CN104448907A - Natural pigment extraction technology - Google Patents
Natural pigment extraction technology Download PDFInfo
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- CN104448907A CN104448907A CN201310431447.XA CN201310431447A CN104448907A CN 104448907 A CN104448907 A CN 104448907A CN 201310431447 A CN201310431447 A CN 201310431447A CN 104448907 A CN104448907 A CN 104448907A
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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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Abstract
The invention discloses a natural pigment extraction technology. The technology comprises the following steps: 1, washing a raw material with water, drying, crushing, sieving by a 100 mesh sieve, carrying out homogeneous extraction in a mixed liquid containing 60-90V% of an ethanol-water solution and 0.1mol/l of an aqueous solution of hydrochloric acid, and filtering to obtain a filtrate, wherein the pH value of the mixed liquid is 2.0-5.0, and the homogeneous extraction comprises a high speed pretreatment phase and a homogeneous extraction phase; 2, neutralizing the filtrate obtained in step 1, centrifuging, and removing residues in order to obtain a supernatant; and 3, concentrating the supernatant obtained in step 2, and drying. The raw material is chestnut shell, black bean skin and pitaya peel. The extraction technology has the advantages of simple process, low requirements on a production device, no destroys to pigment substances, and high extraction rate.
Description
Technical field
The present invention relates to a kind of extracting method of natural pigment, relate to a kind of technique that can be used for the pigments such as Chestnut shell pigment, Brown Pigment From Acorn Shells, hazelnut shell and produce particularly.
Background technology
Natural plant pigment can be divided into four large classes by chemical structure difference, pyrrole derivative class pigment, polyenoid class pigment (carotenoids class prime system), phenol sulfonate, ketone and Quinone Pigments, it is not only nontoxic, and a lot of nutritive substance necessary containing human body or inherently VITAMIN or there is the material of VITAMIN character, as riboflavin, lycopene, β-carotene etc., natural pigment tone is more natural simultaneously, the color of natural goods can be imitated preferably, painted tone waits many factors more naturally, therefore modern food industry more and more trends towards using natural pigment to the selection of pigment, the extraction of natural pigment is also waved vital role increasingly.
The extracting method of current natural pigment has solvent extraction method, microwave extraction method, supercritical fluid extraction, ultrasonic extraction etc.Wherein solvent extraction method is as use the earliest, and simple to operate, becomes nature strength method the most frequently used at present, and its principle is isolated according to the different solubility of target component in different solvents (particularly ethanol).
Summary of the invention
Technical problem to be solved by this invention is to overcome in the existing extracting method to natural pigments such as Chestnut shell pigment, Brown Pigment From Acorn Shells, hazelnut shell, the defects such as cost is higher, extraction yield is lower, and provides a kind of extracting method of natural pigment.Extracting method technique of the present invention is simple, low to production unit requirement, colors is survivable, extraction yield is higher.
The present invention relates to a kind of extracting method of natural pigment, it comprises the following step:
(1) 100 mesh sieves are crossed by after raw material washing, drying, pulverizing, in the mixed solution of the aqueous ethanolic solution of percent by volume 60-90 % (preferred 75%-90%) and the aqueous hydrochloric acid of 0.1 mole often liter, carry out homogeneous extraction, the pH of described mixed solution is 2.0-5.0 (preferably 3.0), filter after extracting, obtain filtrate; Described homogeneous extracts and comprises high speed pretreatment stage and homogeneous extraction stage;
(2) by the neutralization of step (1) gained filtrate, centrifugal slagging-off, supernatant liquor is obtained;
(3) supernatant liquor of step (2) gained is carried out concentrated and dry;
Wherein, described raw material is Chestnut shell pigment, Brown Pigment From Acorn Shells, hazelnut shell etc.
In step (1), described pulverize and sieve after raw material and mixed solution mixing after, solid-to-liquid ratio is preferably mass volume ratio (w/v) 1g: 5ml-1g: 10ml.
In step (1), described homogeneous extracts equipment used and can be commercially available high-shear homogenizing machine.Under described high speed pretreatment stage condition is preferably 5000-10000 (preferred 9000-10000) rpm, effect is no less than 5 minutes (preferred 5-20min); Temperature is preferably room temperature (20 ~ 35 DEG C).It is that under 1000-4000 (preferred 3000-4000) rpm, process is no less than 30 minutes (preferred 30-60min) that described homogeneous extracts stage conditions.
The temperature that described homogeneous extracts the stage can be room temperature (20 ~ 35 DEG C).The time that described homogeneous extracts the stage can be 5 ~ 8 hours.The number of times that described homogeneous extracts the stage is preferably 1 ~ 3 time (preferably 2 times).Namely, after the 1st homogeneous extracts, step (1) gained filter residue can be repeated 1 ~ 2 homogeneous and extract.
In step (2), the method for described neutralization can be conventional neutralization method, as added alkali aqueous solution (such as 0.1 mole of often liter of aqueous sodium hydroxide solution), adjustment pH to 6 ~ 8 (in general, to neutral).Described centrifugal condition can be the normal condition of this area centrifugally operated, and preferably under 200-2000 (preferably 1000) rpm, process 5-30 minute, that better is centrifugal 5-15 minute under 1000 rpms.
In step (3), described drying can be conventional drying means, as lyophilize.
Extracting method of the present invention, better step is as follows:
(1) fresh feed is got through ion, drying, pulverizing, excessively 100 mesh sieves;
(2) add ethanol, hydrochloric acid, adjust pH to acid, homogeneous extracts and filters;
(3) by filter residue by abovementioned steps (2) reprocessing once, filter;
(4) twice filtrate in front and back is merged, with sodium hydroxide solution neutralization, centrifugal slagging-off;
(5) collect centrifuged supernatant, lyophilize concentrated through reduced vacuum obtains this product.
Except specified otherwise, the raw material that the present invention relates to all commercially.
Positive progressive effect of the present invention is:
(1) the present invention adopts the lixiviate of ethanol acid adding, improves the pigment efficiency of pcr product utilizing merely organic solvent and utilize merely acid extraction.
(2) extraction of pigment be high-shear homogenizing machine auxiliary under carry out in two stages, it is less that the powder particle of shell becomes by the high speed homogenization of pretreatment stage, make it more easily be distributed in uniformly in solution, reach extraction effect relatively more even, extraction comparison is thorough; And extract the stage compared with the homogeneous under low rate, also comparatively standing extraction or other extracting method have higher pigment extraction yield.
(3) this extraction process is simple, and require low to production unit, extraction efficiency is high, and colors is survivable, is obviously better than traditional water bath extraction method.
(4) the pigment good water solubility of this processing method extraction, product appearance is bright in colour, and proterties is stablized, and is suitable for as foodstuff additive and healthy food material.
embodiment
Further illustrate the present invention by embodiment below, but the present invention is not limited.
Embodiment 1:
1) get fresh chestnut shell washing, dry, pulverize, cross 100 mesh sieves, for subsequent use.
2) take 100 grams of chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole of often liter of hydrochloric acid adjusts pH value to be 2.0, and solid-liquid ratio quality volume fraction is 1: 5.
3) under room temperature, 10000 rpms of high speed pre-treatment 10min, then filter after 3000 rpms of lower homogeneous extract 30min.
4) by above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous carry 5 hours, filter.
5) twice filtrate is merged, with the sodium hydroxide solution neutralization of 0.1 mole often liter, under 1000 rpms centrifugal 10 minutes, go precipitation, collect to carry out after supernatant concentrating, lyophilize is powdered, obtain Chestnut shell pigment 6.32 grams (color is brown), pigment extraction yield 96.5%.
Embodiment 2:
1) get fresh chestnut shell washing, dry, pulverize, cross 100 mesh sieves, for subsequent use.
2) take 100 grams of chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole of often liter of hydrochloric acid adjusts pH value to be 3.0, and solid-liquid ratio quality volume fraction is 1: 10.
3) under room temperature, 10000 rpms of high speed pre-treatment 20 minutes, then filter after 4000 rpms of lower homogeneous extract 60min.
4) by above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous extract 7 hours, filter.
5) twice filtrate is merged, with the sodium hydroxide solution of 0.1 mole often liter neutralization, under 1000 rpms centrifugal 15 minutes, go precipitation, collect to carry out after supernatant concentrating, lyophilize is powdered, obtains Chestnut shell pigment 6.67 grams, color is brown, pigment extraction yield 97.4%.
Embodiment 3:
1) get fresh chestnut shell washing, dry, pulverize, cross 100 mesh sieves, for subsequent use.
2) take 100 grams of chestnut shell powder, adding volume fraction is 95% ethanol, and 0.1 mole of often liter of hydrochloric acid adjusts pH value to be 4.0, and solid-liquid ratio quality volume fraction is 1: 7.
3) under room temperature, 9000 rpms of high speed pre-treatment 5min, then filter after 4000 rpms of lower homogeneous extract 45min.
4) by above-mentioned steps 3) in filter residue under 3000 rpms again homogeneous extract 8 hours, filter.
5) twice filtrate is merged, with the sodium hydroxide neutralization of 0.1 mole often liter, centrifugal 5min under 1000 rpms, go precipitation, collect to carry out after supernatant concentrating, lyophilize is powdered, obtain Chestnut shell pigment 6.15 grams (color is brown), pigment extraction yield 96.1%.
Embodiment 4:
(1) get fresh acorn cup drying, pulverizing, cross 100 mesh sieves, for subsequent use.
(2) 100 grams of acorn-case powders are taken, add the ethanol that volume fraction is 95%, the hydrochloric acid adjust pH of 0.1 mole often liter is 2.0, solid-liquid ratio is 1: 5 (quality volume fraction), high speed 9000 rpms process 5min under room temperature, filter after the lower homogeneous of low speed 3000 rpms extracts 30min again, collect filter residue, filtrate respectively.
(3) by filter residue by above-mentioned steps (2) reprocessing once, merge twice filtrate after filtering, with 0.1 mole of often liter of sodium hydroxide solution neutralization, the lower 1000 rpms of centrifugal 5min of normal temperature, collect supernatant liquor.
(4) supernatant liquor is after reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Brown Pigment From Acorn Shells, pigment extraction yield 96.85%.
Embodiment 5:
(1) get fresh acorn cup drying, pulverizing, cross 100 mesh sieves, for subsequent use.
(2) 100 grams of acorn-case powders are taken, add the ethanol that volume fraction is 95%, the hydrochloric acid adjust pH of 0.1 mole often liter is 3.0, solid-liquid ratio is 1: 7 (quality volume fraction), 9000 rpms of process 10 minutes are changed at a high speed under room temperature, filter after low speed 4000 rpms of lower homogeneous extract 45 minutes again, collect filter residue, filtrate respectively.
(3) by filter residue by above-mentioned steps (2) reprocessing once, after filtering, twice filtrate is merged, with the neutralization of 0.1 mole of often liter of sodium hydroxide solution, centrifugal 10 minutes of lower 1000 rpms of normal temperature, collection supernatant liquor.
(4) supernatant liquor is after reduced vacuum rotary evaporation is concentrated, and lyophilize is powdered, namely obtains Brown Pigment From Acorn Shells, pigment extraction yield 97.22%.
Claims (10)
1. a nature strength technique, is characterized in that comprising the following step:
(1) 100 mesh sieves are crossed by after raw material washing, drying, pulverizing, in the mixed solution of the aqueous ethanolic solution of percent by volume 60-95% and the aqueous hydrochloric acid of 0.1 mole often liter, carry out homogeneous extraction, the pH of described mixed solution is 2.0-5.0, filter after extracting, obtain filtrate; Described homogeneous extracts and comprises high speed pretreatment stage and homogeneous extraction stage;
(2) by the neutralization of step (1) gained filtrate, centrifugal slagging-off, supernatant liquor is obtained;
(3) supernatant liquor of step (2) gained is carried out concentrated and dry;
Wherein, described raw material is chestnut shell, Testa sojae atricolor, Hylocereus undatus pericarp etc.
2. the extracting method as described in claim 1, is characterized in that: in step (1), described described pulverize and sieve after raw material and mixed solution mixing after, solid-to-liquid ratio is mass volume ratio (w/v) 1g: 5ml-1g: 10ml.
3. the extracting method as described in claim 1, is characterized in that: in step (1), and the percent by volume of described aqueous ethanolic solution is 60%-90%.
4. the extracting method as described in claim 1, is characterized in that: in step (1), and it is commercially available high-shear homogenizing machine that described homogeneous extracts equipment used.
5. the extracting method as described in claim 1, is characterized in that: in step (1), and described high speed pretreatment stage condition is act on 5-20 minute under 5000-10000 rpm.
6. the extracting method as described in claim 1, is characterized in that: in step (1), and the condition that described homogeneous extracts the stage is process 30-60 minute under 1000-4000 rpm.
7. the extracting method as described in claim 1, is characterized in that: in step (1), and the temperature that described homogeneous extracts the stage is 20 ~ 35 DEG C; The time that described homogeneous extracts the stage is 5 ~ 8 hours; The number of times that described homogeneous extracts the stage is 1 ~ 3 time.
8. the extracting method as described in claim 1, is characterized in that: in step (2), and the method for described neutralization is for adding 0. mole of often liter of aqueous sodium hydroxide solution adjustment pH to 6 ~ 8; Described centrifugal condition is process 5-30 minute under 200-2000 rpm.
9. the extracting method as described in claim 8, is characterized in that: in step (2), and described centrifugal condition is centrifugal 5-15 minute under 1000 rpms.
10. the extracting method as described in claim 1, is characterized in that: in step (3), and described drying is lyophilize.
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| CN201310431447.XA CN104448907A (en) | 2013-09-22 | 2013-09-22 | Natural pigment extraction technology |
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| CN201310431447.XA CN104448907A (en) | 2013-09-22 | 2013-09-22 | Natural pigment extraction technology |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670337A (en) * | 2016-03-15 | 2016-06-15 | 常州市阿曼特化工有限公司 | Technology method for extracting pigment from black soy bean peels |
| CN107266343A (en) * | 2017-06-20 | 2017-10-20 | 广州市桐晖药业有限公司 | A kind of extraction process of natural bata-carotene |
| CN108218821A (en) * | 2018-03-29 | 2018-06-29 | 武汉雅仕博科技有限公司 | The method extracted from acorn cup, purify anthocyanidin |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN113462192A (en) * | 2021-07-01 | 2021-10-01 | 上海禧蓝纺织品有限公司 | Extraction and dyeing method of plant dye and plant mordant |
-
2013
- 2013-09-22 CN CN201310431447.XA patent/CN104448907A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105670337A (en) * | 2016-03-15 | 2016-06-15 | 常州市阿曼特化工有限公司 | Technology method for extracting pigment from black soy bean peels |
| CN107266343A (en) * | 2017-06-20 | 2017-10-20 | 广州市桐晖药业有限公司 | A kind of extraction process of natural bata-carotene |
| CN107266343B (en) * | 2017-06-20 | 2019-02-01 | 广州市桐晖药业有限公司 | A kind of extraction process of natural beta-carotin |
| CN108218821A (en) * | 2018-03-29 | 2018-06-29 | 武汉雅仕博科技有限公司 | The method extracted from acorn cup, purify anthocyanidin |
| CN109181356A (en) * | 2018-11-14 | 2019-01-11 | 罗莱生活科技股份有限公司 | A kind of technique extracted pigment from grape pip and prepare dyestuff |
| CN113462192A (en) * | 2021-07-01 | 2021-10-01 | 上海禧蓝纺织品有限公司 | Extraction and dyeing method of plant dye and plant mordant |
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Application publication date: 20150325 |