CN103113438B - A kind of method from Extracting Hesperidin from Orange Peel and Yellow Pigment in Tangerine Peel - Google Patents
A kind of method from Extracting Hesperidin from Orange Peel and Yellow Pigment in Tangerine Peel Download PDFInfo
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- CN103113438B CN103113438B CN201310036105.8A CN201310036105A CN103113438B CN 103113438 B CN103113438 B CN 103113438B CN 201310036105 A CN201310036105 A CN 201310036105A CN 103113438 B CN103113438 B CN 103113438B
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Abstract
The invention provides a kind of Technology simultaneously extracting Hesperidin and Yellow Pigment in Tangerine Peel from tangerine peel, comprise the steps: dried after dried orange peel through with acid alcohol refluxing extraction, filtration, concentrate, neutralize, refilter, filter residue adds alkali dissolution, neutralization, crystallization obtain hesperidine sterling.Filtrate adds alcohol extraction, obtained Yellow Pigment in Tangerine Peel sterling after concentrate drying.The method is simple to operate, significantly reduces the production cost of Yellow Pigment in Tangerine Peel and hesperidine, simplifies its production process.
Description
Art
Belong to Separation of Natural Products technical field, relate to the comprehensive utilization of the medicinal plants such as a kind of citrus peel, more specifically to a kind of Technology extracting Hesperidin and Yellow Pigment in Tangerine Peel from tangerine peel simultaneously.
Background technology
China's oranges and tangerines resource and output Jun Ju third place in the world, output reaches 1,078 ten thousand tons, and all there is cultivation all parts of the country.Current most of tangerine meat is utilized, and a large amount of tangerine peel all goes out of use, and be otherwise known as Chinese medicine orange peel.Also can enter dish, herbal cuisine with fresh orange peel, the gas of orange peel except the smelling of fish or mutton during cooking, can be added.In orange peel, main component is Hesperidin, and the flavonoid compound coexisted in orange peel with Hesperidin also has neohesperidin, citrus xanthosine, Yellow Pigment in Tangerine Peel, auranetin, also has neutral lactone amaroid vitamin P and volatilization wet goods composition in addition.Taste is worked hard, warm in nature nontoxic, has effect of activating QI to eliminate phlegm, can be used as medicine.These pharmacologically actives give the credit to the composition such as Yellow Pigment in Tangerine Peel, Hesperidin in tangerine peel, and the extractive technique thus studying these two kinds of compositions in tangerine peel is significant.
Yellow Pigment in Tangerine Peel, has another name called Yellow Pigment from Tangerine Peel, peel of Citrus reticulata Blanco pigment, naringin.Orange peel is yellow or orange, is wherein rich in orange-yellow carotenoid.Have now been found 20 multiple types carotene in Pigment of Orange Peel, exist mainly with oxygenatedchemicals, as zeaxanthin diepoxide, yellowish matter, epoxy pearl xanthin, zeaxanthin, corpus luteum etc., the nontoxic and easily collecting of tangerine peel is the fine raw material extracting yellow pigment.Orange peel not only can extract pigment, and can extract volatile oil, pectin, realizes the comprehensive utilization of tangerine peel, is a kind of natural resource of worth exploitation.
Hesperidin, has another name called hesperidine, hesperidin, belongs to natural flavone compounds, and its sterling is white needle-like crystals or pale yellow powder, and bitter is warm in nature, molecular formula C
28h
34o
15molecular weight 610.57, fusing point 258-262 DEG C, be dissolved in cold water hardly, but in ethanol or hot water, there is larger solubleness, dissolve in pyridine, glycerine, acetic acid or dilute alkaline soln, be insoluble in chloroform, acetone, ether or benzene, precipitate with iron trichloride, metallic salt reaction solution or generate, react in red-purple with hydrochloric acid-magnesium powder.
Hesperidin is very extensive in distributed in nature, is mainly present in pulse family, white birch, Labiatae, Papilionaceae, Rutaceae, citrus plant body.The effects such as Hesperidin has good biological activity, has lipid peroxidation inhibition and scavenging activated oxygen, anti-inflammatory, antiviral, antibacterial, strengthens capillary vessel toughness, shortens the bleeding time, and anticancer is active and delay senility.Hesperidin has maintenance osmotic pressure, strengthens capillary vessel toughness, shortens the bleeding time, reduce the effects such as cholesterol, clinically for the assisting therapy of cardiovascular system diseases, can cultivate the multiple medicine preventing arteriosclerosis and myocardial infarction, be one of main raw material of patent medicine " Maitong ".Can be used as natural antioxidants in the food industry.Also can be used for cosmetic industry.Hesperidin major part is present in the waste of citrus processing, as in pericarp, fruit capsule, and the content of Hesperidin the highest (endocarp 30%-50%, in tangerine peel, core, pulp 30%-50%, exocarp 10%-20%) in wherein ripe pericarp and tissue.Content lower 1%-5% in juice and tangerine capsule.
Publication number is that the Chinese patent of CN01106994 discloses a kind of method extracting medicinal raw material synephrine from traditional Chinese medicine citrus aurantium, the method uses the water extraction dried immature fruit of citron orange, extracting solution is through concentrated, alcohol precipitation, recovery ethanol, sand filtration, then cationic resin column is gone up, first rinse by suitable quantity of water, again with certain density ammoniacal liquor wash-out, ammoniacal liquor elutriant is through concentrated direct crystallization, and namely recrystallization obtains synephrine.Present method has the advantages such as operating process is simple, production cost is low.
Publication number is that the Chinese patent of CN102276669A discloses the preparation method extracting hesperidine from the dried immature fruit of citron orange, comprises the following steps: (1) prepares raw material and dried immature fruit of citron orange fine powder is poured in extractor; (2) emptying liquid stirring again after configuration alkaline solution makes immersion treatment to material in tank; (3) configure alkaline solution and thermal treatment is done to material in tank; (4) alkaline solution is configured to emptying liquid stirring again after material work first time percolation treatment in tank; (5) alkaline solution is configured to emptying liquid stirring again after material work second time percolation treatment in tank; (6) pump into extracting solution and extract hesperidine; (7) to isolate hesperidine crystallization; (8) hesperidine crystallization is filtered dry, drying and processing.
Publication number is the method that the Chinese patent of CN102050855A discloses a kind of comprehensive extraction synephrine and hesperidine from immature bitter orange raw material, to overcome the wasting of resources that prior art cannot cause two kinds of product comprehensive exploitations, and optimize extraction step, reduce production cost, promote operability.After raw material pulverizing, alkali organic solvent is adopted to extract; United extraction liquid, is concentrated into proportion 1.05, filters, and filtrate is decoloured; Filtrate is adjusted to neutrality, filters to obtain Hesperidin product, yield 25%, content 95%; Filter the mother liquor obtained and be adjusted to strong basicity, adopt mixed organic solvents extraction, be concentrated into certain volume and add little polar solvent crystallization, product yield is 1.2%, and synephrine content is 98%.Present invention achieves and made full use of by immature bitter orange raw material, design technology produces synephrine and hesperidine two kinds of products simultaneously, greatly reduces production cost; Overall leaching process is optimized more, shortens technical process, saves production cost.
Publication number is that the Chinese patent of CN102526295A discloses a kind of method fully utilizing dried orange peel, by dried orange peel 40 crushed after being dried, adopt the continuous control temperature of Subcritical Water Extraction technology and pressure, according to the descending water-soluble polysaccharide (5MPa, 150-180 DEG C) obtained respectively in dried orange peel of polarity, flavones and phenols (5MPa, 120-140 DEG C), triterpenes (5MPa, 100-110 DEG C) and essential oil (5MPa, 70-90 DEG C) composition, yield is respectively 5.1-7.6%, 0.8-1.5%, 0.4-1.1%, 3.0-3.2%.Essential oil can be used for making essence and flavoring agent, and triterpene, flavones and phenols and water-soluble polysaccharide composition can be used for further separation and purification and obtain pharmaceutically acceptable composition, and after extracting, remaining dregs part can in order to make sweetend roll etc.This invention makes the opposed polarity composition of dried orange peel resource obtain application simultaneously, effectively improves the quality of product and the comprehensive utilization ratio of resource.
Chen Yu reports with 95% ethanol for extraction agent in " extraction of Yellow Pigment from Tangerine Peel and stability " document, and solid-liquid ratio is 1: 8(g/mL), at 60 DEG C, extract 6h, its extraction effect is better, but its pigment content is not high.Yellow Pigment from Tangerine Peel is more stable under acidity and weak basic condition, and common food additive, oxygenant, reductive agent are not obvious to its stability influence, have stronger resistance to oxidation reducing power.
Li Youji report in " Yellow Pigment from Tangerine Peel Study on extraction " document orange peel adopt dehydrated alcohol 65 DEG C, solid-liquid ratio is 1: 8(g/mL), pH is 5.0 times lixiviate 5h, obtain its extracting solution, filter to get filtrate, repeat once, merging filtrate, centrifugal removal of impurities, obtains supernatant liquor, thick yellow pigment is concentrated to obtain again, refining finished product through vacuum-drying.
Jia Changying reports with 70% ethanol for extraction agent in " Extraction Technology of Yellow Pigment from Orange Peel research " document, adopts the solid-liquid ratio of 1: 8 (g/mL), and flood 3 times under the dipping temperature of 50 DEG C, each 5h, needs 15h altogether; Adopt soxhlet extraction, with the Extraction solvent identical with pickling process and solid-liquid ratio, under 95 DEG C of bath temperatures, the 2h that only need reflux just can reach the extraction effect of pickling process, shortens extraction time significantly.Practical problems in its commercial process is not considered in extraction for Yellow Pigment in Tangerine Peel, and high temperature is too large to the demand of energy consumption, and the ethanol of high density is too high to the requirement of extraction equipment, also easily blasts, larger to the risk of pollution of environment.Also have report to adopt microwave extracting to carry out the extraction of Yellow Pigment in Tangerine Peel, but microwave extracting equipment cannot carry out suitability for industrialized production at present.
Yellow Pigment in Tangerine Peel content in dried orange peel is the highest, and Hesperidin also has certain content in dried orange peel, draws materials conveniently, widely distributed, low price.Disclosed documents and materials fail to carry out comprehensive development and utilization to its effective constituent in leaching process at present, and thus carry out comprehensive deep processing to dried orange peel and mean a great, explore extract orange yellow pigment and Hesperidin simultaneously from dried orange peel, its meaning is quite long-range.
Summary of the invention
The technical solution used in the present invention comprises: the dried orange peel after dried through with acid alcohol refluxing extraction, filtration, concentrate, neutralize, refilter, filter residue adds alkali dissolution, neutralization, crystallization obtain hesperidine sterling.Filtrate adds alcohol extraction, obtained Yellow Pigment in Tangerine Peel sterling after concentrate drying.
Therefore, the invention provides a kind of method extracting Yellow Pigment in Tangerine Peel and hesperidine from tangerine peel, step comprises:
(1) pulverize dry dried orange peel, and by dried orange peel, 45% aqueous ethanolic solution by weight (kg)/volume ratio (L)=1:3-5 mix, 40 DEG C of refluxing extraction;
(2), after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to the 1/5-1/8 of original volume;
(3) concentrated solution 0.01mol/L hydrochloric acid soln is regulated about pH to 7, leave standstill more than 5h, once obtain filter residue through ceramic membrane filter.
(4) dissolved by filter residue 0.001mol/LNaOH solution, filter residue and 0.001mol/LNaOH solution is (kg)/volume ratio (L)=1:3-4 by weight;
(5) after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to the 1/5-1/8 of original volume, regulates about pH to 7 with 0.01mol/L aqueous hydrochloric acid, leaves standstill more than 5h, obtains Hesperidin sterling through ceramic membrane filter.
(6) by the filtrate that (3) step obtains, with the extraction into ethyl acetate of 2-3 times of volume, discard ethyl acetate layer, and concentrating under reduced pressure will not be carried out containing ethyl acetate layer at 40 DEG C, until obtain dry thing, be Yellow Pigment in Tangerine Peel sterling.
In one embodiment, 45% aqueous ethanolic solution described in step (1), wherein containing the ethanol of 45%, the aqueous solution of 0.001mol/LNaOH.
Technique effect
1, raw material used in the inventive method, equipment are common common raw material, equipment, avoid the dependence for expensive raw materials, instrument in commercial process, greatly reduce its production cost.
2, mandarin orange planting is easy, and output is high, price is low, convenient sources, and following resource is secure.
3, use dried orange peel as extraction raw material, both substantially increased the utilising efficiency of dried orange peel, and turn improved the added value of dried orange peel.
4, the inventive method is simple to operate, significantly reduces the production cost of Yellow Pigment in Tangerine Peel and hesperidine, simplifies its production process.
5, the reagent that the present invention is used is chemical reagent that is nontoxic, cheap, volume production, ripe reagent can be utilized to reclaim routine techniques, significantly reduce to environmental emission waste in whole process.
Tool stops embodiment
Below, the present invention will be further detailed by embodiment, but it is not limited to any one or similar example of these embodiments.
Embodiment 1
(1) select content of hesperidin in the dried immature fruit of citron orange 5.14%, to take 100kg by below dried immature fruit of citron orange crushed after being dried to 10 order, add 400L containing 0.001mol/LNaOH, 45% the aqueous solution of ethanol mix, 40 DEG C of refluxing extraction; (2), after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 60L; (3) concentrated solution 0.01mol/L hydrochloric acid soln is regulated about pH to 7, leave standstill more than 5h, once obtain filter residue 13.4kg through ceramic membrane filter; (4) NaOH solution of the 0.001mol/L of filter residue 35L is dissolved; (5) after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 6L, regulates about pH to 7 with 0.01mol/L aqueous hydrochloric acid, leaves standstill more than 5h, obtains hesperidine sterling 3.85kg through ceramic membrane filter; (6) by the filtrate that (3) step obtains, with the extraction into ethyl acetate of 3 times of volumes, discard ethyl acetate layer, and concentrating under reduced pressure will not be carried out containing ethyl acetate layer at 40 DEG C, until obtain dry thing, be Yellow Pigment in Tangerine Peel sterling 2.45kg.Test set is Agilent1100 high performance liquid chromatograph, chromatographic column is HypersilODS (250mm × 4.6mm, 5 μ), the testing conditions of hesperidine: moving phase is water: acetonitrile: acetic acid solution (80:16:4, V/V), determined wavelength are 280nm, flow velocity is lml/min, sample size is 20 μ L; The spectrophotometry colorimetric detection condition of Yellow Pigment in Tangerine Peel: solubilising reagent is ethanol, determined wavelength is 370nm.The purity of hesperidine sample is 95.54%, the purity of Yellow Pigment in Tangerine Peel sample is 97.25%.
Embodiment 2
(1) select content of hesperidin in the dried immature fruit of citron orange 5.14%, to take 200kg by below dried immature fruit of citron orange crushed after being dried to 10 order, add 800L containing 0.001mol/LNaOH, 45% the aqueous solution of ethanol mix, 40 DEG C of refluxing extraction; (2), after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 100L; (3) concentrated solution 0.01mol/L hydrochloric acid soln is regulated about pH to 7, leave standstill more than 5h, once obtain filter residue 28.1kg through ceramic membrane filter; (4) NaOH solution of the 0.001mol/L of filter residue 60L is dissolved; (5) after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 13L, regulates about pH to 7 with 0.01mol/L aqueous hydrochloric acid, leaves standstill more than 5h, obtains hesperidine sterling 7.87kg through ceramic membrane filter; (6) by the filtrate that (3) step obtains, with the extraction into ethyl acetate of 2.5 times of volumes, discard ethyl acetate layer, and concentrating under reduced pressure will not be carried out containing ethyl acetate layer at 40 DEG C, until obtain dry thing, be Yellow Pigment in Tangerine Peel sterling 4.96kg.Carry out detection hesperidine and Yellow Pigment in Tangerine Peel sample by the detection method of embodiment 1, the purity of hesperidine sample is 96.25%, the purity of Yellow Pigment in Tangerine Peel sample is 97.62%.
Embodiment 3
(1) select content of hesperidin in the dried immature fruit of citron orange 5.14%, to take 400kg by below dried immature fruit of citron orange crushed after being dried to 10 order, add 1400L containing 0.001mol/LNaOH, 45% the aqueous solution of ethanol mix, 40 DEG C of refluxing extraction; (2), after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 200L; (3) concentrated solution 0.01mol/L hydrochloric acid soln is regulated about pH to 7, leave standstill more than 5h, once obtain filter residue 54.5kg through ceramic membrane filter; (4) NaOH solution of the 0.001mol/L of filter residue 120L is dissolved; (5) after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to 20L, regulates about pH to 7 with 0.01mol/L aqueous hydrochloric acid, leaves standstill more than 5h, obtains hesperidine sterling 15.78kg through ceramic membrane filter; (6) by the filtrate that (3) step obtains, with the extraction into ethyl acetate of 3 times of volumes, discard ethyl acetate layer, and concentrating under reduced pressure will not be carried out containing ethyl acetate layer at 40 DEG C, until obtain dry thing, be Yellow Pigment in Tangerine Peel sterling 9.94kg.Carry out detection hesperidine and Yellow Pigment in Tangerine Peel sample by the detection method of embodiment 1, the purity of hesperidine sample is 98.36%, the purity of Yellow Pigment in Tangerine Peel sample is 97.29%.
Claims (2)
1. extract a method for Yellow Pigment in Tangerine Peel and hesperidine from tangerine peel, step comprises:
(1) dry dried orange peel is pulverized, and by dried orange peel, 45% aqueous ethanolic solution by weight/volume ratio=1:3-5 mixes, 40 DEG C of refluxing extraction, wherein the weight of dried orange peel is in units of kg, the volume of 45% aqueous ethanolic solution is in units of L, and 45% aqueous ethanolic solution refers to containing the ethanol of 45%, the aqueous solution of 0.001mol/LNaOH;
(2), after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to the 1/5-1/8 of original volume;
(3) concentrated solution 0.01mol/L hydrochloric acid soln is regulated about pH to 7, leave standstill more than 5h, once obtain filter residue through ceramic membrane filter;
(4) filter residue 0.001mol/LNaOH solution is dissolved, filter residue and 0.001mol/LNaOH solution by weight/volume ratio=1:3-4, the weight of filter residue thinks kg unit, and the volume of 0.001mol/LNaOH solution is in units of L;
(5) after ceramic membrane filter once removes the gred, filtrate carrying out is evaporated to the 1/5-1/8 of original volume, regulates about pH to 7 with 0.01mol/L aqueous hydrochloric acid, leaves standstill more than 5h, obtains Hesperidin sterling through ceramic membrane filter;
(6) by the filtrate that (3) step obtains, with the extraction into ethyl acetate of 2-3 times of volume, discard ethyl acetate layer, and concentrating under reduced pressure will not be carried out containing ethyl acetate layer at 40 DEG C, until obtain dry thing, be Yellow Pigment in Tangerine Peel sterling.
2. method according to claim 1, filters described in step (2), (3), (5), refers to the ceramic membrane filter of employing 0.2 μm of pore size once.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103483403B (en) * | 2013-09-24 | 2016-03-09 | 重庆主流生物工程有限公司 | A kind of circulation extracting method of hesperidine of purifying from tangerine slag |
| CN104403357A (en) * | 2014-10-29 | 2015-03-11 | 宁波广源纺织品有限公司 | Orange peel vegetable dye extraction method |
| CN104402952B (en) * | 2014-12-15 | 2017-09-12 | 承德天原药业股份有限公司 | A kind of method that mandarin oil and aurantiamarin are extracted in orange peel |
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| WO2000032062A1 (en) * | 1998-12-02 | 2000-06-08 | Adumim Chemicals Ltd. | A method for selectively obtaining antioxidant rich extracts from citrus fruits |
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| CN101747394A (en) * | 2009-12-31 | 2010-06-23 | 浙江工业大学 | Method for extracting hesperidin from tangerine peel |
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2013
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Patent Citations (7)
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| US4150038A (en) * | 1977-05-16 | 1979-04-17 | Dynapol | Conversion of hesperidin into hesperetin |
| WO2000032062A1 (en) * | 1998-12-02 | 2000-06-08 | Adumim Chemicals Ltd. | A method for selectively obtaining antioxidant rich extracts from citrus fruits |
| EP1157701A1 (en) * | 1999-12-23 | 2001-11-28 | ASAC Compania de Biotecnologia E Investigacion, S.A. | Method for obtaining olive leaf extracts and applications thereof |
| CN101265283A (en) * | 2008-04-22 | 2008-09-17 | 复旦大学 | Method for extracting hesperidin and naringin |
| CN101643489A (en) * | 2009-05-26 | 2010-02-10 | 苏州派腾生物医药科技有限公司 | Process for preparing hesperidin |
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