CN100360516C - Method for extracting apple polyphenol from apple pomace by supercritical CO2 - Google Patents

Method for extracting apple polyphenol from apple pomace by supercritical CO2 Download PDF

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Publication number
CN100360516C
CN100360516C CNB2005100481680A CN200510048168A CN100360516C CN 100360516 C CN100360516 C CN 100360516C CN B2005100481680 A CNB2005100481680 A CN B2005100481680A CN 200510048168 A CN200510048168 A CN 200510048168A CN 100360516 C CN100360516 C CN 100360516C
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apple
supercritical
extracting
polyphenol
extraction
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CN1803790A (en
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魏福祥
曲恩超
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Hebei University of Science and Technology
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Hebei University of Science and Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The present invention provides a method for extracting apple polyphenol from apple pomace by supercritical CO2, which is completed by adopting the following steps: A, firstly, the apple pomace is pulverized to 40 meshes; according to the proportion that 100 ml of 95% alcohol is added to 100g of apple powder, and then, the apple powder is sufficiently mixed into mud-shaped objects; B, the apple pomace mud is added to a supercritical fluid extraction tank; a CO2 steel bottle is opened; extraction is carried out by making the alcohol used as a carrying agent; the temperature of an extractor is from 50 to 60 DEG C; extraction pressure is from 25 to 35MPa; CO2 flow capacity is from 40 to 45 kg/h; extraction time is from 2 to 4h, and finally, apple polyphenol crude products are obtained. The present invention makes apple pomace plant cells break walls and dissolve effective ingredients by making use of the high pressure and the high penetrability of the CO2, and apple polyphenol yield is higher than that extracted by organic solvent; the method has the advantages of simple and reliable process and stable operation; the disused resources are sufficiently utilized, and corresponding economical benefit and social benefit are generated.

Description

The method of supercritical co extracting apple polyphenol from apple residue
Technical field
The present invention relates to a kind of from apple residue the method for extracting apple polyphenol, particularly a kind of supercritical CO 2The method of extracting apple polyphenol from apple residue belongs to the extracting method technical field of active ingredient of natural plant.
Background technology
Apple polyphenol is a naturally occurring class important biomolecule active substance in the apple, has numerous important physical functions and great development and application values.It has strong anti-oxidation, the different originality of resistance and prevention of dental caries effect, can develop healthcare products, natural antioxidants or functional food additives, is one of natural compounds that receives much attention at present.At present, produce the method for Fructus Mali pumilae extract, adopt traditional organic solvent extractionprocess both at home and abroad, never extract the apple polyphenol crude extract in the transparent apple, through resin or column chromatographic isolation and purification.The patent No. is that the patent of invention of 01120589.X discloses and a kind ofly extracts the production technique of apple polyphenol with apple peel, continues to use aforesaid method, and this method extraction time is long, the organic solvent consumption is big.
Summary of the invention
The object of the present invention is to provide a kind of supercritical CO 2The method of extracting apple polyphenol from the apple residue after the squeezing Sucus Mali pumilae.Because the polyphenols in the apple mainly contains pycnogenols, phenolic acid and Flavonoid substances, polarity is very strong, single CO with low-pole 2Be difficult to extract, the present invention selects to add the extraction of polarity entrainment agent.
Technical scheme of the present invention is achieved in that the method for this supercritical co extracting apple polyphenol from apple residue, adopts following steps to finish:
A, elder generation are crushed to 40 orders with apple residue, add 100mL95% alcoholic acid ratio according to 100g apple powder, fully stir into mud shape thing;
B, apple residue mud is added in the supercritical fluid extraction jar, open CO 2Steel cylinder begins extraction with ethanol for carrying agent, and the extractor temperature is 50~60 ℃, and extracting pressure is 25~35MPa, CO 2Flow is 40~45Kg/h, and the extraction time is 2~4h, obtains the apple polyphenol crude product.
The method of described supercritical co extracting apple polyphenol from apple residue, the described CO of step B 2Behind the gas process cleaner I, enter condenser liquefaction, enter cleaner II again by the ram pump pressurization then and further liquefy, enter the extractor bottom, be dissolved with the CO of solute by pipeline 2Fluid comes out to enter separator by the extractor top, forms to reflux.
The method of described supercritical co extracting apple polyphenol from apple residue, the pressure of setting primary separator I is 6MPa, temperature is 60 ℃; The pressure of second-stage separator II is 6MPa, and temperature is 45 ℃.
The method of described supercritical co extracting apple polyphenol from apple residue, step B is described, and to carry agent be 95% ethanol or dehydrated alcohol.
Technical progress effect of the present invention shows: adopt supercritical CO 2Extracting apple polyphenol from apple residue utilizes CO 2High pressure, high seepage force, make the apple residue plant cell wall breaking, the stripping effective ingredient, the apple polyphenol yield is higher than the apple polyphenol yield of organic solvent extraction, and flow process is simple and reliable, stable operation, waste resource is made full use of, produce corresponding economic benefit and social benefit.
Description of drawings
Fig. 1 is a supercritical CO of the present invention 2Fluid extraction part schema
Embodiment
Embodiment 1, dried apple residue is crushed to 40 orders, takes by weighing 100g and add and make mud shape medicinal extract after 95% ethanol 100mL fully stirs, pack in the supercritical fluid extraction device, open CO 2Steel cylinder behind the gas process cleaner I, enters condenser liquefaction, enters cleaner II again by the ram pump pressurization then and further liquefies, and enters the extractor bottom by pipeline, sets extractor extracting pressure 35MPa, 55 ℃ of temperature, and static extracting 1 hour utilizes CO 2High pressure, high seepage force, make the apple residue plant cell wall breaking, the stripping effective ingredient; Then, start the entrainment agent pump and inject 95% ethanol simultaneously, dynamic extraction 1-2 hour, the entrainment agent flow was 0.1L/h, obtained product from two separators, and the pressure of setting separator I is 6MPa, and temperature is 60 ℃; The pressure of second-stage separator II is 6MPa, and temperature is 45 ℃.Adopt the Folin-Ciocalteu method to measure polyphenol total amount in the extract, the apple polyphenol yield is 0.12%-0.16%.
60 ℃ of embodiment 2, setting extraction temperature, extracting pressure 30MPa, entrainment agent changes dehydrated alcohol into, and other is with the preparation method of embodiment 1.Adopt the Folin-Ciocalteu method to measure polyphenol total amount in the extract, the apple polyphenol yield is 0.12%-0.15%.
Embodiment 3, extraction using alcohol apple polyphenol controlled trial
Take by weighing and be crushed to 40 purpose apple ground-slag 100g, extract 3 times down in 80 ℃ with 300mL ethanol, each 2 hours, adopt the Folin-Ciocalteu method to measure polyphenol total amount in the extract, the apple polyphenol yield is 0.09%-0.11%.
Adopt supercritical CO by the apple polyphenol yield explanation that comparative examples 1,2,3 is measured 2Extracting apple polyphenol is higher than the apple polyphenol yield of organic solvent extraction from apple residue.
Supercritical CO of the present invention 2Extraction equipment is selected from Huaan, Nantong supercritical extraction company limited; The pomace source is Baoding subsidiary factory of fruit juice factory of Huiyuan, and is the tankage after squeezing the juice.
Listed examples of the present invention is intended to set forth further processing method, and scope of the present invention is not constituted any restriction.The product that example of the present invention obtains and all can obtain the thick product of apple polyphenol via the described method of claims 1-4 of the present invention.

Claims (3)

1, the method for supercritical co extracting apple polyphenol from apple residue is characterized in that adopting following steps to finish:
A, elder generation are crushed to 40 orders with apple residue, add 100mL95% alcoholic acid ratio according to 100g apple powder, fully stir into mud shape thing;
B, apple residue mud is added in the supercritical fluid extraction jar, open CO 2Steel cylinder, CO 2Behind the gas process cleaner I, enter condenser liquefaction, enter cleaner II again by the ram pump pressurization then and further liquefy, enter the extractor bottom, be dissolved with the CO of solute by pipeline 2Fluid comes out to enter separator by the extractor top, forms to reflux;
Begin extraction with ethanol for carrying agent, the extractor temperature is 50~60 ℃, and extracting pressure is 25~35MPa, CO 2Flow is 40~45Kg/h, and the extraction time is 2~4h, obtains the apple polyphenol crude product.
2, the method for supercritical co according to claim 1 extracting apple polyphenol from apple residue is characterized in that: described separator is two, and the pressure of setting primary separator I is 6MPa, and temperature is 60 ℃; The pressure of second-stage separator II is 6MPa, and temperature is 45 ℃.
3, the method for supercritical co according to claim 1 extracting apple polyphenol from apple residue is characterized in that: step B is described, and to carry agent be 95% ethanol or dehydrated alcohol.
CNB2005100481680A 2005-12-09 2005-12-09 Method for extracting apple polyphenol from apple pomace by supercritical CO2 Expired - Fee Related CN100360516C (en)

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101829210B (en) * 2010-05-21 2011-10-05 西安应化生物技术有限公司 Method for preparing apple polyphenol
CN104262423B (en) * 2014-09-30 2017-04-05 桂林三宝药业有限公司 A kind of method that phlorhizin is extracted from litchi rind
CN107828421A (en) * 2017-11-28 2018-03-23 马鞍山菌菌食品科技有限公司 A kind of preparation method for being sustained olive pomace discarded object soil conditioner

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1166662C (en) * 2001-07-25 2004-09-15 於洪建 Malic polyphenol producing process with apple peel slag

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1166662C (en) * 2001-07-25 2004-09-15 於洪建 Malic polyphenol producing process with apple peel slag

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
苹果多酚的开发及应用. 唐传核,彭志英.《中国食品添加剂》. 2001 *
超临界CO_2萃取技术及其在生物资源开发利用中应用的最新进展(Ⅱ). 马海乐.《包装与食品机械》. 2001 *

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