CN101885925B - Method for extracting brown pigment from oil-tea camellia husks - Google Patents
Method for extracting brown pigment from oil-tea camellia husks Download PDFInfo
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- CN101885925B CN101885925B CN 201010221929 CN201010221929A CN101885925B CN 101885925 B CN101885925 B CN 101885925B CN 201010221929 CN201010221929 CN 201010221929 CN 201010221929 A CN201010221929 A CN 201010221929A CN 101885925 B CN101885925 B CN 101885925B
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Abstract
The invention discloses a method for extracting a brown pigment from oil-tea camellia husks. The method comprises the following steps of: cleaning the oil-tea camellia husks, drying the cleaned oil-tea camellia husks in the sun, and grinding the oil-tea camellia husks into powder; mixing the oil-tea camellia husk powder with water or ethanol, and performing ultrasonic extraction to obtain extraction mixed solution; performing suction filtration on the extraction mixed solution to obtain filtrate; performing reduced pressure distillation on the filtrate to evaporate the ethanol out so as to obtain concentrated pigment solution; adjusting the pH value of the concentrated pigment solution, and then adsorbing the concentrated pigment solution by using a chromatography column; eluting the chromatography column by using the ethanol to obtain purified pigment solution; performing reduced pressure distillation on the purified pigment solution to evaporate the ethanol out so as to obtain concentrated purified pigment solution; and performing vacuum drying on the concentrated purified pigment solution to obtain a brown pigment product. The method has a simple process, the needed instruments and equipment are common, the extraction rate can reach 3.0 to 5.6 percent, and the color value is high; the raw materials are the oil-tea camellia husks and can be changed from waste into valuable, the ethanol in the production process can be recycled, and the production cost is low; besides, the method uses the water or the ethanol as an extracting agent which causes no adverse effect on the environment.
Description
Technical field
The present invention relates to plant brown pigments production technical field, specifically a kind of method of extracting brown pigments from oil-tea camellia husks.
Background technology
Food dye is divided into two classes usually: edible natural pigment and edible synthesized coloring matter.Synthetic colour is owing to having strong coloring force, lovely luster, good stability, odorless, tasteless, quality homogeneous, is easy to dissolving and colorant match, and the advantage such as with low cost, once once is widely used.But, the event such as Sudan red, malachite green has caused that one takes turns the another food safety caution of taking turns, thereby people also deepen gradually to synthetic colour security doubt, and natural pigment, but constantly embody it self to the advantage of the useful many uniquenesses of human health, the natural food colour of greatly developing " natural, nutrition, multi-functional " is the developing policy of China's food dye industry.In addition, China has rich and varied animal and plant resource, the flower of a lot of plants, leaf, really, the shell of skin or animal, meat etc. all contain various pigments, and these pigments are except as also having the several functions composition tinting material, therefore can extract natural pigment from the tankage of the herbal medicine of medicine-food two-purpose and animal.Therefore, many-sided development research and application natural pigment to guaranteeing the mankind's health, promote green food industry all to be of great significance.
There is oil tea fifty-five million mu in China, and main product is in the south China each province, annual produce oil 1,500,000,000 kg, and this will bring the oil-tea camellia husks of more than 100 hundred million kg.Oil tea has very high comprehensive utilization value, contain tea saponin, tea seed polysaccharide, tea seed albumen etc. in leached tea oil slag, be all the raw material of chemical industry, light industry, food, fodder industry product etc., tea seed shell also can be made into furfural, gac etc., tea shell or a kind of good culture medium of edible fungus.Oil-tea camellia husks comprises fruit Pu shell and plants shell two portions, but China's oil-tea camellia husks does not almost utilize and discards.Although in recent years the utilization research of oil-tea camellia husks is also being carried out rapidly, present research only concentrates in the preparation of furfural, gac and Xylitol.Oil-tea camellia husks contains the pigment of suitable composition, and Liu Xiaogeng has reported the composition analysis and utilization research of oil tea byproduct in 1993, measure the yield of tea pigment (oil-tea camellia husks pigment, tea-cake dregs pigment) and have light stability and thermostability preferably.Ling Chengde etc. have reported domestic edible natural pigment tea oil shell brown pigments toxicity test in 1985, pointed out that the oil-tea camellia husks brown pigments is a kind of safe natural food colour.Find according to applicant's research, the brown pigments that contains in oil-tea camellia husks can reach 4.0～5.9%, extracts brown pigments take oil-tea camellia husks as raw material, can turn waste into wealth, and increases economic efficiency.Up to the present, the extraction of oil-tea camellia husks brown pigments research yet there are no report.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting brown pigments from oil-tea camellia husks.
The method of extracting brown pigments from oil-tea camellia husks of the present invention comprises the following steps:
(1) oil-tea camellia husks is cleaned with clear water, dried, use the grinder mill powdered, cross 40 mesh sieves;
(2) getting oil-tea camellia husks powder and water or volume fraction is that 10～80% ethanol mixes with the ratio of 1g: 10～20mL, be 300～500W at ultrasonic power, extract temperature and be under the condition of 30～50 ℃, supersound extraction 10～30min obtains extracting mixed solution;
(3) will extract mixed solution suction filtration under vacuum tightness 0.09～0.05MPa condition, obtain filtrate;
(4) get filtrate underpressure distillation under vacuum tightness 0.09～0.05MPa condition, ethanol is steamed, obtain concentrated pigment solution;
(5) concentrating pigment solution, to be adjusted to the pH value with citric acid-dipotassium hydrogen phosphate damping fluid be 5.5～6.5, under 15～35 ℃ with the flow velocity of 1～3mL/min, press 10～10.5 times of volumes of resin bed volume, adsorb by the chromatography column that the D-101 macroporous resin of handling well is housed;
(6) under 15～35 ℃, with volume fraction 80% ethanol elution chromatography column, eluent flow rate is 1～3ml/min, and efflux volume is 10～10.5BV (resin bed volume), obtains the purifying pigment solution;
(7) with the underpressure distillation under the condition of vacuum tightness 0.09～0.05Mpa of purifying pigment solution, steam etoh solvent, the purifying pigment solution that obtains concentrating;
(8) with concentrated purifying pigment solution vacuum-drying, drying temperature is 25～50 ℃, obtains the brown pigments product.
The inventive method extracts from oil-tea camellia husks that the brown pigments extraction process is simple, and required plant and instrument is common, and extraction yield can reach 3.0～5.6%, and the look valency is higher; Raw material is oil-tea camellia husks discarded in the tea oil production process, can turn waste into wealth, and the etoh solvent in production process can recycle and reuse, and production cost is low; And water or ethanol cooks extraction agent, and production process has no adverse effects to environment.
Embodiment
Below by embodiment, the present invention is done further specific descriptions, but embodiments of the present invention are not limited to this.
Oil-tea camellia husks is cleaned with clear water, dried, use the grinder mill powdered, cross 40 mesh sieves standby; Accurately take the above-mentioned standby oil-tea camellia husks powder of 5.0g, be placed in 150mL tool plug Erlenmeyer flask, add the ethanolic soln 50mL of volume fraction 40%, stir with glass rod, the oil-tea camellia husks powder is immersed in solution fully.Under the condition of 40 ℃ of ultrasonic power 400W, temperature, supersound extraction 15min, suction filtration obtains filtrate;
With filtrate underpressure distillation under vacuum tightness 0.09Mpa condition, steam most of ethanol; Obtain concentrated pigment solution, cooling after, add the dipotassium hydrogen phosphate solution of 0.2mol/L of 12.6mL and the citric acid solution of 7.4mL 0.1mol/L, this moment, pH value of solution=6, be pigment solution;
At 20 ℃ of flow velocitys with 1mL/min, press 10 times of volumes of resin bed volume, adsorb by the chromatography column that the D-101 macroporous resin of handling well is housed;
With 80% ethanol elution, eluent flow rate is 2ml/min, and efflux volume is 10BV, obtains the purifying pigment solution;
The underpressure distillation under vacuum tightness 0.05Mpa condition of purifying pigment solution is steamed solvent, the purifying pigment solution that obtains concentrating;
With concentrated purifying pigment solution vacuum-drying, 35 ℃ of drying temperatures obtain brown pigments product 0.2005g, productive rate 4.01%.
Measuring the above-mentioned look valency that makes pigment according to 2.2 potassium dichromate solution colorimetries in GB5525 is 22.9.These pigmentary colours are coffee-like, and are identical or close with general brown pigments character.Pigment is water-soluble, is dissolved in ethanol, is dissolved in hardly non-polar solvent.The polyphenol qualitative reaction is positive, and to general oxygenant, reductive agent stable in properties, temperature is stable in 0～100 ℃ of scope, and is stable to common metal ion.Near ultraviolet region 278nm, absorption peak is arranged, 1718cm in infrared spectra
-1, 1610cm
-1, 1219cm
-1Near strong absorption band is arranged.
Claims (1)
1. a method of extracting brown pigments from oil-tea camellia husks, is characterized in that, comprises the following steps:
(1) oil-tea camellia husks is cleaned with clear water, dried, use the grinder mill powdered, cross 40 mesh sieves;
(2) getting oil-tea camellia husks powder and volume fraction is that 10～80% ethanol mixes with the ratio of 1g: 10～20mL, is 300～500W at ultrasonic power, extracts temperature and is under the condition of 30～50 ℃, and supersound extraction 10～30min obtains extracting mixed solution;
(3) will extract mixed solution suction filtration under vacuum tightness 0.09～0.05MPa condition, obtain filtrate;
(4) get filtrate underpressure distillation under vacuum tightness 0.09～0.05MPa condition, ethanol is steamed, obtain concentrated pigment solution;
(5) concentrating pigment solution, to be adjusted to the pH value with citric acid-dipotassium hydrogen phosphate damping fluid be 5.5～6.5, under 15～35 ℃ with the flow velocity of 1～3mL/min, press 10～10.5 times of volumes of resin bed volume, adsorb by the chromatography column that the D-101 macroporous resin of handling well is housed;
(6) under 15～35 ℃, with volume fraction 80% ethanol elution chromatography column, eluent flow rate is 1～3mL/min, and efflux volume is 10～10.5BV resin bed volume, obtains the purifying pigment solution;
(7) with the underpressure distillation under the condition of vacuum tightness 0.09～0.05MPa of purifying pigment solution, steam etoh solvent, the purifying pigment solution that obtains concentrating;
(8) with concentrated purifying pigment solution vacuum-drying, drying temperature is 25～50 ℃, obtains the brown pigments product.
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| CN 201010221929 CN101885925B (en) | 2010-07-01 | 2010-07-01 | Method for extracting brown pigment from oil-tea camellia husks |
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| CN 201010221929 CN101885925B (en) | 2010-07-01 | 2010-07-01 | Method for extracting brown pigment from oil-tea camellia husks |
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| CN101885925A CN101885925A (en) | 2010-11-17 |
| CN101885925B true CN101885925B (en) | 2013-05-15 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516803B (en) * | 2010-12-14 | 2013-05-08 | 常州云卿纺织品有限公司 | Camellia oleifera shell dye liquor prepared from camellia oleifera shells, preparation method of the camellia oleifera shell dye liquor, and dyeing method adopting the camellia oleifera shell dye liquor |
| CN102153882B (en) * | 2011-02-24 | 2015-08-12 | 常州大学 | Reddish-brown natural dye of oil-tea camellia shells extracts and dyeing process |
| CN102210786B (en) * | 2011-06-08 | 2012-09-05 | 中国林业科学研究院林产化学工业研究所 | Method for extracting natural antioxidant from shells of camellia oleifera |
| CN105441508A (en) * | 2015-11-25 | 2016-03-30 | 华南理工大学 | Tea seed coat xylooligosaccharide and preparation method thereof |
| CN105710107B (en) * | 2016-01-30 | 2018-11-16 | 贵州民族大学 | The method and system of Compositions of Bamboo Shoot Shell high value comprehensive utilization |
| CN106221284B (en) * | 2016-07-29 | 2018-05-08 | 威海大洋纺织有限公司 | A kind of extraction process of vegetable dyeing agent |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556150A (en) * | 2004-01-12 | 2004-12-22 | 四川大学 | Extraction and separation of proto flower haematochrome and preparation method of its derivatives |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556150A (en) * | 2004-01-12 | 2004-12-22 | 四川大学 | Extraction and separation of proto flower haematochrome and preparation method of its derivatives |
Non-Patent Citations (4)
| Title |
|---|
| 微波辐照提取油茶果壳棕色素及其稳定性研究;邱贺媛等;《食品科学》;20091231;第30卷(第16期);198-202 * |
| 栀子黄色素的提取及精制研究;陆伟等;《中国调味品》;20091231;第34(总)卷(第11期);84-87 * |
| 邱贺媛等.微波辐照提取油茶果壳棕色素及其稳定性研究.《食品科学》.2009,第30卷(第16期),198-202. |
| 陆伟等.栀子黄色素的提取及精制研究.《中国调味品》.2009,第34(总)卷(第11期),84-87. |
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