CN1340574A - Process for extracting yellow pigment from leftover of ginkgone - Google Patents
Process for extracting yellow pigment from leftover of ginkgone Download PDFInfo
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- CN1340574A CN1340574A CN 00126930 CN00126930A CN1340574A CN 1340574 A CN1340574 A CN 1340574A CN 00126930 CN00126930 CN 00126930 CN 00126930 A CN00126930 A CN 00126930A CN 1340574 A CN1340574 A CN 1340574A
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Abstract
A process for extracting yellow pigment from the leftover of ginkgone includes such steps as using petroleum ether to extract cytochrome from the said leftover; adding the alcohol solution of sodium hydroxide to the petroleum ether solution of cytochrome, saponifying chlorophyll, separating the alcohol solution of chlorophyll, concentrating the petroleum solution to semi-fluid state, separating out other components, purifying yellow pigment; and concentrating and baking.
Description
This invention relates to extract the method for natural yellow pigment, specifically, is the method for separation and Extraction natural yellow pigment from the bilobanone tankage.
The extraction of natural yellow pigment, known some from the leaf of bamboo, extract, some is from Orange Peel.For example:
1, Forestry Science Inst., Jiangxi Prov. applies for a patent, and publication number is CN1063704A.
Method: (1) raw material is prepared: the leaf of bamboo is removed the leaf that goes rotten, go into pulverizer and pulverize standby.
(2) extract: get and pulverize about 1 kilogram of the leaf of bamboo, add 90% ethanol, add-on is with submergence leaf of bamboo degree of being, in the following immersion of 50～60 ℃ of conditions, stir on the limit, extracted 8 hours, filters, get ethanolic soln, filter residue is used extraction using alcohol twice again as above-mentioned condition, collect three filtrates and combine.
(3) concentrate: above-mentioned filtrate is placed vacuum concentrator,, be condensed under 600 * 133.322 MPa pressure and contain solid and account for 30% concentrated solution in 70 ℃.
(4) separate: add in the extraction using alcohol concentrated solution after 1.5 times ether (or gasoline) stirs, add 100 ml waters, standing demix is emitted ethanol liquid that lower floor contains xenthophylls to critical surface, stays upper strata chlorophyll diethyl ether solution.
(5) separate for the second time: in the chlorophyll diethyl ether solution of upper strata, add 150 milliliters of ethanolic solns that contain 8%NaOH, stir half an hour after, standing demix again, the upper strata is the ether solution that contains carotene, lower floor washs 3～4 times with ether or gasoline for containing chlorophyllous ethanol liquid, to remove impurity.
(6) put copper: use in the hydrochloric acid and chlorophyl liquid, make PH to 7, add copper sulfate 40 grams, transfer PH to 2～3 with hydrochloric acid again, be heated to 60～70 ℃, stir half an hour, get Chlorophyll Cu liquid.
(7) put calcium: the aqua calcis of adding 10% in above-mentioned liquid, transfer PH to 11, be heated to 70 ℃, cooling is filtered, and precipitation washes with water 5 times, and the hydrochloric acid of adding 3% makes PH to 2～3 in precipitation.
(8) salify: use washing with alcohol dissolution precipitation 3 times, add 10% calcium hydroxide, regulate PH to 11, filter, wash 2～3 times, and merging filtrate.
(9) drying: filtrate is placed moisture eliminator, is heated to 60～80 ℃, vacuum-drying 4 hours, pulverize sodium copper chlorophyllin powdery finished product, its yield can reach 0.6% (i.e. 6 grams).
This method separates to get the xenthophylls crude product for the first time when sodium copper chlorophyllin is made in extraction, can get the carotene crude product for the second time.100596.7
2, Lee of Anshun, Anshun City, Guizhou Province teachers training school has the open patent of invention of firm application, and publication number is CN1075729A.
Method: (1) orange peel pre-treatment and pulverizing: orange peel is selected, removes foreign material such as green pericarp, stone sand, mud, and again with the clear water wash clean of sterilizing, 60～70 ℃ of oven dry down, the granularity that is ground into 1～3mm is used again.
(2) lixiviate: get boiling range and be 60～90 ℃ sherwood oil, press sherwood oil: the deal of raw material=3.5: 1 is mixed, lixiviate under agitation 1 hour, and extraction temperature is a normal temperature, this operation can repeat lixiviate 4～5 times.
(3) filter: the raw material of above-mentioned extracted filtrate, filter residue being made to extract pectin.
(4) concentrate: the filtering filtrate of lixiviate is several times merged, and is 0.04～0.05 MPa in vacuum tightness, and temperature is to carry out concentrating under reduced pressure under 40～60 ℃ of conditions, and remakes solvent when reclaiming following batch of raw material lixiviate of sherwood oil confession and be used.
(5) distillation: above-mentioned gained enriched material is obtained aqueous tangerine oil through steam distillation again,, collect tangerine oil, discard water with the profit standing demix.
(6) sherwood oil is refining: is to concentrate under 0.04～0.05 MPa, 38～70 ℃ of temperature condition with 6 times of pigment materials to above-mentioned distillation residue thing in vacuum tightness, reclaim whole petroleum ether solvents, the paste of natural yellow pigment, if need solid phase prod, spray-dried again and get.
The enrichment of bilobanone tankage the cytopigment of Ginkgo Leaf, i.e. carotenoid and chlorophyll.The present invention seeks to refuse to be reused for the above natural pigment of separation and Extraction from the bilobanone tankage.
The method that yellow pigment from leftover of ginkgone extracts:
(1) extraction: get a certain amount of bilobanone tankage, add its 1.5 times of (volume) boiling ranges and be 60～90 ℃ sherwood oil, stir, leave standstill 4 hours after, leach upper solution, filter.Add same volume sherwood oil re-extract once to precipitation again, filter.Merge filtrate twice.Filter residue can be used as the main raw material of preparing biological pesticide.
(2) separate: chlorophyll content in the sampling check sherwood oil filtered liquid by the ratio of chlorophyll and solid caustic soda is
Add solid caustic soda at 1: 1.2, and add 32 times ethanol, the limit edged stirs when adding alkali, after saponification half an hour, leaves standstill 10 minutes, and telling lower floor's ethanolic soln is exactly the saponification chlorophyl liquid.Can produce the sodium copper chlorophyllin marennin.Remaining is the yellow pigment petroleum ether solution.
(3) concentrate: the yellow pigment petroleum ether solution in vaporizer, under 60～90 ℃ of temperature, is condensed into the semi-fluid shape, and reclaims sherwood oil.
(4) separate for the second time: in semi-fluid shape concentrated solution, add 95% ethanol of 4 times of volumes, fully stir, leave standstill 1.5 hours after.Leach filtration.Use twice of same volume 95% ethanol repeated isolation again.Merge three filtrate and filter residue.
(5) concentrate drying: above-mentioned filtrate is placed vacuum concentrator,, be condensed into paste carotenoid under 600 * 133.322 handkerchief pressure, need concentrate the back spraying drying if get dry powder in 70 ℃.
If need further separation and Extraction carotene, can in paste carotenoid, add 95% ethanol, fully stirring and dissolving, leaving standstill 1 hour, and leached filtration, is carotene after precipitation and the filter residue and drying, be carotenoid behind the filtrate concentrate drying, separating for several times can get carotene and xenthophylls.
(6) separate for the third time: isolating precipitation and filter residue add the sherwood oil (boiling range is 60～90 ℃) of 4 times of volumes for the second time, stir, and it is fully dissolved, and leave standstill 1 hour, leach filtration, extract once with same volume sherwood oil repeated isolation again.Merge filtrate twice.
(7) concentrate: in vaporizer, filtrate is condensed into the semi-fluid shape and reclaims sherwood oil at 80～90 ℃.
(8) washing: in above-mentioned semi-fluid shape concentrated solution, add 2 times of volume 95% ethanol, stirred 20 minutes, leave standstill half an hour, leach filtration.
(9) concentrate oven dry: with above-mentioned precipitation and filter residue, in baker, under 80～90 ℃ of temperature, dry, carotene, with above-mentioned filtrate in vacuum concentrator in 70 ℃, 600 * 133.322 handkerchief pressure are condensed into paste carotenoid and reclaim ethanol.
This invention positively effect is:
1, remove environmental pollution: bilobanone tankage black glues paste, and without putrefaction is difficult for being decomposed, serious environment pollution.The present invention all utilizes each composition of bilobanone tankage, has removed environmental pollution.
2, comprehensive utilization of waste materials: can separation and Extraction (coproduction) carotenoid from the bilobanone tankage, carotene, sodium copper chlorophyllin.More than three kinds of pigments be nontoxic natural colorant, can be used for aspects such as food, beverage, medicine.Slag after the extraction can also be prepared biological pesticide.
3, separable extraction carotenoid 15% from the bilobanone tankage, carotene 0.8%, sodium copper chlorophyllin 1%.The extraction yield of sodium copper chlorophyllin is 1.67 times of leaf of bamboo extraction yield.The extraction yield of carotenoid and carotene is also very high, and is elaboration.
4, the present invention has saved raw material processing and leaching process, so can save solvent.
The present invention will be illustrated by embodiment and accompanying drawing.Accompanying drawing is represented the skeleton diagram of yellow pigment from leftover of ginkgone extracting method of the present invention.
Example is as follows:
1, extraction: get 1 kilogram of bilobanone tankage, add its 1.5 times of (volume) boiling ranges and be 60～90 ℃ sherwood oil, stir, leave standstill 4 hours after, leach upper solution, filter.Add same volume sherwood oil re-extract once to precipitation again, filter.Merge filtrate twice.Filter residue can be used as the main raw material of preparing biological pesticide.
2, separate: chlorophyll content in the sampling check sherwood oil filtered liquid by the ratio of chlorophyll and solid caustic soda is
Add solid caustic soda at 1: 1.2, and add 32 times ethanol, the limit edged stirs when adding alkali, after saponification half an hour, leaves standstill 10 minutes, and telling lower floor's ethanolic soln is exactly the saponification chlorophyl liquid.Can produce the sodium copper chlorophyllin marennin.
3, concentrate: petroleum ether solution in vaporizer, under 60～90 ℃ of temperature, is condensed into the semi-fluid shape, and reclaims sherwood oil.
4, separate for the second time: in semi-fluid shape concentrated solution, add 95% ethanol of 4 times of volumes, fully stir, leave standstill 1.5 hours after, leach filtration, use twice of same volume 95% ethanol repeated isolation again.Merge three filtrate and filter residue.
5, concentrate drying: above-mentioned filtrate is placed vacuum concentrator,, be condensed into paste carotenoid under 600 * 133.322 MPa pressure, promptly get carotenoid 150 grams in 70 ℃.Need concentrate the back spraying drying if get dry powder.
6, separate for the third time: isolating precipitation and filter residue add the sherwood oil (boiling range is 60～90 ℃) of 4 times of volumes for the second time, stir, and it is fully dissolved, and leave standstill 1 hour, leach filtration, extract once with same volume sherwood oil repeated isolation again.Merge filtrate twice.
7, concentrate: in vaporizer, filtrate is condensed into the semi-fluid shape and reclaims sherwood oil at 80～90 ℃.
8, washing: in above-mentioned semi-fluid shape concentrated solution, add 2 times of volume 95% ethanol, stirred 20 minutes, leave standstill half an hour, leach filtration.
9, concentrate oven dry: with above-mentioned precipitation and filter residue, in baker, under 80～90 ℃ of temperature, dry, get carotene 8 grams, with above-mentioned filtrate in vacuum concentrator in 70 ℃, 600 * 133.322 handkerchief pressure are condensed into paste carotenoid 3 gram and reclaim ethanol.
Claims (3)
1, the method for yellow pigment from leftover of ginkgone extraction:
(1) extraction: get a certain amount of bilobanone tankage, add its 1.5 times of (volume) boiling ranges and be 60～90 ℃ sherwood oil, stir, leave standstill 4 hours after, leach upper solution, filter.Add same volume sherwood oil re-extract once to precipitation again, filter.Merge filtrate twice.Filter residue can be used as the main raw material of preparing biological pesticide.
(2) separate: chlorophyll content in the sampling check sherwood oil filtered liquid by the ratio of chlorophyll and solid caustic soda is
Add solid caustic soda at 1: 1.2, and add 32 times ethanol, the limit edged stirs when adding alkali, after saponification half an hour, leaves standstill 10 minutes, and telling lower floor's ethanolic soln is exactly the saponification chlorophyl liquid.Can produce the sodium copper chlorophyllin marennin.
(3) concentrate: petroleum ether solution in vaporizer, under 60～90 ℃ of temperature, is condensed into the semi-fluid shape, and reclaims sherwood oil.
(4) separate for the second time: in semi-fluid shape concentrated solution, add 95% ethanol of 4 times of volumes, fully stir, leave standstill 1.5 hours after, leach filtration, use twice of same volume 95% ethanol repeated isolation again.Merge three filtrate and filter residue.
(5) concentrate drying: above-mentioned filtrate is placed vacuum concentrator,, be condensed into paste carotenoid under 600 * 133.322 handkerchief pressure, need concentrate the back spraying drying if get dry powder in 70 ℃.
(6) separate for the third time: isolating precipitation and filter residue add the sherwood oil (boiling range is 60～90 ℃) of 4 times of volumes for the second time, stir, and it is fully dissolved, and leave standstill 1 hour, leach filtration, extract once with same volume sherwood oil repeated isolation again.Merge filtrate twice.
(7) concentrate: in vaporizer, filtrate is condensed into the semi-fluid shape and reclaims sherwood oil at 80～90 ℃.
(8) washing: in above-mentioned semi-fluid shape concentrated solution, add 2 times of volume 95% ethanol, stirred 20 minutes, leave standstill half an hour, leach filtration.
(9) concentrate oven dry: with above-mentioned precipitation and filter residue, in baker, under 80～90 ℃ of temperature, dry, carotene, with above-mentioned filtrate in vacuum concentrator in 70 ℃, 600 * 133.322 handkerchief pressure are condensed into paste carotenoid and reclaim ethanol.
2, according to the extracting method of claim 1 yellow pigment from leftover of ginkgone, yellow pigment is to extract with Ginkgo Leaf that isolated mixture is a raw material in bilobanone (flavonoid compound) process, separation is purified, and is the method that raw material extracts yellow pigment so the present invention also is suitable for the Ginkgo Leaf.
3, according to claim 1, the bilobanone tankage are to produce isolated mixture in the bilobanone process, so the present invention also is suitable for when producing bilobanone the method for producing yellow pigment simultaneously.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 00126930 CN1340574A (en) | 2000-09-03 | 2000-09-03 | Process for extracting yellow pigment from leftover of ginkgone |
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| CN 00126930 CN1340574A (en) | 2000-09-03 | 2000-09-03 | Process for extracting yellow pigment from leftover of ginkgone |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341332A (en) * | 2014-10-24 | 2015-02-11 | 湖北诺克特药业有限公司 | Method for extracting carotenoid from waste oil sludge of ginkgo leaf extraction process |
| CN104725387A (en) * | 2015-02-05 | 2015-06-24 | 浙江得乐康食品股份有限公司 | Preparation method for preparing sodium copper chlorophyllin from gingko leaves |
| CN110200021A (en) * | 2019-07-23 | 2019-09-06 | 江苏贝斯康药业有限公司 | A kind of preparation method of ginkgo biloba leaf total organic salt |
-
2000
- 2000-09-03 CN CN 00126930 patent/CN1340574A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341332A (en) * | 2014-10-24 | 2015-02-11 | 湖北诺克特药业有限公司 | Method for extracting carotenoid from waste oil sludge of ginkgo leaf extraction process |
| CN104341332B (en) * | 2014-10-24 | 2016-08-24 | 湖北诺克特药业股份有限公司 | A kind of method extracting carotenoid from ginkgo leaf extraction process waste oil sludge |
| CN104725387A (en) * | 2015-02-05 | 2015-06-24 | 浙江得乐康食品股份有限公司 | Preparation method for preparing sodium copper chlorophyllin from gingko leaves |
| CN110200021A (en) * | 2019-07-23 | 2019-09-06 | 江苏贝斯康药业有限公司 | A kind of preparation method of ginkgo biloba leaf total organic salt |
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