CN104402952A - Method for extracting mandarin oil and hesperidin from orange peel - Google Patents
Method for extracting mandarin oil and hesperidin from orange peel Download PDFInfo
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- CN104402952A CN104402952A CN201410770252.2A CN201410770252A CN104402952A CN 104402952 A CN104402952 A CN 104402952A CN 201410770252 A CN201410770252 A CN 201410770252A CN 104402952 A CN104402952 A CN 104402952A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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Abstract
The invention relates to a method for extracting mandarin oil and hesperidin from orange peel and belongs to the technical field of plant extracts. The method for extracting the mandarin oil and the hesperidin from the orange peel comprises the following steps: rolling the orange peel to obtain flake orange peel; extracting the flake orange peel by a mixed solvent of an vegetable oil extracting solvent and ethyl alcohol, adding water into an extraction solution to separate and obtain an ethyl alcohol-water layer and a vegetable oil extracting solvent layer; concentrating the vegetable oil extracting solvent, and removing solvent residues to obtain mandarin oil; concentrating the ethyl alcohol-water layer, carrying out acid precipitation and filtering to obtain a hesperidin wet crystal, and drying the hesperidin wet crystal to obtain a hesperidin product. By virtue of the method for extracting mandarin oil and hesperidin from orange peel, the orange peel is rolled, so that the loss of the mandarin oil fragrance is effectively avoided; the mandarin oil and the hesperidin are extracted by the mixed solvent; the content of the extracted effective components is greater than 90%; the hesperidin is few in impurities; the purity of the hesperidin can reach over 90%; the yield of the hesperidin can reach over 95%; the dried raw material has no influence on the content of the pectin and the production of the pectin; the raw material can be fully used.
Description
Technical field
The present invention relates to plant milk extract technical field, be specifically related to a kind of method extracting mandarin oil and Hesperidin in peel of Citrus reticulata Blanco.
Background technology
Orange peel accounts for the 40-50% of whole fruit weight in wet base, and Chinese output peel of Citrus reticulata Blanco about reached 3,000 ten thousand tons in recent years, and year, Citrus procession amount was at about 2,000,000 tons, can produce the oranges and tangerines wet pelt of about 1,000,000 tons every year.Peel of Citrus reticulata Blanco is a kind of new Biological resources abroad, is not yet fully utilized, causes the great wasting of resources, cause pollution simultaneously to environment in China.If this resource is fully utilized, will turn waste into wealth, not only can extend the industrial chain of China's Citrus Industry, more greatly can improve the economic benefit of Citrus Industry.Peel of Citrus reticulata Blanco, except containing except moisture, Mierocrystalline cellulose, xylogen, also contains abundant pigment, pectin, Hesperidin, mandarin oil etc.Therefore, one of the main path that utilizes of peel of Citrus reticulata Blanco around its ingredient extraction and launch, as therefrom extracted pigment, pectin, Hesperidin, mandarin oil, food fibre.
In recent years, the report extracting the higher material of economic worth from peel of Citrus reticulata Blanco was a lot, but ubiquity extraction benefit is not high, and research shortage considers, and has extracted product often and can not get benefit.The domestic people of having utilizes peel of Citrus reticulata Blanco to produce pectin, extracts natural yellow pigment, Hesperidin etc., but due to products production unicity, the backwardness of Technology, economic benefit is not high, adds purchase and the storing technology problem of peel of Citrus reticulata Blanco, causes peel of Citrus reticulata Blanco not utilized very well for a long time.Except the peel of Citrus reticulata Blanco of China is used as medicine except volatile oil processed and as Chinese medicine, most of peel of Citrus reticulata Blanco is by fertile as feed or fermentation to produce biological, and major part is outwelled even in vain.
Mandarin oil is present in orange or the tiny gland of peel of Citrus reticulata Blanco, is the significant by-products in orange or Citrus procession.Be widely used in the production of seasonings, beverage, food, makeup, soap, pharmaceutical products, sterilant and freshener.About the report of mandarin oil physiological action gets more and more, mandarin oil can be more widely used.
Hesperidin belongs to flavanone sugar aminoglycoside, has and maintains blood vessel normal osmotic pressure, and reduce vascular fragility, shorten the effects such as bleeding time, the medicine effect of Hesperidin has been widely recognized.Hesperidin extracting method and technology have solvent extraction process, alkali to soak acid-precipitation method, ion exchange method, ultrafiltration process, ultrasonic technology, membrane separation technique, supercritical extraction technique, high-speed countercurrent chromatography.
Prior art discloses the method for multiple extraction volatile oil or Hesperidin, such as steam distillation and milling process extract orange peel essential oil, and its extraction yield is generally at about 1.5-3.5%.But there is more defect: steam distillation is higher due to service temperature, can cause the thermolysis of thermographic compound in essential oil and the hydrolysis of facile hydrolysis composition, thermal treatment also can cause the loss of essential oil fragrance; Milling process products obtained therefrom is impure, may have moisture, chlorophyll, mucus etc., is difficult to essential oil completely to squeeze out simultaneously.Therefore how to make full use of this abundant cheap resource of orange peel, have positive meaning.
CN1075729 discloses a kind of method extracting natural yellow pigment, mandarin oil and pectin from peel of Citrus reticulata Blanco.The method long flow path, needs to use industrial chemicals sherwood oil in leaching process, because sherwood oil consumption is large, volatile, cause solvent loss in production process very large, economic benefit is not high.
CN201210310088.8 discloses a kind of method extracting Hesperidin from orange peel, wherein refer to the extracting method of mandarin oil, Hesperidin; Technical process is longer, and step by step arithmetic mandarin oil, pectin, Hesperidin, step by step arithmetic is comparatively large on subsequent step impact, and the soda acid used in production process is more, and the product purities such as the pectin obtained, Hesperidin are lower.And pericarp absorbs and residual organic solvent in a large number, brings inconvenience to follow-up pectin extraction.
Relevant scholar, have studied the improvement of extracting Obtaining Perfume Essential Oil from peel of Citrus reticulata Blanco, in September, 2004, disclose a kind of method extracting volatile oil from orange peel, equally, essential oil, pigment, pectin and Hesperidin article in the combined extracting orange peel delivered in magazine " biomass chemical engineering ", in January, 2007, a kind of Technology extracting essential oil, pigment, pectin, Hesperidin from orange peel continuously announced, above-mentioned document improves multiple step; But its insufficient fragrance, the low yield of mandarin oil and Hesperidin, Hesperidin impurity is more, and complex process is not suitable for the defects such as large-scale industrial production.
The anxious one to be needed of prior art can effectively extract Hesperidin and mandarin oil, and product output efficiency height is applicable to the processing technology of technique simple possible.
Summary of the invention
The present invention is directed to the defect of prior art, provide a kind of method extracting mandarin oil and Hesperidin in peel of Citrus reticulata Blanco, the method obtains mandarin oil and Hesperidin two kinds of products simultaneously, and production efficiency is high, and in product, active constituent content is high, and yield is high, is applicable to suitability for industrialized production.
The object of the present invention is to provide a kind of method extracting mandarin oil and Hesperidin in peel of Citrus reticulata Blanco, concrete grammar is: peel of Citrus reticulata Blanco is carried out roll sheet and obtain sheet peel of Citrus reticulata Blanco; Extract sheet peel of Citrus reticulata Blanco with the mixed solvent of vegetable oil extraction solvent and ethanol, extracting solution adds water separation, obtains alcohol-water layer and vegetable oil extraction solvent layer; Vegetable oil extraction solvent layer is concentrated, remove molten residual after, obtain mandarin oil; Concentrated by alcohol-water layer, acid is heavy, filter and obtain Hesperidin and to wet crystal, Hesperidin crystal drying of wetting obtains Hesperidin product.
In the present invention, before described peel of Citrus reticulata Blanco rolls sheet, moisture is 8-13wt%; Described to roll the thickness that sheet obtains sheet peel of Citrus reticulata Blanco be 0.1-0.5mm, and sheet peel of Citrus reticulata Blanco 20 mesh sieve percent of pass is less than 12%.
In the present invention, the ethanol-water solution of described ethanol to be volume fraction be 90-95%, in described mixed solvent, the volume ratio of vegetable oil extraction solvent and 90-95% ethanol is 1:2.5-3.5.
In the present invention, described Extracting temperature is 45-55 DEG C; The feed liquid mass volume ratio of described extraction is 1:4-6, and described mass unit is kilogram, and described volume unit is for rising; Stirring velocity is 60-200r/min; Extract 3-5 time, often all over extracting 1-2 hour.
In the present invention, the described acid condition of sinking is: pH value is 4.5-5.5; Settling time is 24-48 hour.
In the present invention, described extracting solution adds water in sepn process, and the volume ratio of extracting solution and water is 1:0.5-1, is separated after stratification.
In the present invention, described alcohol-water layer employing vacuum concentration condition is: vapor pressure is 0.085-0.095MPa, and gas phase temperature is 63-67 DEG C, vacuum tightness 0.09-0.095MPa.
In the present invention, the described Hesperidin crystal drying conditions that wets is: vacuum tightness is 0.09 ± 0.001MPa, temperature 60-70 DEG C.
In the present invention, the feed liquid of described extraction uses 100 mesh filter screens to filter, and filter residue disk dryer carries out drying, and dried material pulp water sub-control is built in 6-12wt%.
Percentage composition described in the present invention if no special instructions, all refers to mass percentage.
The detection method of mandarin oil of the present invention is the mensuration of volatile oil content " in People's Republic of China (PRC) agricultural industry criteria NY/T 2013-2011 citrus fruit and the goods "; Hesperidin detection method is the mensuration of Hesperidin, naringin content " in People's Republic of China (PRC) agricultural industry criteria NY/T 2014-2011 citrus fruit and the goods ".
Beneficial effect of the present invention is: 1, roll sheet to peel of Citrus reticulata Blanco, both obtain cytoclasis, be applicable to the sheet-shaped material of extraction, effectively avoid again the loss of mandarin oil fragrance, and adopt mixed solvent to extract, can ensure that extracting effective components content yield is more than 90%, thus subsequent purification technique can be simplified.
2, present method rolls blade technolgy, can abundant smudge cells, suitable fines content can be controlled again, impurity is extracted than powder few, higher than block stock extraction yield during soak extraction, superior product quality, the content that cannot extract can be controlled within 5%, ensure that overall high yield pulp1 and high production efficiency.
3, present method adopts vegetable oil extraction solvent and the mixed solvent of 90-95% ethanol contend than 1:2.5-1:3.5, and decrease the stripping of water-soluble impurity in peel of Citrus reticulata Blanco, Hesperidin impurity is less, and high purity more than 90%, yield reaches more than 95%.
4, dried raw material, does not affect the content of pectin and the production of pectin, achieves the sufficient utilization of raw material.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1:
Take 100kg peel of Citrus reticulata Blanco raw material, in raw material, mandarin oil content is 1.2%, and content of hesperidin is 4.7%.Peel of Citrus reticulata Blanco moisture is kept to be 10wt%, adopt pair roller flaking machine to roll sheet; Rolling the sheet peel of Citrus reticulata Blanco thickness that sheet obtains is 0.25mm, fines content be 7.8%(and granularity be less than that 20 orders account for gross weight 7.8%).
According to vegetable oil extraction solvent: 90% ethanol=1:2.5(volume ratio) mixed preparing mixed solvent, sheet peel of Citrus reticulata Blanco is extracted with this mixed solvent, solid-liquid ratio is 1:4(kg/L), extraction temperature 47 DEG C, stirring velocity 60r/min, extract 5 times, the time is respectively 2 times 2 hours, 2 times 1.5 hours, 1 time 1 hour, obtains mixed solvent extracting solution; It is 6.9wt% that wet feed slag obtains moisture after super-dry, and the siccative slag of dissolvent residual 420ppm is used for pectin production.
According to 1:1(volume in mixed solvent extracting solution) ratio add water, stratification, be separated obtain alcohol-water layer and vegetable oil extraction solvent layer, the Residual oil of alcohol layer controls below 0.1%.Described vegetable oil extraction solvent layer filters, concentrated, desolvation residual after obtain 1.18kg mandarin oil.
Alcohol-water layer is 0.09MPa at vapor pressure, gas phase temperature is 65 DEG C, concentrated under vacuum tightness 0.09MPa condition, obtains concentrated solution, concentrated solution uses hydrochloric acid adjust pH 5.0, leaving standstill 24 hours, filter and obtain wet crystal, is 0.09 ± 0.001MPa in vacuum tightness afterwards, vacuum-drying under temperature 65 DEG C of conditions, product drying obtained, carry out mechanical disintegration to 80 ~ 120 orders, obtains the Hesperidin powder-product 4.8kg that content is 93.5%.
Embodiment 2:
Take 100kg peel of Citrus reticulata Blanco raw material, in raw material, mandarin oil content is 1.2%, and content of hesperidin is 4.7%; Keep peel of Citrus reticulata Blanco moisture to be 8 wt %, adopt pair roller flaking machine to roll sheet; Roll sheet peel of Citrus reticulata Blanco thickness that sheet obtains at 0.4mm, fines content be 5.5%(and granularity be less than that 20 orders account for gross weight 5.5%).
According to vegetable oil extraction solvent: 93% ethanol=1:3(volume) mixed preparing mixed solvent, sheet peel of Citrus reticulata Blanco is extracted with this mixed solvent, solid-liquid ratio is 1:5(kg/l), extraction temperature 50 DEG C, stirring velocity 120r/min, extract 4 times, the time is respectively 2 times 2 hours, 2 times 1.5 hours, obtains mixed solvent extracting solution; It is that the siccative slag of 7.5 wt %, dissolvent residual 500ppm is for pectin production that wet feed slag obtains moisture after super-dry.
According to 1:0.8(volume in mixed solvent extracting solution) ratio add water, stratification, be separated obtain alcohol-water layer and vegetable oil extraction solvent layer, the Residual oil of alcohol layer controls below 0.1%.Described vegetable oil extraction solvent layer filters, concentrated, desolvation residual after obtain 1.17kg mandarin oil.
Alcohol-water layer is 0.09MPa at vapor pressure, gas phase temperature is 63 DEG C, concentrated under vacuum tightness 0.09MPa condition, obtains concentrated solution, concentrated solution uses hydrochloric acid adjust pH 4.7, leaving standstill 36 hours, filter and obtain wet crystal, is 0.09 ± 0.001MPa in vacuum tightness afterwards, vacuum-drying under temperature 60 C condition, product drying obtained, carry out mechanical disintegration to 80 ~ 120 orders, obtains the Hesperidin powder-product 4.95kg that content is 91.5%.
Embodiment 3:
Take 100kg peel of Citrus reticulata Blanco raw material, in raw material, mandarin oil content is 1.2%, and content of hesperidin is 4.7%; Keep peel of Citrus reticulata Blanco moisture to be 13 wt %, adopt pair roller flaking machine to roll sheet; Roll sheet peel of Citrus reticulata Blanco thickness that sheet obtains at 0.5mm, fines content be 6.3%(and granularity be less than that 20 orders account for gross weight 6.3%).
According to vegetable oil extraction solvent: 95% ethanol=1:3.5(volume) mixed preparing mixed solvent, extract sheet peel of Citrus reticulata Blanco with this mixed solvent, solid-liquid ratio is 1:6(kg/l), extraction temperature 55 DEG C, stirring velocity 200r/min, extracts 3 times, each 2 hours, obtain mixed solvent extracting solution; It is that the siccative slag of 6.4 wt %, dissolvent residual 640ppm is for pectin production that wet feed slag obtains moisture after super-dry.
According to 1:0.5(volume in mixed solvent extracting solution) ratio add water, stratification, be separated obtain alcohol-water layer and vegetable oil extraction solvent layer, the Residual oil of alcohol layer controls below 0.1%.Described vegetable oil extraction solvent layer filters, concentrated, desolvation residual after obtain 1.19kg mandarin oil.
Alcohol-water layer is 0.09MPa at vapor pressure, gas phase temperature is 67 DEG C, concentrated under vacuum tightness 0.09MPa condition, obtains concentrated solution, concentrated solution uses hydrochloric acid adjust pH 4.7, leaving standstill 48 hours, filter and obtain wet crystal, is 0.09 ± 0.001MPa in vacuum tightness afterwards, vacuum-drying under temperature 68 DEG C of conditions, product drying obtained, carry out mechanical disintegration to 80 ~ 120 orders, obtains the Hesperidin powder-product 5kg that content is 90.2%.
Embodiment 4:
Take 100kg peel of Citrus reticulata Blanco raw material, in raw material, mandarin oil content is 1.2%, and content of hesperidin is 4.7%.Peel of Citrus reticulata Blanco moisture is kept to be 12 wt %, adopt pair roller flaking machine to roll sheet; Rolling the sheet peel of Citrus reticulata Blanco thickness that sheet obtains is 0.45mm, fines content be 5%(and granularity be less than that 20 orders account for gross weight 7.8%).
According to vegetable oil extraction solvent: 91% ethanol=1:2.5(volume ratio) mixed preparing mixed solvent, sheet peel of Citrus reticulata Blanco is extracted with this mixed solvent, solid-liquid ratio is 1:4.5(kg/L), extraction temperature 45 DEG C, stirring velocity 70r/min, extract 3 times, the time is respectively 2 times 2 hours, 1 time 1 hour, obtains mixed solvent extracting solution; It is that the siccative slag of 6 wt %, dissolvent residual 435ppm is for pectin production that wet feed slag obtains moisture after super-dry.
According to 1:0.7(volume in mixed solvent extracting solution) ratio add water, stratification, be separated obtain alcohol-water layer and vegetable oil extraction solvent layer, the Residual oil of alcohol layer controls below 0.1%.Described vegetable oil extraction solvent layer filters, concentrated, desolvation residual after obtain 1.17kg mandarin oil.
Alcohol-water layer is 0.085MPa at vapor pressure, gas phase temperature is 64 DEG C, concentrated under vacuum tightness 0.095MPa condition, obtains concentrated solution, concentrated solution uses hydrochloric acid adjust pH 4.5, leaving standstill 30 hours, filter and obtain wet crystal, is 0.09 ± 0.001MPa in vacuum tightness afterwards, vacuum-drying under temperature 70 C condition, product drying obtained, carry out mechanical disintegration to 80 ~ 120 orders, obtains the Hesperidin powder-product 4.8kg that content is 93.7%.
Embodiment 5:
Take 100kg peel of Citrus reticulata Blanco raw material, in raw material, mandarin oil content is 1.2%, and content of hesperidin is 4.7%; Keep peel of Citrus reticulata Blanco moisture to be 8 wt %, adopt pair roller flaking machine to roll sheet; Roll sheet peel of Citrus reticulata Blanco thickness that sheet obtains at 0.1mm, fines content be 10%(and granularity be less than that 20 orders account for gross weight 10%).
According to vegetable oil extraction solvent: 94% ethanol=1:3(volume) mixed preparing mixed solvent, sheet peel of Citrus reticulata Blanco is extracted with this mixed solvent, solid-liquid ratio is 1:5.5(kg/l), extraction temperature 52 DEG C, stirring velocity 90r/min, extracts 4 times, and the time is respectively 2 times 2 hours, 1 time 1.5 hours, 1 time 1 hour, obtain mixed solvent extracting solution; It is that the siccative slag of 12 wt %, dissolvent residual 500ppm is for pectin production that wet feed slag obtains moisture after super-dry.
According to 1:0.6(volume in mixed solvent extracting solution) ratio add water, stratification, be separated obtain alcohol-water layer and vegetable oil extraction solvent layer, the Residual oil of alcohol layer controls below 0.1%.Described vegetable oil extraction solvent layer filters, concentrated, desolvation residual after obtain 1.17kg mandarin oil.
Alcohol-water layer is 0.095MPa at vapor pressure, gas phase temperature is 66 DEG C, concentrated under vacuum tightness 0.092MPa condition, obtains concentrated solution, concentrated solution uses hydrochloric acid adjust pH 5.5, leaving standstill 42 hours, filter and obtain wet crystal, is 0.09 ± 0.001MPa in vacuum tightness afterwards, vacuum-drying under temperature 62 DEG C of conditions, product drying obtained, carry out mechanical disintegration to 80 ~ 120 orders, obtains the Hesperidin powder-product 4.95kg that content is 92.7%.
Above by embodiment to invention has been detailed description; but described content is only preferred embodiment of the present invention; utilize technical solutions according to the invention; or those skilled in the art is under the inspiration of technical solution of the present invention; design similar technical scheme; and reach above-mentioned technique effect, be all fall into protection scope of the present invention.
Claims (9)
1. extract a method for mandarin oil and Hesperidin in peel of Citrus reticulata Blanco, it is characterized in that: peel of Citrus reticulata Blanco is carried out roll sheet and obtain sheet peel of Citrus reticulata Blanco; Extract sheet peel of Citrus reticulata Blanco with the mixed solvent of vegetable oil extraction solvent and ethanol, extracting solution adds water separation, obtains alcohol-water layer and vegetable oil extraction solvent layer; Vegetable oil extraction solvent layer is concentrated, remove molten residual after, obtain mandarin oil; Concentrated by alcohol-water layer, acid is heavy, filter and obtain Hesperidin and to wet crystal, Hesperidin crystal drying of wetting obtains Hesperidin product.
2. extract the method for mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco according to claim 1, it is characterized in that: before described peel of Citrus reticulata Blanco rolls sheet, moisture is 8-13wt%; Described to roll the thickness that sheet obtains sheet peel of Citrus reticulata Blanco be 0.1-0.5mm, and sheet peel of Citrus reticulata Blanco 20 mesh sieve percent of pass is less than 12%.
3. according to the method extracting mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco described in claim 1, it is characterized in that: the ethanol-water solution of described ethanol to be volume fraction be 90-95%, in described mixed solvent, the volume ratio of vegetable oil extraction solvent and 90-95% ethanol is 1:2.5-3.5.
4. extract the method for mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco according to claim 3, it is characterized in that: described Extracting temperature is 45-55 DEG C; The feed liquid mass volume ratio of described extraction is 1:4-6, and described mass unit is kilogram, and described volume unit is for rising; Stirring velocity is 60-200r/min; Extract 3-5 time, often all over extracting 1-2 hour.
5. extract the method for mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco according to claim 1-4 any one, it is characterized in that: the described acid condition of sinking is: pH value is 4.5-5.5; Settling time is 24-48 hour.
6. extract the method for mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco according to claim 1-4 any one, it is characterized in that: described extracting solution adds water in sepn process, the volume ratio of extracting solution and water is 1:0.5-1, is separated after stratification.
7. in a kind of peel of Citrus reticulata Blanco according to claim 1-4 any one, extract the method for mandarin oil and Hesperidin, it is characterized in that: described alcohol-water layer employing vacuum concentration condition is: vapor pressure is 0.085-0.095MPa, gas phase temperature is 63-67 DEG C, vacuum tightness 0.09-0.095MPa.
8. extract the method for mandarin oil and Hesperidin in a kind of peel of Citrus reticulata Blanco according to claim 7 any one, it is characterized in that: the described Hesperidin crystal drying conditions that wets is: vacuum tightness is 0.09 ± 0.001MPa, temperature 60-70 DEG C.
9. in a kind of peel of Citrus reticulata Blanco according to Claim 8 described in any one, extract the method for mandarin oil and Hesperidin, it is characterized in that: the feed liquid of described extraction uses 100 mesh filter screens to filter, filter residue disk dryer carries out drying, and dried material pulp water sub-control is built in 6-12wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558003A (en) * | 2022-09-30 | 2023-01-03 | 台州学院 | Method for extracting citrus essential oil and hesperidin from citrus peel |
| CN116333010A (en) * | 2023-03-27 | 2023-06-27 | 昆明理工大学 | Method for improving extraction amount of hesperidin in citrus peel |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445440A (en) * | 2008-12-23 | 2009-06-03 | 晨光天然色素集团有限公司 | Method for extracting refined curcumin and curcuma oil from curcuma |
| CN101704867A (en) * | 2009-11-03 | 2010-05-12 | 国家海洋局第三海洋研究所 | Method for preparing naringin or hesperidin |
| CN102816191A (en) * | 2012-08-23 | 2012-12-12 | 高伟 | Method for producing neohesperidin dihydrochalcone |
| CN102839053A (en) * | 2012-08-23 | 2012-12-26 | 高伟 | Method for extracting aurantiamarin from orange peel |
| CN103113438A (en) * | 2013-01-30 | 2013-05-22 | 唐忠海 | Method for extracting hesperidin and orange peel uranidin from orange peel |
| CN103833809A (en) * | 2014-01-21 | 2014-06-04 | 李玉山 | Novel extraction and separation process of naringin |
-
2014
- 2014-12-15 CN CN201410770252.2A patent/CN104402952B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445440A (en) * | 2008-12-23 | 2009-06-03 | 晨光天然色素集团有限公司 | Method for extracting refined curcumin and curcuma oil from curcuma |
| CN101704867A (en) * | 2009-11-03 | 2010-05-12 | 国家海洋局第三海洋研究所 | Method for preparing naringin or hesperidin |
| CN102816191A (en) * | 2012-08-23 | 2012-12-12 | 高伟 | Method for producing neohesperidin dihydrochalcone |
| CN102839053A (en) * | 2012-08-23 | 2012-12-26 | 高伟 | Method for extracting aurantiamarin from orange peel |
| CN103113438A (en) * | 2013-01-30 | 2013-05-22 | 唐忠海 | Method for extracting hesperidin and orange peel uranidin from orange peel |
| CN103833809A (en) * | 2014-01-21 | 2014-06-04 | 李玉山 | Novel extraction and separation process of naringin |
Non-Patent Citations (3)
| Title |
|---|
| 李建敏，等: "联合提取柑桔皮中精油、色素、果胶和橙皮苷", 《生物质化学工程》, vol. 41, no. 1, 31 January 2007 (2007-01-31), pages 22 - 24 * |
| 郑旭煦，等: "从橙皮中提取香精油的工艺条件研究", 《天然产物研究与开发》, vol. 15, no. 6, 31 December 2003 (2003-12-31) * |
| 马丽萍，等: "柑桔皮渣中香精油和橙皮苷的联合提取纯化工艺研究", 《食品工业科技》, vol. 29, no. 3, 31 December 2008 (2008-12-31), pages 151 - 154 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115558003A (en) * | 2022-09-30 | 2023-01-03 | 台州学院 | Method for extracting citrus essential oil and hesperidin from citrus peel |
| CN116333010A (en) * | 2023-03-27 | 2023-06-27 | 昆明理工大学 | Method for improving extraction amount of hesperidin in citrus peel |
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