CN103013164A - Method for extracting natural pigment from persimmon peels - Google Patents
Method for extracting natural pigment from persimmon peels Download PDFInfo
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- CN103013164A CN103013164A CN2012105399042A CN201210539904A CN103013164A CN 103013164 A CN103013164 A CN 103013164A CN 2012105399042 A CN2012105399042 A CN 2012105399042A CN 201210539904 A CN201210539904 A CN 201210539904A CN 103013164 A CN103013164 A CN 103013164A
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- pericarpium kaki
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Abstract
The invention discloses a method for extracting natural pigment from persimmon peels. The method comprises the steps of taking peels obtained during the dried persimmon production as the raw material, extracting and separating the persimmon peel pigment by utilizing countercurrent and macroporous adsorption resin, wherein during the countercurrent extraction, a heated solvent is adopted for carrying out reverse extraction on the persimmon peel raw material, so that the concentration difference of the solvent is formed in the flowing process, the solvent can also be in full contact with medicines, the leaching of active ingredients is benefited and the reverse flowing plays a role of fully stirring in the extracting process at the same time; and by utilizing the macroporous adsorption resin, natural pigment ingredients can be selectively adsorbed, the production is simple and easy to control and high-content natural pigment can be separated. The method disclosed by the invention is easy to operate and little in investment and has the advantages that by adopting efficient and energy saving countercurrent extraction technology, the natural pigment of the persimmon peels is fully extracted by using small-times amount solvent and short extraction time; shortcomings of long extraction time, large solvent times amount, low extraction rate of extraction modes such as percolation and soaking are overcome; the extract purity is increased; and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of method of extracting natural pigment from Pericarpium Kaki.
Background technology
Food dye is the chief component of foodstuff additive, and it not only is widely used in foodstuffs industry to improve the color and luster of food, increases people to Beautiful treat, and is widely used in medicine and cosmetic industry, to increase the external quality of commodity.Synthetic colour is because its security is lower, and use is subject to certain restrictions, thereby the T of exploitation extraction pigment take edible animals and plants as raw material more and more receives people's concern.
Pericarpium Kaki is the pericarp of dicotyledons Ebenaceae persimmon [Diospyros Kaki L.f].The history in existing more than 1,000 year of the cultivation of persimmon tree.The Northern Song Dynasty, poet Zhang Zhongshu claimed that " Hua Linfangdi that distinguished the flavor of, look Yang Jing Shen Zhu that holds concurrently, gently even deep red wax is wrapped up in a shortcake to U.S. persimmon ︰, unlike human world sweet dew." contain abundant natural pigment in the Pericarpium Kaki, at present, have report to extract pigment in the persimmon pericarps with methods such as immersions, diafiltrations, but these method extraction time length, solvent consumption are large, extraction yield is low, is not suitable for commercial scale production.
Summary of the invention
The purpose of this invention is to provide the method that a kind of Pericarpium Kaki extracts natural pigment.The skin that the method is transferred to when producing dried persimmon extracts as raw material, and technique is simple and easy to control, and extraction time is short, extraction yield is high, production cost is low.
The technical scheme that realizes the object of the invention is: a kind of Pericarpium Kaki extracts the method for natural pigment, the skin of transfering to during take the production dried persimmon is as raw material, utilize countercurrent extraction to separate the Pericarpium Kaki pigment in conjunction with the macroporous adsorbent resin separation and Extraction, the solvent of countercurrent extraction utilization heating is reverse to be extracted the Pericarpium Kaki raw material, make solvent in flow process, form concentration difference, solvent also can fully contact with medicinal material, more be conducive to the leaching of effective constituent, well-beaten effect is played in simultaneously countercurrent flow in leaching process; Utilize the macroporous adsorbent resin can selective adsorption natural pigment composition, produce simple and easy to controlly, and isolate the high natural pigment of content.
Its concrete extracting method may further comprise the steps:
1, in countercurrent extractor, add Pericarpium Kaki, the low-carbon alcohol that 5-7 times of concentration of adding raw material is 60-80%, temperature is controlled at 70-80 ℃ of countercurrent extraction 90min, extracts three times, united extraction liquid, smart worry obtains the Pericarpium Kaki extracting solution;
2, be 60 ℃ below concentrating under reduced pressure at pressure for-0.08MPa, temperature with the Pericarpium Kaki extracting solution, reclaim alcohol, behind the Recycled ethanol, the 3-5 that is concentrated to raw material doubly measures;
3, the Pericarpium Kaki concentrated solution is filtered with sheet frame first, through macroporous adsorptive resins absorption, flow rate control is at 0.5-1.5V/hr again for its filtrate; After resin absorption is saturated, washed 3 hours with pure water, flow rate control is at 1-2 V/hr; With the absorption of 50% ethanolysis, flow rate control is washed till the elutriant color and shoals at 0.5-1.5V/hr, collects elutriant at last;
4, be 60 ℃ below concentrated at pressure for-0.08MPa, temperature with elutriant, Recycled ethanol;
5, with the concentrated solution vacuum microwave drying, its microwave pressure is below 60 ℃ for-0.08MPa, temperature, pulverizes and obtains Pericarpium Kaki natural pigment powder.
Low-carbon alcohol described in the step 1 is methyl alcohol, ethanol, propyl carbinol.
Resin model described in the step 3 is D101, D130, HPD100
Present method is extracted the Pericarpium Kaki natural pigment that separates, and its Pericarpium Kaki natural pigment content is more than 60%.
The invention has the beneficial effects as follows: (1) uses energy-efficient countercurrent extraction technology, use the solvent of little times of amount, short extraction time fully extracts the Pericarpium Kaki natural pigment, has overcome the shortcoming that the extracting mode such as diafiltration, immersion extraction time is long, solvent is doubly measured greatly, extraction yield is not high; (2) improved the purity of extract, reduced production cost, simple to operate, less investment is more suitable for industrialized production.
Embodiment
Embodiment 1
Take by weighing Pericarpium Kaki 100kg and put into countercurrent extractor, at container for storing liquid heating 600L60% ethanol, with pump ethanol is inputted instant well heater (pure water is heated to 70-80 ℃) heating and afterwards the Herba Centellae raw material in the extractor is carried out countercurrent extraction, in the leaching process, temperature is controlled at 70-80 ℃ in the extractor, extract 90min, emit extracting solution; Add 600L60% ethanol in extractor, carry out the countercurrent extraction second time, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; Add 600L60% ethanol in extractor, carry out for the third time countercurrent extraction, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; United extraction liquid, concentration and recovery ethanol obtains Pericarpium Kaki concentrated solution 400L.The Pericarpium Kaki concentrated solution is crossed first Plate Filtration, and filtrate is advanced macroporous adsorbent resin D101, and flow rate control is at 0.5-1.5V/hr; After resin absorption is saturated, washed 3 hours with pure water, flow rate control is at 1-2 V/hr; With the absorption of 50% ethanolysis, flow rate control is washed till the elutriant color and shoals at 0.5-1.5V/hr, collects elutriant at last.With elutriant concentration and recovery ethanol (pressure :-0.08MPa, temperature: below 60 ℃).Concentrated solution with vacuum microwave drying (pressure :-0.08MPa, temperature: below 60 ℃), is pulverized, and sterilising packaging obtains Pericarpium Kaki natural pigment powder finished product.
Embodiment 2
Take by weighing Pericarpium Kaki 100kg and put into countercurrent extractor, at container for storing liquid heating 600L60% methyl alcohol, with pump ethanol is inputted instant well heater (pure water is heated to 70-80 ℃) heating and afterwards the Herba Centellae raw material in the extractor is carried out countercurrent extraction, in the leaching process, temperature is controlled at 70-80 ℃ in the extractor, extract 90min, emit extracting solution; Add 600L60% methyl alcohol in extractor, carry out the countercurrent extraction second time, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; Add 600L60% methyl alcohol in extractor, carry out for the third time countercurrent extraction, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; United extraction liquid, concentration and recovery methyl alcohol obtains Pericarpium Kaki concentrated solution 400L.The Pericarpium Kaki concentrated solution is crossed first Plate Filtration, and filtrate is advanced macroporous adsorbent resin D130, and flow rate control is at 0.5-1.5V/hr; After resin absorption is saturated, washed 3 hours with pure water, flow rate control is at 1-2 V/hr; With the absorption of 50% ethanolysis, flow rate control is washed till the elutriant color and shoals at 0.5-1.5V/hr, collects elutriant at last.With elutriant concentration and recovery ethanol (pressure :-0.08MPa, temperature: below 60 ℃).Concentrated solution with vacuum microwave drying (pressure :-0.08MPa, temperature: below 60 ℃), is pulverized, and sterilising packaging obtains Pericarpium Kaki natural pigment powder finished product.
Embodiment 3
Take by weighing Pericarpium Kaki 100kg and put into countercurrent extractor, at the saturated propyl carbinol of container for storing liquid heating 600L, with pump ethanol is inputted instant well heater (pure water is heated to 70-80 ℃) heating and afterwards the Herba Centellae raw material in the extractor is carried out countercurrent extraction, in the leaching process, temperature is controlled at 70-80 ℃ in the extractor, extract 90min, emit extracting solution; Add the saturated propyl carbinol of 600L in extractor, carry out the countercurrent extraction second time, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; Add the saturated propyl carbinol of 600L in extractor, carry out for the third time countercurrent extraction, temperature is controlled at 70-80 ℃ in the extractor, extracts 90min, emits extracting solution; United extraction liquid, the concentration and recovery propyl carbinol adds water and obtains Pericarpium Kaki concentrated solution 400L.The Pericarpium Kaki concentrated solution is crossed first Plate Filtration, and filtrate is advanced macroporous adsorbent resin HPD100, and flow rate control is at 0.5-1.5V/hr; After resin absorption is saturated, washed 3 hours with pure water, flow rate control is at 1-2 V/hr; With the absorption of 50% ethanolysis, flow rate control is washed till the elutriant color and shoals at 0.5-1.5V/hr, collects elutriant at last.With elutriant concentration and recovery ethanol (pressure :-0.08MPa, temperature: below 60 ℃).Concentrated solution with vacuum microwave drying (pressure :-0.08MPa, temperature: below 60 ℃), is pulverized, and sterilising packaging obtains Pericarpium Kaki natural pigment powder finished product.
Claims (3)
1. a method of extracting natural pigment from Pericarpium Kaki comprises the steps:
(1) add Pericarpium Kaki in countercurrent extractor, 5-7 times of adding material quantity, its concentration are the low-carbon alcohol of 60-80%, and temperature is controlled at 70-80 ℃ of countercurrent extraction 90min, extract three times, and united extraction liquid, smart worry obtains the Pericarpium Kaki extracting solution;
(3) filter with sheet frame after the Pericarpium Kaki extracting solution is concentrated, through macroporous adsorptive resins absorption, flow rate control is at 0.5-1.5V/hr again for its filtrate; After resin absorption is saturated, washed 3 hours with pure water, flow rate control is at 1-2 V/hr; With the absorption of 50% ethanolysis, flow rate control is washed till the elutriant color and shoals at 0.5-1.5V/hr, collects elutriant at last;
(4) elutriant is concentrated, Recycled ethanol;
(5) with the concentrated solution vacuum microwave drying, pulverize and obtain Pericarpium Kaki natural pigment powder.
2. method according to claim 1, it is characterized in that: the low-carbon alcohol described in the step 1 is methyl alcohol, ethanol or propyl carbinol.
3. method according to claim 1, it is characterized in that: the resin model described in the step 3 is D101, D130 or HPD100.
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| CN2012105399042A CN103013164A (en) | 2012-12-14 | 2012-12-14 | Method for extracting natural pigment from persimmon peels |
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| CN2012105399042A CN103013164A (en) | 2012-12-14 | 2012-12-14 | Method for extracting natural pigment from persimmon peels |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804945A (en) * | 2014-01-24 | 2014-05-21 | 武汉市林业果树科学研究所 | Extraction method of black persimmon peel pigment |
| CN104559304A (en) * | 2014-12-19 | 2015-04-29 | 桂林得坤生物科技股份有限公司 | Method for extracting pigment in persimmon |
| CN104693834A (en) * | 2015-03-31 | 2015-06-10 | 桂林得坤生物科技股份有限公司 | Method for preparing persimmon fruit pigments |
| CN108541909A (en) * | 2018-03-09 | 2018-09-18 | 陕西农产品加工技术研究院 | By-product Pericarpium Kaki is processed into the crisp method of Pericarpium Kaki in a kind of dried persimmon process |
| CN109575635A (en) * | 2019-01-23 | 2019-04-05 | 西北农林科技大学 | The extraction separation method of persimmon natural pigment |
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| JP2007046015A (en) * | 2005-08-12 | 2007-02-22 | Tohoku Univ | Method for producing carotenoid pigment |
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN102321982A (en) * | 2011-08-10 | 2012-01-18 | 无锡市联盛印染有限公司 | Dyeing method by using persimmon natural dye |
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2012
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Patent Citations (5)
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| KR20030042320A (en) * | 2001-11-22 | 2003-05-28 | (주)우리 | Extraction method of persimmon juice for natural dyeing and automatic dyeing system thereof |
| CN1786081A (en) * | 2004-12-10 | 2006-06-14 | 西北工业大学 | Method of extracting natural yellow pigment from persimon leaf or persion bark |
| JP2007046015A (en) * | 2005-08-12 | 2007-02-22 | Tohoku Univ | Method for producing carotenoid pigment |
| CN101381420A (en) * | 2008-10-30 | 2009-03-11 | 河北科技大学 | Continuous extraction method of pectin, tannin and pigment from persimmon exocarp |
| CN102321982A (en) * | 2011-08-10 | 2012-01-18 | 无锡市联盛印染有限公司 | Dyeing method by using persimmon natural dye |
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| 贾贵东: "柿子皮乙醇提取物的体外抗氧化活性研究", 《陕西师范大学硕士学位论文》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804945A (en) * | 2014-01-24 | 2014-05-21 | 武汉市林业果树科学研究所 | Extraction method of black persimmon peel pigment |
| CN103804945B (en) * | 2014-01-24 | 2015-05-27 | 武汉市林业果树科学研究所 | Extraction method of black persimmon peel pigment |
| CN104559304A (en) * | 2014-12-19 | 2015-04-29 | 桂林得坤生物科技股份有限公司 | Method for extracting pigment in persimmon |
| CN104693834A (en) * | 2015-03-31 | 2015-06-10 | 桂林得坤生物科技股份有限公司 | Method for preparing persimmon fruit pigments |
| CN108541909A (en) * | 2018-03-09 | 2018-09-18 | 陕西农产品加工技术研究院 | By-product Pericarpium Kaki is processed into the crisp method of Pericarpium Kaki in a kind of dried persimmon process |
| CN108541909B (en) * | 2018-03-09 | 2021-08-10 | 陕西农产品加工技术研究院 | Method for processing persimmon peel into crisp persimmon peel in persimmon cake processing process |
| CN109575635A (en) * | 2019-01-23 | 2019-04-05 | 西北农林科技大学 | The extraction separation method of persimmon natural pigment |
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Application publication date: 20130403 |