CN1530376A - Extraction of eight products, such as pectine, naringin, etc. - Google Patents
Extraction of eight products, such as pectine, naringin, etc. Download PDFInfo
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- CN1530376A CN1530376A CNA031181759A CN03118175A CN1530376A CN 1530376 A CN1530376 A CN 1530376A CN A031181759 A CNA031181759 A CN A031181759A CN 03118175 A CN03118175 A CN 03118175A CN 1530376 A CN1530376 A CN 1530376A
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Abstract
A process for extracting essence oil, fruit juice, pectin, edible fibres, naringoside, hesperidin, 3,3',3',5,6,7,8-heptamethoxy flavone and limonoid from pomelo fruit features respective use of cold grinding, squeezing, nano filtering, microwave or reflux extracting, ultrafiltering concentrating, chromatographic separating and alcohol extracting. Its advantages are high output rate and quality of products, easy removal of impurities, and no use of toxic and harmful organic solvent.
Description
[technical field] the invention belongs to deep processing of farm products and natural medicine technical field, be specifically related to a kind of volatile oil, fruit juice, pectin, food fiber and naringin thereof, hesperidine, 3 of from shaddock, extracting simultaneously, 3 ', 4 ', 5,6,7, the method for 8-Heptamethoxyflavone monomer and limonoids.
[background technology] shaddock is the mature fruit of rutaceae evergreen fruit trees teak.China's shaddock has shatian pomelo by the region branch, the close shaddock of herdsman's small stream, the fragrant shaddock of western Hunan gold, kinds such as Jiang Yongxiang shaddock.Shaddock ped volatile oil has the fragrant local flavor of charming uniqueness, form by compounds such as terpenes, alcohol, aldehyde and esters, be correctives, the reodorant of beverage, beer, candy, cake, essence also has been widely used in daily necessities such as perfume, face cream, toothpaste, perfumed soap.Naringin energy blood viscosity lowering reduces the formation of blood fat and thrombus, and cardiovascular system diseases is had good efficacy, and blister stomatitis and stomach ulcer are also had tangible curative effect.Pectin (pectin) mainly is present in the shaddock pericarp, in foodstuffs industry, is used for jam, candy, beverage and food with low sugar content in a large number as foodstuff additive, is used as jelling agent, thickening material, emulsifying agent and stablizer.Pectin also is used for medicine industry, have antibiotic, to the heavy metal detoxification isoreactivity, pectin or pectin aluminium salt can suppress the absorption of enteron aisle to cholesterol and triglyceride, also can be used as the auxiliary therapeutical agent of cardiovascular disordeies such as arteriosclerosis.The shaddock fiber has fat-reducing and antihyperglycemic, can be used as the filler of some food.3,3 ', 4 ', 5,6,7, the 8-Heptamethoxyflavone has the effect of treatment leukemia, and limonoids (Limonoids) (obacunone glycoside, Nomilin glycoside) has extremely strong antitumour activity.Limonoids can activate the intravital toxenzyme of mainly separating---the activity of Thiadiazolidine isomerase (GSH-S-transferase) strongly.A large amount of animal experiment proof limonoidss have the cancer effects such as liver cancer, carcinoma of small intestine, oral carcinoma and skin carcinoma that inhibition is caused by chemical substance.
More existing at present report documents to shaddock processing disclose a kind of particularly method of naringin of flavonoid glycoside of extracting as Chinese patent CN1072933A from plant, Chinese patent CN1356327A discloses a kind of method of extracting flavones from shaddock ped.But all have the following disadvantages: (1) product is single.A kind of single product can only be produced in the flow process, as can only obtaining pectin, or only naringin can be obtained.(2) separation efficiency is low, and product purity is not high.(3) the organic solvent consumption is big, have in addition use the poisonous and harmful solvent.
[summary of the invention] the purpose of this invention is to provide a kind of from shaddock, can extract simultaneously volatile oil, fruit juice, pectin, food fiber and naringin thereof, hesperidine, 3,3 ', 4 ', 5,6,7, the method for 8-Heptamethoxyflavone monomer and limonoids.
The present invention is a raw material with Hunan Jiang Yongxiang shaddock, adopts cold grinding method or milling process to obtain volatile oil and the residual fruit of shaddock in conjunction with distillation method; Adopt milling process from the residual fruit of shaddock, to obtain Fructus Citri grandis juice and the thick slag of shaddock; The gained Fructus Citri grandis juice is by the polymeric adsorbent debitterize, and the ceramic membrane filter clarification obtains high dense no bitter shaddock juice after nanofiltration is concentrated; The thick slag of shaddock is made solvent with ethanol after crushed, adopts microwave or backflow lixiviate, and natural settling agent precipitation is removed macromole impurity in conjunction with ultrafiltration, and gained solution is through ultrafiltration and concentration, the macroporous adsorbent resin enrichment, and stepwise elution obtains naringin, hesperidine monomer; After adopting preparative chromatography to separate, another part cut solution obtains 3,3 respectively ', 4 ', 5,6,7,8-Heptamethoxyflavone monomer and limonoids; Ethanol lixiviate insolubles employing hydrochloric acid or phosphoric acid, sulfuric acid acidation hydrolysis, hydrolyzed solution decolours through polymeric adsorbent, and transferring pH is 6～8, and ultrafiltration and concentration obtains pectin powder with spraying drying; The acid hydrolysis insolubles leaches with NaOH solution, and leach liquor is with activated carbon decolorizing, and adjust pH obtains the caustic solubility food fiber near neutral with spray-drying process then.
The present invention extracts when also being applicable in other regional shaddock above-mentioned product simultaneously.
The present invention adopts cold grinding method to extract shaddock volatile oil, can significantly improve the rate of recovery and the quality of volatile oil; Adopt ethanolic soln microwave or backflow lixiviate, strengthen the stripping of effective constituent, shorten extraction time, improve productive rate, reduce the impurity stripping; Natural settling agent sedimentations such as employing glucomannan compounds are beneficial to the removal of macromole impurity such as protein, starch in conjunction with ultra-filtration technique, are better than separation technology such as present used alcohol precipitation; The employing nanofiltration concentrates, and normal temperature does not have phase transformation, has both saved the energy, has avoided the decomposition of activeconstituents to destroy again; With polymeric adsorbent chromatography column separation system, bigger resolution and the accumulation rate that has improved naringin and hesperidine; Adopt preparative chromatography, make 3,3 ', 4 ', 5,6,7,8-Heptamethoxyflavone monomer and limonoids are effectively separated, and obtain high-purity Heptamethoxyflavone monomer.Do not use the poisonous and harmful organic solvent in the whole separation and Extraction process, realize the green extraction of whole process.
[description of drawings] Fig. 1: process flow diagram of the present invention.
[embodiment] gets Jiang Yongxiang shaddock fresh fruit 50kg, and cold grinding obtains the about 7L of oil-water mixture.Divide oil with water-and-oil separator, left standstill the about 300g of sucking-off upper strata clarified oil 3 hours under 5 ℃.The residual fruit of shaddock adopts milling process to obtain Fructus Citri grandis juice and the thick slag of shaddock.Fructus Citri grandis juice is by a kind of resin debitterize, and through ceramic filter, nanofiltration concentrates and obtains high dense no bitter shaddock juice 2kg.The thick slag of shaddock with 8 times of amounts, 75% ethanol microwave lixiviate 3 times, 1h/ time, filters after crushed.Filtrate adds natural settling agent sedimentation, and the ultrafiltration and concentration separation obtains the 2.5L concentrated solution, then through the polymeric adsorbent enrichment, and stepwise elution, vacuum-drying obtains the about 140g of naringin monomer, hesperidine monomer 15g.All the other stepwise elution cuts separate through preparative chromatography, and lyophilize obtains 3,3 ', 4 ', 5,6,7,8-Heptamethoxyflavone monomer 13mg, limonoids 70mg.Ethanol lixiviate insolubles adopts 10 times of amount 0.01mol/L hcl acidifyings, and 85 ℃ of following hydrolysis twice, each 1h merges hydrolyzed solution, adds 100g macroporous adsorbent resin vibration decolouring 25min in the hydrolyzed solution.Filter, after filtrate was adjusted pH to 8 with 2% ammoniacal liquor, ultrafiltration and concentration obtained pectin powder 1.2kg 80 ℃ of spraying dryings.The acid hydrolysis insolubles adopts 10 times of amount 0.5mol/L NaOH solution to soak 3 hours at 35 ℃, adds the 25g activated carbon decolorizing in the leach liquor, filters then, and filtrate is transferred pH to 8, and the spray-dried caustic solubility food fiber that obtains is about 1.4kg.
Claims (2)
1. extract the method for eight kinds of products such as pectin, naringin from shaddock simultaneously, it is characterized in that: the present invention is a raw material with Hunan Jiang Yongxiang shaddock, adopts cold grinding method or milling process to obtain volatile oil and the residual fruit of shaddock in conjunction with distillation method; Adopt milling process from the residual fruit of shaddock, to obtain Fructus Citri grandis juice and the thick slag of shaddock; The gained Fructus Citri grandis juice is by the polymeric adsorbent debitterize, and the ceramic membrane filter clarification obtains high dense no bitter shaddock juice after nanofiltration is concentrated; The thick slag of shaddock is made solvent with ethanol after crushed, adopts microwave or backflow lixiviate, and natural settling agent precipitation is removed macromole impurity in conjunction with ultrafiltration, and gained solution is through ultrafiltration and concentration, the macroporous adsorbent resin enrichment, and stepwise elution obtains naringin, hesperidine monomer; After adopting preparative chromatography to separate, another part cut solution obtains 3,3 respectively ', 4 ', 5,6,7,8-Heptamethoxyflavone monomer and limonoids; Ethanol lixiviate insolubles employing hydrochloric acid or phosphoric acid, sulfuric acid acidation hydrolysis, hydrolyzed solution decolours through polymeric adsorbent, and transferring pH is 6～8, and ultrafiltration and concentration obtains pectin powder with spraying drying; The acid hydrolysis insolubles leaches with NaOH solution, and leach liquor is with activated carbon decolorizing, and adjust pH obtains the caustic solubility food fiber near neutral with spray-drying process then.
2. method according to claim 1 is characterized in that: the present invention extracts when also being applicable in other regional shaddock above-mentioned product simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031181759A CN1530376A (en) | 2003-03-12 | 2003-03-12 | Extraction of eight products, such as pectine, naringin, etc. |
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| CNA031181759A CN1530376A (en) | 2003-03-12 | 2003-03-12 | Extraction of eight products, such as pectine, naringin, etc. |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332008C (en) * | 2005-05-31 | 2007-08-15 | 浙江大学 | Process for extracting tangerine essential oil |
| CN101066986B (en) * | 2007-06-05 | 2010-05-26 | 浙江省农业科学院 | Process of extracting flavone from side product of orange processing |
| CN101037485B (en) * | 2007-04-20 | 2010-06-09 | 兰州大学 | Pectin extraction method |
| CN101020860B (en) * | 2007-01-16 | 2011-01-05 | 刘思强 | Anti-senility golden shaddock oil |
| CN102161712A (en) * | 2011-03-04 | 2011-08-24 | 重庆莱美药业股份有限公司 | Method for preparing micromolecule pectin |
| CN102326746A (en) * | 2011-06-13 | 2012-01-25 | 徐春根 | Process for compressively utilizing grapefruits |
| CN102864019A (en) * | 2012-09-29 | 2013-01-09 | 集美大学 | Method for co-production of essential oil and pectin by shaddock peels |
| CN103484257A (en) * | 2013-10-14 | 2014-01-01 | 厦门大学 | Comprehensive utilization method for pomelo peels |
| CN105061532A (en) * | 2015-08-10 | 2015-11-18 | 厦门世达膜科技有限公司 | Production method for hesperidin |
| CN105995326A (en) * | 2016-05-20 | 2016-10-12 | 西南大学柑桔研究所 | Method for acquiring pectin, tangerine peel fiber and tangerine peel fermented beverage by classifying citrus peels |
| CN106188181A (en) * | 2016-06-30 | 2016-12-07 | 湖南鑫利生物科技有限公司 | A kind of method extracting naringin from pomelo peel |
| CN106479677A (en) * | 2016-12-27 | 2017-03-08 | 广东梅州市富柚生物科技有限公司 | A kind of production method of Fructus Citri grandiss quintessence oil |
| CN106511114A (en) * | 2016-11-18 | 2017-03-22 | 苏州丽舒雅生物科技有限公司 | Broad spectrum bactericidal pure natural orange extract essence and preparation method thereof |
| CN106632547A (en) * | 2016-12-14 | 2017-05-10 | 雅安太时生物科技股份有限公司 | Method for extracting naringin, synephrine and pectin from young shaddock fruits |
| CN109096353A (en) * | 2018-08-08 | 2018-12-28 | 曹庸 | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit |
| CN110272567A (en) * | 2017-02-15 | 2019-09-24 | Cp凯可股份公司 | Biomass compositions, product and the production method of pectin comprising activation |
| CN111748008A (en) * | 2020-08-03 | 2020-10-09 | 华中农业大学 | Method for extracting naringin and limonin from shaddock peel |
| CN113501892A (en) * | 2021-07-23 | 2021-10-15 | 江西莱檬生物科技有限责任公司 | Combined extraction method for different functional components in citrus fruit peel residues |
| CN114177228A (en) * | 2021-10-25 | 2022-03-15 | 惠州学院 | Grapefruit young fruit-based functional component combined extraction method |
-
2003
- 2003-03-12 CN CNA031181759A patent/CN1530376A/en active Pending
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1332008C (en) * | 2005-05-31 | 2007-08-15 | 浙江大学 | Process for extracting tangerine essential oil |
| CN101020860B (en) * | 2007-01-16 | 2011-01-05 | 刘思强 | Anti-senility golden shaddock oil |
| CN101037485B (en) * | 2007-04-20 | 2010-06-09 | 兰州大学 | Pectin extraction method |
| CN101066986B (en) * | 2007-06-05 | 2010-05-26 | 浙江省农业科学院 | Process of extracting flavone from side product of orange processing |
| CN102161712A (en) * | 2011-03-04 | 2011-08-24 | 重庆莱美药业股份有限公司 | Method for preparing micromolecule pectin |
| CN102161712B (en) * | 2011-03-04 | 2013-05-01 | 重庆莱美药业股份有限公司 | Method for preparing micromolecule pectin |
| CN102326746A (en) * | 2011-06-13 | 2012-01-25 | 徐春根 | Process for compressively utilizing grapefruits |
| CN102864019A (en) * | 2012-09-29 | 2013-01-09 | 集美大学 | Method for co-production of essential oil and pectin by shaddock peels |
| CN103484257A (en) * | 2013-10-14 | 2014-01-01 | 厦门大学 | Comprehensive utilization method for pomelo peels |
| CN103484257B (en) * | 2013-10-14 | 2015-11-11 | 厦门大学 | A kind of method of comprehensive utilization of shaddock ped |
| CN105061532B (en) * | 2015-08-10 | 2019-01-18 | 厦门世达膜科技有限公司 | A kind of production method of hesperidine |
| CN105061532A (en) * | 2015-08-10 | 2015-11-18 | 厦门世达膜科技有限公司 | Production method for hesperidin |
| CN105995326A (en) * | 2016-05-20 | 2016-10-12 | 西南大学柑桔研究所 | Method for acquiring pectin, tangerine peel fiber and tangerine peel fermented beverage by classifying citrus peels |
| CN106188181A (en) * | 2016-06-30 | 2016-12-07 | 湖南鑫利生物科技有限公司 | A kind of method extracting naringin from pomelo peel |
| CN106188181B (en) * | 2016-06-30 | 2018-10-30 | 湖南鑫利生物科技有限公司 | A method of extracting aurantiin from pomelo peel |
| CN106511114A (en) * | 2016-11-18 | 2017-03-22 | 苏州丽舒雅生物科技有限公司 | Broad spectrum bactericidal pure natural orange extract essence and preparation method thereof |
| CN106632547B (en) * | 2016-12-14 | 2019-03-26 | 雅安太时生物科技股份有限公司 | A method of extracting naringin, synephrine and pectin from shaddock young fruit |
| CN106632547A (en) * | 2016-12-14 | 2017-05-10 | 雅安太时生物科技股份有限公司 | Method for extracting naringin, synephrine and pectin from young shaddock fruits |
| CN106479677A (en) * | 2016-12-27 | 2017-03-08 | 广东梅州市富柚生物科技有限公司 | A kind of production method of Fructus Citri grandiss quintessence oil |
| CN110272567A (en) * | 2017-02-15 | 2019-09-24 | Cp凯可股份公司 | Biomass compositions, product and the production method of pectin comprising activation |
| CN110272567B (en) * | 2017-02-15 | 2022-04-15 | Cp凯可股份公司 | Biomass composition comprising activated pectin, products and methods of production |
| CN109096353A (en) * | 2018-08-08 | 2018-12-28 | 曹庸 | A kind of method that continuous phase transistion extracts aurantiamarin and pectin in citrus young fruit |
| CN111748008A (en) * | 2020-08-03 | 2020-10-09 | 华中农业大学 | Method for extracting naringin and limonin from shaddock peel |
| CN113501892A (en) * | 2021-07-23 | 2021-10-15 | 江西莱檬生物科技有限责任公司 | Combined extraction method for different functional components in citrus fruit peel residues |
| CN114177228A (en) * | 2021-10-25 | 2022-03-15 | 惠州学院 | Grapefruit young fruit-based functional component combined extraction method |
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