquid with the content of 0.0007 percent, and carrying out the next washing procedure;
water washing: after the sample loading is finished, the column is washed by purified water, and when the washing liquid flows out, the flow rate of the washing liquid is controlled to be 4BV by an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.2, and starting ethanol desorption;
③ washing with alcohol and desorbing: after the water washing is finished, the valve is switched to ethanol for desorption, and 1.0BV is used firstly Column Ethanol with volume fraction of 70 percent in 4BV Column Eluting at flow rate of/h, recovering eluate, and recycling 8BV Column Ethanol with volume fraction of 85 percent in 4BV Column Desorbing at the flow rate of/h, and finishing elution when the concentration of the eluent is less than 0.002%;
3) concentrating, drying, and collecting the ethanol desorption solution to obtain the radish red pigment extract.
The concentration is vacuum concentration, and the concentration temperature is controlled at 60 deg.C, and the vacuum degree is greater than 0.06 Mpa.
The drying is vacuum drying, specifically vacuum drying at 55 ℃ and under 0.100 MPa.
EXAMPLE III
1) Acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 50 ℃, adding chopped black radish fruits, wherein the weight ratio of the water to the black radish fruits is 11:1, introducing the crushed raw materials into an extraction tank, adding water and citric acid, stirring, and carrying out primary extraction for 3 hours to obtain a primary extraction solution, wherein the concentration of the citric acid in the material liquid is controlled to be 5 per thousand;
II, extracting: performing secondary extraction on extraction residues in the extraction tank, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 30 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 2 hours to obtain a secondary extraction solution, wherein the weight ratio of the extraction residues in the suspension is 1:11, and the concentration of the citric acid in the suspension is 5 per thousand;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 30 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 3 hours to obtain three-time extraction liquid, wherein the weight ratio of the extraction residues in the suspension is 1:11, and the concentration of the citric acid in the suspension is 5 per thousand; temporarily storing the third extracting solution in a storage tank to be used as an extracting solvent for the second batch of first extraction;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a 250-mesh plate frame to obtain a fine filtrate, and performing column chromatography:
sampling: controlling the flow rate of the fine filtrate to be 4BV during sample loading Column Stopping sampling when the effluent is close to the liquid with the content of 0.0007 percent, and carrying out the next washing procedure;
washing with water: after the sample loading is finished, the column is washed by purified water, and when the water washing liquid flows out, the flow rate of the water washing liquid is controlled to be 3BV by an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.5, and starting ethanol desorption;
③ washing with alcohol and desorbing: after the water washing is finished, the valve is switched to ethanol desorption, and 0.8BV is firstly used Column Ethanol with volume fraction of 40% in 4BV Column Eluting at flow rate of h, recovering eluent, and reusing 7BV Column Ethanol with volume fraction of 80% in 3BV Column Desorbing at the flow rate of/h, and ending the elution when the concentration of the eluent is less than 0.002%;
3) concentrating, drying, and collecting the ethanol desorption solution to obtain radix Raphani red pigment extract;
the concentration is vacuum concentration, and the concentration temperature is controlled at 55 deg.C and the vacuum degree is greater than 0.06 Mpa. The drying is vacuum drying, specifically vacuum drying at 50 ℃ and vacuum degree of-0.090 MPa.
Example four
1) Acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 52 ℃, adding minced black radish fruits, wherein the weight ratio of the water to the black radish fruits is 10:1, introducing the crushed raw materials into an extraction tank, adding water and citric acid, stirring, and carrying out primary extraction for 3 hours to obtain a primary extraction solution, wherein the concentration of the citric acid in the material liquid is controlled to be 3.5 per thousand;
II, extracting: performing secondary extraction on extraction residues in the extraction pool, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 2 hours to obtain a secondary extraction solution, wherein the weight ratio of the extraction residues in the suspension is 1:10, and the concentration of the citric acid in the suspension is 3.5 per thousand;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 2 hours to obtain three-time extraction liquid, wherein the weight ratio of the extraction residues in the suspension is 1:10, and the concentration of the citric acid in the suspension is 3.5 per thousand; temporarily storing the third extracting solution in a storage tank to be used as an extracting solvent for the second batch of first extraction;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a 250-mesh plate frame to obtain a fine filtrate, and performing column chromatography:
sampling: controlling the flow rate of the fine filtrate to be 2BV during sample loading Column Stopping sampling when the effluent is close to the liquid with the content of 0.0007%, and performing the next washing process;
water washing: after the sample loading is finished, the column is washed by purified water, and when the water washing liquid flows out, the flow rate of the water washing liquid is controlled to be 2BV by an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.4, and starting ethanol desorption;
③ washing with alcoholDesorbing: after the water washing is finished, the valve is switched to ethanol for desorption, and 0.7BV is used firstly Column Ethanol with volume fraction of 60% in 2BV Column Eluting at flow rate of/h, recovering eluent, and reusing 8BV Column Ethanol with volume fraction of 70 percent in a volume ratio of 2BV Column Desorbing at the flow rate of/h, and ending the elution when the concentration of the eluent is less than 0.002%;
3) concentrating, drying, and collecting the ethanol desorption solution to obtain the radish red pigment extract.
The concentration is vacuum concentration, and the concentration temperature is controlled at 55 deg.C, and the vacuum degree is greater than 0.06 Mpa.
The drying is vacuum drying, specifically vacuum drying at 50 deg.C and vacuum degree of 0.100 MPa.
EXAMPLE five
1) Acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 48 ℃, adding minced black radish fruits, wherein the weight ratio of the water to the black radish fruits is 12:1, introducing the crushed raw materials into an extraction tank, adding water and citric acid, stirring, and carrying out primary extraction for 2 hours to obtain a primary extraction solution, wherein the concentration of the citric acid in the material liquid is controlled to be 4.5 per thousand;
second, the method comprises the following steps: performing secondary extraction on extraction residues in the extraction pool, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 3 hours to obtain a secondary extraction solution, wherein the weight ratio of the extraction residues in the suspension is 1:12, and the concentration of the citric acid in the suspension is 4.5 per thousand;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28 ℃, adding the extraction residues to obtain a suspension, stirring and extracting for 3 hours to obtain three-time extraction liquid, wherein the weight ratio of the extraction residues in the suspension is 1:12, and the concentration of the citric acid in the suspension is 4.5 per thousand; temporarily storing the third extracting solution in a storage tank to serve as the extracting solvent for the first extraction of the second batch;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a 250-mesh plate frame to obtain a fine filtrate, and performing column chromatography:
sampling: controlling the flow rate of the fine filtrate to be 4BV during sample loading Column Stopping sampling when the effluent is close to the liquid with the content of 0.0007 percent, and carrying out the next washing procedure;
washing with water: after the sample loading is finished, the column is washed by purified water, and when the washing liquid flows out, the flow rate of the washing liquid is controlled to be 4BV by an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.2, and starting ethanol desorption;
③ washing with alcohol and desorbing: after the water washing is finished, the valve is switched to ethanol for desorption, and 1.0BV is used firstly Column Ethanol with volume fraction of 40 percent at 4BV Column Eluting at flow rate of/h, recovering eluate, and recycling 8BV Column Ethanol with volume fraction of 70 percent in 4BV Column Desorbing at the flow rate of/h, and ending the elution when the concentration of the eluent is less than 0.002%;
3) concentrating, drying, and collecting the ethanol desorption solution to obtain the radish red pigment extract.
The concentration is vacuum concentration, and the concentration temperature is controlled at 50 deg.C and the vacuum degree is greater than 0.06 Mpa.
The drying is vacuum drying, specifically vacuum drying at 45 ℃ and under 0.100 MPa.
The above are merely characteristic embodiments of the present invention, and do not limit the scope of the present invention in any way. All technical solutions formed by equivalent exchanges or equivalent substitutions fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a radish red pigment extract is characterized by comprising the following steps:
1) acid water extraction:
firstly, extracting: adding water into an extraction tank, heating to 28-32 ℃, adding the chopped black radish fruits, crushing to form a feed liquid, introducing the feed liquid into an extraction tank, adding water and citric acid, and stirring and extracting to obtain a primary extracting solution;
II, extracting: performing secondary extraction on the extraction residues in the extraction tank, wherein the secondary extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28-32 ℃, adding the extraction residues to obtain suspension, and stirring and extracting to obtain a secondary extraction solution;
three-stage extraction: extracting the extraction residues in the extraction tank for three times, wherein the three-time extraction specifically comprises the steps of adding water and citric acid into a container, heating to 28-32 ℃, adding the extraction residues to obtain a suspension, stirring and extracting to obtain three-time extraction liquid, and temporarily storing the third-time extraction liquid in a storage tank to serve as an extraction solvent for the second batch of first extraction;
2) and (3) filtering: mixing the primary extract and the secondary extract in the step 1), filtering by a plate frame to obtain a fine filtrate, and performing column chromatography;
3) concentrating, drying, and collecting ethanol desorption solution to obtain radix Raphani red pigment extract.
2. The method for preparing the radish red pigment extract according to claim 1, wherein the column chromatography in the step 2) comprises the following steps:
sampling: controlling the flow rate of the fine filtrate to be 2-4 BV during sample loading Column Stopping sampling when the content of the red pigment in the effluent is 0.0007 percent, and performing the next washing procedure;
washing with water: after sample loading is finished, washing the column with purified water, and when the washing liquid flows out, controlling the flow rate of the washing liquid to be 2-4 BV by using an outlet valve Column Stopping water washing when the pH value of the water washing liquid is 2.2-2.7, and starting ethanol desorption;
elution and desorption: after the water washing is finished, the valve is switched to ethanol for desorption, and 0.5-1.0 BV is used firstly Column Ethanol with the volume fraction of 30-70 percent is used for 2-4 BV Column Eluting at a flow rate of/h, recovering the eluent, and then using 6-8 BV Column Ethanol with volume fraction of 70-85% for 2-4 BV Column Desorbing at the flow rate of/h, and finishing the elution when the concentration of the red pigment in the eluent is less than 0.002 percent.
3. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: in the step 1), the weight ratio of the black radish fruits to water in the first extraction is 1: 10-12.
4. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: in the step 1), the weight ratio of the black radish fruits to water in the first extraction is 1: 10.
5. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: in the first step 1), the concentration of citric acid in the feed liquid is 3.5-6.5 per mill.
6. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: in the step 1), the concentration of the citric acid in the feed liquid is 5.5 per mill.
7. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: stirring and extracting time of the first extraction, the second extraction and the third extraction in the step 1) is 2-3 h.
8. The method for preparing the radish red pigment extract according to claim 1, characterized in that: in the step 1), the weight ratio of extraction residues in the secondary extraction and the tertiary extraction in the suspension is 1: 10-12, and the concentration of citric acid in the suspension is 3.5-6.5 per mill.
9. The method for preparing the radish red pigment extract according to claim 1, characterized in that: the concentration in the step 3) is vacuum concentration, and the specific concentration temperature is controlled to be 50-60 ℃, and the vacuum degree is more than 0.06 Mpa.
10. The method for preparing the radish red pigment extract according to claim 1, which is characterized in that: the drying in the step 3) is vacuum drying, the temperature of the vacuum drying is 45-55 ℃, and the vacuum degree is-0.090-0.100 MPa.
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