CN1939979A - Extraction of natural melanin from myrtillin leaves - Google Patents
Extraction of natural melanin from myrtillin leaves Download PDFInfo
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- CN1939979A CN1939979A CN 200510104210 CN200510104210A CN1939979A CN 1939979 A CN1939979 A CN 1939979A CN 200510104210 CN200510104210 CN 200510104210 CN 200510104210 A CN200510104210 A CN 200510104210A CN 1939979 A CN1939979 A CN 1939979A
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Abstract
Extraction of natural melanin from myrtillin chloride leaves is carried out by stocking, preparing buffer solution, preparing enzyme liquid, batching, enzymolyzing, and extracting to obtain the final product. It's safe, qualified, simple, convenient and efficient.
Description
Under technical field the present invention relates to a kind of extraction method of natural pigments, particularly a kind of from myrtillin leave the method for extraction of natural melanin.
Melanochrome in the background technology plant has the erythrolabe of promotion resynthesis, Vp model machine energy, improves blood microcirculation, antiulcer agent, anti-inflammatory, the anti-ageing multiple pharmacologically active of waiting for a long time.It comprises anthocyanidin, multiple pigment compositions such as flavonoid pigment, and it mainly is solvent-extraction process that melanochrome extracts.
" food and fermentation industries " delivers the article " extraction of flavonoid pigment and separation and purification in the myrtillin leave " of Wang Li, Yao Yuanhui on 2004 the 30th the 9th phases of volume, establish the optimum extraction condition of flavonoid pigment: extraction time 2 times, ethanol volume fraction 60%, 60 ℃ of temperature, solid-to-liquid ratio 1g: 35ml.
" Chinese wild plant resource " delivers the article " myrtillin leave pigment extraction process and pigment character are studied again " of Hu Zhijie, Jiang Ping etc. on 1997 the 22nd the 4th phases of volume, determine to make solvent with 55% ethanol, 55 ℃ of extractions, total extraction time is no more than 6.5 hours and is optimum.
Patent of invention " is extracted melanic method with Semen Sesami Nigrum " (application number: 91104469.8), introduced with the melanic method in the alkaline solution lixiviate Semen Sesami Nigrum.
" Chinese grain and oil journal " delivers the article " comparative studies of natural pigment character in black rice, Semen sojae atricolor, the Semen Sesami Nigrum " of Zhang Mingwei, Sun Ling etc. on 1998 the 13rd the 2nd phases of volume, introduced acidic alcohol solvent column chromatography and extracted melanic method.
Above-mentioned melanic extracting method does not all adopt zymin, influences melanic extraction yield.
Summary of the invention purpose of the present invention is to utilize zymin in conjunction with melanochrome in the solvent extraction myrtillin leave, improves melanic extraction yield.
Of the present invention a kind of from myrtillin leave the method for extraction of natural melanin, raw material is a myrtillin leave, reagent has polygalacturonase (30000IU), cellulase (15000IU), 95% ethanol (food grade), citric acid (food grade), Sodium phosphate dibasic (food grade).
Of the present invention a kind of from myrtillin leave the method for extraction of natural melanin, form by following steps:
(1) get the raw materials ready: with fresh myrtillin leave drying, pulverizing, 40 orders sieve, and it is standby to obtain myrtillin leave dry powder.
(2) preparation buffered soln: the 0.1mol/L citric acid solution is mixed by 1: 1.5～2 volume ratio with the 0.2mol/L disodium phosphate soln, and thin up is 2 times again, is mixed with buffered soln.
(3) preparation enzyme liquid: mix buffered soln, polygalacturonase and cellulase, and fully stirring is dissolved it fully, thereby form uniform enzyme liquid; The consumption of buffered soln is in myrtillin leave dry powder weight (kg): the ratio of volume of buffer solution (L)=1: 15～30 is calculated; The consumption of polygalacturonase and cellulase is that the buffered soln of every L adds 0.1～0.3g polygalacturonase and 0.1～0.3g cellulase.
(4) feed intake: in myrtillin leave dry powder weight (kg): the ratio of volume of buffer solution (L)=1: 15～30 adds myrtillin leave dry powder in the enzyme liquid.
(5) enzymolysis: after myrtillin leave dry powder and enzyme liquid stirred, lucifuge insulation in 50～55 ℃ thermostat water bath, every 30min stirs once, and enzymolysis 3～4h generates the mixture of enzymolysis solution and residue.
(6) extract: the 75-97% alcoholic acid method by every kg myrtillin leave dry powder adding 15～30L, 75-97% ethanol is added in above-mentioned enzymolysis solution and the residue mixture, under 60～65 ℃ of conditions, extract 2～3h, after filtration, obtain the black extracting solution.
(7) finished product: put the black extracting solution and in 60～70 ℃ baking oven, dry to constant weight, obtain natural black pigment.
Of the present invention a kind of from myrtillin leave the method for extraction of natural melanin, with the natural phant myrtillin leave is main raw material, adopt zymin in conjunction with the solvent extraction natural black pigment, its advantage is that the natural black pigment Product Safety is good, quality good (seeing Table 1), and the melanochrome extraction yield is followed the example of high by 30～40% than alcohol extracting, and enzyme preparation amount is few, and technology is simple, easy to operate, the efficient height is fit to suitability for industrialized production.Use polygalacturonase and cellulase can destroy in the plant material pectin substance that cell wall structure and iuntercellular thereof based on Mierocrystalline cellulose link to each other, the extraction resistance to mass transfer is reduced, make content melanochrome composition be easy to stripping.Ethanolic soln is as the melanic extraction solvent of pure dissolubility.Citric acid-phosphate buffer solution plays the effect of regulator solution pH value.By the buffered soln of method of the present invention preparation, its pH=6 after testing can guarantee the best effect of zymin effect.
Get the melanochrome extracting solution that melanochrome extracting solution of the present invention and alcohol extracting method obtain, all dilute 100 times, use the uv-spectrophotometric instrument, under the maximum absorption wavelength 243nm of pigment, measure its light absorption value (seeing Table 1).Adopt the melanochrome of enzyme process of the present invention in conjunction with solvent extraction, its light absorption value is 0.538, extracts melanic light absorption value 0.417 apparently higher than alcohol extracting method; Extraction yield is followed the example of high by 30% than alcohol extracting as calculated.
Table 1 enzyme process is in conjunction with the light absorption value contrast of solvent extraction and alcohol extracting method extraction
| Extracting method | Enzyme process is in conjunction with solvent extraction | Alcohol extracting method |
| Light absorption value (A) | 0.538 | 0.417 |
Specific embodiment: for fully disclose of the present invention a kind of from myrtillin leave the method for extraction of natural melanin, be illustrated below in conjunction with embodiment.
Embodiment: a kind of from myrtillin leave the method for extraction of natural melanin
The natural myrtillin leave of getting collection period and be the 5-6 month is a raw material, and extracting method may further comprise the steps:
(1) put fresh myrtillin leave and dry in 65 ℃ of baking ovens, pulverize with high-speed tissue mashing machine, 40 orders sieve, and it is standby to obtain myrtillin leave dry powder.
(2) get 0.1mol/L citric acid solution 180ml, 0.2mol/L disodium phosphate soln 320ml mixes and dilution is settled to 1000ml, is mixed with buffered soln.
(3) get the buffered soln of 250ml, add 0.05g polygalacturonase and 0.075g cellulase, stirring is dissolved it fully, forms uniform enzyme liquid.
(4) the myrtillin leave dry powder of adding 10g in above-mentioned enzyme liquid.
(5) the back lucifuge insulation in 50 ℃ thermostat water bath that stirs, every 30min stirs once, and enzymolysis 3h generates the mixture of enzymolysis solution and residue.
(6) in the mixture of enzymolysis solution and residue, add 250ml95% ethanol, under 60 ℃ of conditions, extract 2h, get the black extracting solution after filtration.
(7) put the black extracting solution and in 65 ℃ baking oven, dry to constant weight, obtain natural black pigment.
Claims (3)
1, a kind of from myrtillin leave the method for extraction of natural melanin, it is characterized in that forming by following steps:
(1) get the raw materials ready: with fresh myrtillin leave drying, pulverizing, 40 orders sieve, and it is standby to obtain myrtillin leave dry powder;
(2) preparation buffered soln: the 0.1mol/L citric acid solution is mixed by 1: 1.5～2 volume ratio with the 0.2mol/L disodium phosphate soln, and thin up is 2 times again, is mixed with buffered soln;
(3) preparation enzyme liquid: mix buffered soln, polygalacturonase and cellulase, and fully stirring is dissolved it fully, thereby form uniform enzyme liquid; The consumption of buffered soln is in myrtillin leave dry powder weight (kg): the ratio of volume of buffer solution (L)=1: 15～30 is calculated; The consumption of polygalacturonase and cellulase is that the buffered soln of every L adds 0.1～0.3g polygalacturonase and 0.1～0.3g cellulase;
(4) feed intake: in myrtillin leave dry powder weight (kg): the ratio of volume of buffer solution (L)=1: 15～30 adds myrtillin leave dry powder in the enzyme liquid;
(5) enzymolysis: after myrtillin leave dry powder and enzyme liquid stirred, lucifuge insulation in 50～55 ℃ thermostat water bath, every 30min stirs once, and enzymolysis 3～4h generates the mixture of enzymolysis solution and residue;
(6) extract: the 75-97% alcoholic acid method by every kg myrtillin leave dry powder adding 15～30L, 75-97% ethanol is added in above-mentioned enzymolysis solution and the residue mixture, under 60～65 ℃ of conditions, extract 2～3h, after filtration, obtain the black extracting solution;
(7) finished product: put the black extracting solution and in 60～70 ℃ baking oven, dry to constant weight.
2, according to claim 1 a kind of from myrtillin leave the method for extraction of natural melanin, it is characterized in that forming by following steps:
(1) put fresh myrtillin leave and dry in 65 ℃ of baking ovens, pulverize with high-speed tissue mashing machine, 40 orders sieve, and it is standby to obtain myrtillin leave dry powder;
(2) get 0.1mol/L citric acid solution 180ml, 0.2mol/L disodium phosphate soln 320ml mixes and dilution is settled to 1000ml, is mixed with buffered soln;
(3) get the buffered soln of 250ml, add 0.05g polygalacturonase and 0.075g cellulase, stirring is dissolved it fully, forms uniform enzyme liquid;
(4) the myrtillin leave dry powder of adding 10g in above-mentioned enzyme liquid;
(5) the back lucifuge insulation in 50 ℃ thermostat water bath that stirs, every 30min stirs once, and enzymolysis 3h generates the mixture of enzymolysis solution and residue;
(6) in the mixture of enzymolysis solution and residue, add 250ml95% ethanol, under 60 ℃ of conditions, extract 2h, get the black extracting solution after filtration;
(7) putting the black extracting solution dries to constant weight in 65 ℃ baking oven.
3, according to the natural black pigment of the method for claim 1 or 2 preparation.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102399824A (en) * | 2010-09-13 | 2012-04-04 | 浙江医药股份有限公司新昌制药厂 | Method for preparing plant carbon black substitute by using leaves of Vaccinium plants as raw material |
| CN102558901A (en) * | 2010-12-14 | 2012-07-11 | 武汉华珍药业有限公司 | Method for extracting brown pigment in acorn shells by enzymolysis |
| CN102732048A (en) * | 2012-05-29 | 2012-10-17 | 天津北洋百川生物技术有限公司 | Extraction method for melanin of Aureobasidium pullulans |
| CN102747105A (en) * | 2011-04-19 | 2012-10-24 | 浙江医药股份有限公司新昌制药厂 | Method for preparing water-soluble plant melanin |
| CN103113756A (en) * | 2013-03-06 | 2013-05-22 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
| CN103408964A (en) * | 2013-08-15 | 2013-11-27 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
| CN103468747A (en) * | 2013-09-27 | 2013-12-25 | 江苏九久环境科技有限公司 | Method for preparing vaccinium bracteatum thunb leaf pigment through enzymic method |
| CN107261157A (en) * | 2017-06-14 | 2017-10-20 | 苏州大学 | Inclusion compound of blueberry leaf melanin and its preparation method and application |
| CN108354111A (en) * | 2018-01-08 | 2018-08-03 | 浙江大学 | Natural colorant and its preparation method and application based on oriental blueberry leaf |
| CN109097413A (en) * | 2018-08-01 | 2018-12-28 | 江南大学 | A method of the different indigo pigments of tone are prepared based on Vaccinium bracteatum Thunb. Leaves |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1181079A (en) * | 1967-03-03 | 1970-02-11 | Vnii Chainoi Promy | Colour Derived from Vegetable Raw Material and method of manufacturing the same |
| WO1980002695A1 (en) * | 1979-06-04 | 1980-12-11 | Mauri Brothers & Thomson | Edible colourant |
| RU2018511C1 (en) * | 1992-11-11 | 1994-08-30 | Всероссийский научно-исследовательский институт консервной и овощесушильной промышленности | Method for producing food dye of vegetable raw materials |
| CN1160064A (en) * | 1997-01-14 | 1997-09-24 | 王国良 | Method for extracting melanin using lauraceae tree leaves and use thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102399824A (en) * | 2010-09-13 | 2012-04-04 | 浙江医药股份有限公司新昌制药厂 | Method for preparing plant carbon black substitute by using leaves of Vaccinium plants as raw material |
| CN102399824B (en) * | 2010-09-13 | 2013-08-07 | 浙江医药股份有限公司新昌制药厂 | Method for preparing plant carbon black substitute by using leaves of Vaccinium plants as raw material |
| CN102558901A (en) * | 2010-12-14 | 2012-07-11 | 武汉华珍药业有限公司 | Method for extracting brown pigment in acorn shells by enzymolysis |
| CN102747105B (en) * | 2011-04-19 | 2014-10-08 | 浙江医药股份有限公司新昌制药厂 | Method for preparing water-soluble plant melanin |
| CN102747105A (en) * | 2011-04-19 | 2012-10-24 | 浙江医药股份有限公司新昌制药厂 | Method for preparing water-soluble plant melanin |
| CN102732048A (en) * | 2012-05-29 | 2012-10-17 | 天津北洋百川生物技术有限公司 | Extraction method for melanin of Aureobasidium pullulans |
| CN103113756A (en) * | 2013-03-06 | 2013-05-22 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
| CN103113756B (en) * | 2013-03-06 | 2014-12-10 | 无锡市金和泰农业生物技术有限公司 | Method for efficiently extracting and preparing vaccinium leaves pigment |
| CN103408964A (en) * | 2013-08-15 | 2013-11-27 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
| CN103408964B (en) * | 2013-08-15 | 2014-12-10 | 宜兴市红豆杉生态科技有限公司 | Method for improving extraction yield of melanin in Vaccinium bracteatum Thunb by using polyphenol oxidase and tea polyphenol |
| CN103468747A (en) * | 2013-09-27 | 2013-12-25 | 江苏九久环境科技有限公司 | Method for preparing vaccinium bracteatum thunb leaf pigment through enzymic method |
| CN103468747B (en) * | 2013-09-27 | 2015-02-18 | 江苏九久环境科技有限公司 | Method for preparing vaccinium bracteatum thunb leaf pigment through enzymic method |
| CN107261157A (en) * | 2017-06-14 | 2017-10-20 | 苏州大学 | Inclusion compound of blueberry leaf melanin and its preparation method and application |
| CN107261157B (en) * | 2017-06-14 | 2020-01-10 | 苏州大学 | Inclusion compound of vaccinium bracteatum leaf melanin and preparation method and application thereof |
| CN108354111A (en) * | 2018-01-08 | 2018-08-03 | 浙江大学 | Natural colorant and its preparation method and application based on oriental blueberry leaf |
| CN108354111B (en) * | 2018-01-08 | 2022-05-17 | 浙江大学 | Natural colorant based on Vaccinium bracteatum leaves, and preparation method and application thereof |
| CN109097413A (en) * | 2018-08-01 | 2018-12-28 | 江南大学 | A method of the different indigo pigments of tone are prepared based on Vaccinium bracteatum Thunb. Leaves |
| CN109097413B (en) * | 2018-08-01 | 2020-12-29 | 江南大学 | Method for preparing indigo pigment with different colors based on vaccinium bracteatum leaves |
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| CN100562543C (en) | 2009-11-25 |
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