CN102617655A - Method for subcritical water extraction of oleuropein - Google Patents
Method for subcritical water extraction of oleuropein Download PDFInfo
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- CN102617655A CN102617655A CN201210062636XA CN201210062636A CN102617655A CN 102617655 A CN102617655 A CN 102617655A CN 201210062636X A CN201210062636X A CN 201210062636XA CN 201210062636 A CN201210062636 A CN 201210062636A CN 102617655 A CN102617655 A CN 102617655A
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Abstract
The invention discloses a method for extracting oleuropein from canarium album raeusch fruits by utilizing a subcritical water extraction technology, and belongs to the technical field of separation of active ingredients from natural products. The method comprises the following steps of: performing extraction by taking pre-treated canarium album raeusch fruit flesh as a raw material and taking water as a solvent under the extraction pressure of 5 to 10 MPa and the extraction temperature of 200 to 270 DEG C for 20 to 60 minutes, performing cooling, filtration and concentration, performing separation and purification by using a macroporous resin chromatographic column, and performing vacuum concentration and freeze-drying on eluent to obtain an oleuropein product with the phenol content of over 85 percent. According to the extraction method, the use of an organic solvent is avoided; the method is clean, environment-friendly, simple in equipment, easy to operate, high in extraction speed and high in efficiency, and has broad industrial application prospect; and the product is natural and nontoxic.
Description
Technical field
The present invention relates to a kind of method of utilizing the Subcritical Water Extraction technology from olive fruits, to extract olive polyphenol, belong to the natural product active ingredient separation technology field.
Background technology
Olive (Canarium album Raeusch.) is the distinctive subtropical fruit tree in China south, mainly is distributed in the areas such as Guangdong, Fujian of China.Olive fruits is the traditional medicine-food two-purpose resource of China, has higher edible and pharmaceutical use.Olive polyphenol is as effective component important in the olive fruits; Has very strong anti-oxidant function; Its active promoting function to HUMAN HEALTH has caused that area research persons such as food, medicine pay close attention to widely, and the development and use research of olive polyphenol becomes focus wherein.
At present, the research of the industrialized developing of relevant olive polyphenol product is just risen, and mainly concentrates in recent years in the extraction separation research of olive polyphenol.The olive polyphenol process for extracting of having reported mainly contains hot water extraction, alkali extraction and acid precipitation, ethanolic soln extraction, methyl alcohol normal temperature extraction, ultrasonic auxiliary ethanol extraction method, microwave-assisted ethanol extraction method etc.All there is certain deficiency in this several method, and the product impurity that obtains like water extract method is many, the separation and purification difficulty; Normal temperature organic solvent method general extraction time is long, and efficient is not high; UW, microwave-assisted extraction method extraction time is short, and efficient is higher relatively, but crude extract purity is not high, brings certain difficulty for follow-up separation and purification work, and leaching process uses organic solvents such as a large amount of ethanol, methyl alcohol, has problems such as environmental protection.Therefore, seek environmental friendliness, the extractive technique method is the key issue that present olive polyphenol extraction field be badly in need of to solve more efficiently.
The sub-critical flow body technique is that last century Mo rises and just arrives a new technology of every field at rapid permeability.Wherein the research with subcritical water is the most extensive, and subcritical water both can be used as solvent, can be used as reactant and catalyzer again, makes it become chemical industry and food, the compelling technology of medicine field thereby this specific character can be used for substituting poisonous and hazardous organic solvent.Subcritical water also is referred to as high-temperature water, ultra adds hot water, high-pressure water heating or hot liquid water, is meant that under certain pressure water is heated to 100 ℃ with the high temperature below the upper critical temperature, and water body still remains on liquid state.Through can change polarity, surface tension and the viscosity of water to the control of subcritical water temperature and pressure.Temperature raises, and polarity reduces, and subcritical water increases organic dissolving power greatly.With subcritical water is environmentally friendly solvent; Can change phase behavior, the accelerated solvent effect of extraction system, the heterogeneous reaction that becomes under the conventional solvent condition is single reaction, increases spread coefficient; Than low mass transfer and heat transmission resistance; Can in shorter time, reach extraction equilibrium, shorten the treatment time, can also control the distribution of extracting product through the temperature and the pressure of subcritical system.And relevant subcritical water extractive technique is applied to the extraction research of olive polyphenol and does not appear in the newspapers as yet.
Therefore; In order to overcome the deficiency of present olive polyphenol extractive technique; This novel environmental type extractive technique of Subcritical Water Extraction technology is introduced in the research of olive polyphenol,, thereby realized extraction corresponding polarity olive polyphenol composition through the polarity of control Subcritical Water Extraction temperature and pressure and then control water; Reach and extract purposes such as efficient, that impurity is few, be convenient to obtain highly purified olive polyphenol product.
Summary of the invention
The object of the invention: propose the method that a kind of subcritical water extracts olive polyphenol.With fresh olive fruits is raw material, adopts the Subcritical Water Extraction technology to extract the polyphenolic compound in the olive, obtains the olive polyphenol crude extract, carries out further separation and purification through the macroporous resin chromatography again, obtains highly purified olive polyphenol product.
Technical scheme of the present invention: with the olive fruits is raw material; Raw material is carried out pre-treatment; Comprise cleaning, blanching, stoning, making beating, vacuum-drying, pulverizing etc., carry out polyphenol with Subcritical Water Extraction equipment then and extract that extracting liquid filtering is after concentrate; The separation and purification of last macroporous resin chromatography column, vacuum concentration, lyophilize obtain the olive polyphenol product, and said method specifically may further comprise the steps:
1, raw materials pretreatment: with the olive fresh fruit is raw material, and water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling, and broken stoning adds 1: 1 water making beating, and pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.
2, subcritical water extracts: olive pulp powder raw material is placed extraction kettle; Pump into deionized water with pump by 1: 20～1: 30 solid-liquid ratio; Control extracting pressure 5～10Mpa, 200～270 ℃ of extraction temperature, 20～60 minutes extraction time; Extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.
3, macroporous resin chromatography column separation and purification: the olive polyphenol extraction liquid is rotated evaporation concentration; Liquid concentrator is gone up the macroporous resin chromatography column again and is adsorbed; Successively the spirituous solution of water, 70-90% as eluent with the aldehydes matter separation and concentration; And, obtaining the olive polyphenol extract product through vacuum concentration, lyophilize, product phenols purity reaches more than 85%.
Beneficial effect of the present invention: the invention provides the method that a kind of subcritical water extracts olive polyphenol.Through Subcritical Water Extraction technology and the separation and purification of macroporous resin chromatography column, obtain highly purified olive polyphenol product.Leaching process of the present invention not with an organic solvent, the technological process environmental protection, operation of equipment is simple, is fit to suitability for industrialized production, has important pushing effect for the development and use of olive polyphenol active component.
Embodiment
Embodiment 1:
With the olive fresh fruit is raw material, and water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling, and broken stoning adds 1: 1 water making beating, and pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.Olive pulp powder is positioned in the extraction kettle, pumps into deionized water by 1: 20 solid-liquid ratio, control extracting pressure 5Mpa, 200 ℃ of extraction temperature, 20 minutes extraction time, extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.Extraction liquid concentrates through rotary evaporation; Last macroporous resin chromatography column adsorbs; Elder generation's water removes impurity such as desaccharification, albumen as eluent, aldehydes matter eluted as eluent with 70% spirituous solution again, and through vacuum concentration, lyophilize; Obtain solid-state olive polyphenol extract product, product phenols purity is 85%.
Embodiment 2:
With the olive fresh fruit is raw material, and water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling, and broken stoning adds 1: 1 water making beating, and pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.Olive pulp powder is positioned in the extraction kettle, pumps into deionized water by 1: 25 solid-liquid ratio, control extracting pressure 8Mpa, 230 ℃ of extraction temperature, 30 minutes extraction time, extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.Extraction liquid concentrates through rotary evaporation; Last macroporous resin chromatography column adsorbs; Elder generation's water removes impurity such as desaccharification, albumen as eluent, aldehydes matter eluted as eluent with 75% spirituous solution again, and through vacuum concentration, lyophilize; Obtain solid-state olive polyphenol extract product, product phenols purity is 87%.
Embodiment 3:
With the olive fresh fruit is raw material, and water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling, and broken stoning adds 1: 1 water making beating, and pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.Olive pulp powder is positioned in the extraction kettle, pumps into deionized water by 1: 30 solid-liquid ratio, control extracting pressure 10Mpa, 250 ℃ of extraction temperature, 60 minutes extraction time, extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.Extraction liquid concentrates through rotary evaporation; Last macroporous resin chromatography column adsorbs; Elder generation's water removes impurity such as desaccharification, albumen as eluent, aldehydes matter eluted as eluent with 80% spirituous solution again, and through vacuum concentration, lyophilize; Obtain solid-state olive polyphenol extract product, product phenols purity is 90%.
Embodiment 4:
With the olive fresh fruit is raw material, and water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling, and broken stoning adds 1: 1 water making beating, and pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.Olive pulp powder is positioned in the extraction kettle, pumps into deionized water by 1: 30 solid-liquid ratio, control extracting pressure 8Mpa, 270 ℃ of extraction temperature, 50 minutes extraction time, extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.Extraction liquid concentrates through rotary evaporation; Last macroporous resin chromatography column adsorbs; Elder generation's water removes impurity such as desaccharification, albumen as eluent, aldehydes matter eluted as eluent with 90% spirituous solution again, and through vacuum concentration, lyophilize; Obtain solid-state olive polyphenol extract product, product phenols purity is 89%.
Claims (1)
1. a subcritical water extracts the method for olive polyphenol; It is characterized in that with the olive fruits being raw material, raw material is carried out pre-treatment, comprise cleaning, blanching, stoning, making beating, vacuum-drying, pulverizing etc.; Carrying out polyphenol with Subcritical Water Extraction equipment then extracts; Extracting liquid filtering is after concentrated, and the separation and purification of last macroporous resin chromatography column, vacuum concentration, lyophilize obtain the olive polyphenol product, and said method comprises the steps:
(1) raw materials pretreatment: the fresh fruit with China olive subject plant olive Canarium album Raeusch. is a raw material; Water cleans up, and puts into the boiling water blanching 2～5min that contains 0.1% Hydrocerol A, cooling; Broken stoning; Add 1: 1 water making beating, pulp was pulverized 40 mesh sieves and was got olive pulp powder through vacuum-drying.
(2) subcritical water extracts: olive pulp powder raw material is placed extraction kettle; Pump into deionized water with pump by 1: 20～1: 30 solid-liquid ratio; Control extracting pressure 5～10Mpa, 200～270 ℃ of extraction temperature, 20～60 minutes extraction time; Extraction is opened pressure release valve after finishing, and is cooled to room temperature, obtains the olive polyphenol extraction liquid.
(3) macroporous resin chromatography column separation and purification: the olive polyphenol extraction liquid is rotated evaporation concentration; Liquid concentrator is gone up the macroporous resin chromatography column again and is adsorbed; Successively the spirituous solution of water, 70-90% as eluent with the aldehydes matter separation and concentration; And, obtaining the olive polyphenol extract product through vacuum concentration, lyophilize, product phenols purity is more than 85%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102935101A (en) * | 2012-12-10 | 2013-02-20 | 青岛海尔软件有限公司 | Extraction method of olive leaf polyphenol |
| CN103652945A (en) * | 2013-11-14 | 2014-03-26 | 江苏大学 | Subcritical water extraction on dietary fiber and preparation method of dietary fiber |
| CN104000935A (en) * | 2014-05-06 | 2014-08-27 | 浙江工商大学 | Method for extracting anti-oxidative phenolic acids from potato peel slag |
| CN104367611A (en) * | 2014-12-01 | 2015-02-25 | 江西师范大学 | Efficient preparation method for sweet potato leaf polyphenol |
| CN104490977A (en) * | 2014-11-28 | 2015-04-08 | 桂林市和胤祥新型材料有限公司 | Method for extracting olive polyphenol from olive leaves |
| CN104771930A (en) * | 2015-04-02 | 2015-07-15 | 江苏大学 | Subcritical water extraction agent and method for extracting polyphenol substances from lotus solid wastes |
| CN106668116A (en) * | 2016-12-27 | 2017-05-17 | 云南中烟工业有限责任公司 | Supercritical extraction method for improving oleuropein flavor quality |
| CN107177638A (en) * | 2017-05-19 | 2017-09-19 | 惠州嘉联生物科技开发有限公司 | The highly enriched fermentation process and its active product of Yunnan olive polyphenol |
| CN107308033A (en) * | 2017-05-22 | 2017-11-03 | 福建省亚热带植物研究所 | A kind of preparation method of olive fruits high-purity polyphenol and its application in cosmetics |
| CN108815401A (en) * | 2018-06-22 | 2018-11-16 | 江苏大学 | A kind of method of total polyphenols in Subcritical Water Extraction sorghum bran |
| CN111991432A (en) * | 2020-09-03 | 2020-11-27 | 昆明理工大学 | Method for extracting mango leaf polyphenol |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015333A (en) * | 2006-12-18 | 2007-08-15 | 江南大学 | Olive comprehensive utilization method |
-
2012
- 2012-03-12 CN CN201210062636XA patent/CN102617655A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101015333A (en) * | 2006-12-18 | 2007-08-15 | 江南大学 | Olive comprehensive utilization method |
Non-Patent Citations (3)
| Title |
|---|
| 何志勇: "橄榄酚类化合物的分离纯化和结构研究", 《工程科技I辑》 * |
| 赵健 等: "亚临界水萃取技术及其在食品方面的应用", 《食品工业科技》 * |
| 陈赟 等: "亚临界水萃取技术及其在天然产物分析中的应用", 《中药材》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102935101A (en) * | 2012-12-10 | 2013-02-20 | 青岛海尔软件有限公司 | Extraction method of olive leaf polyphenol |
| CN103652945B (en) * | 2013-11-14 | 2016-04-06 | 江苏大学 | Subcritical Water Extraction of a kind of dietary fiber and preparation method thereof |
| CN103652945A (en) * | 2013-11-14 | 2014-03-26 | 江苏大学 | Subcritical water extraction on dietary fiber and preparation method of dietary fiber |
| CN104000935A (en) * | 2014-05-06 | 2014-08-27 | 浙江工商大学 | Method for extracting anti-oxidative phenolic acids from potato peel slag |
| CN104000935B (en) * | 2014-05-06 | 2017-07-07 | 浙江工商大学 | A kind of method that anti-oxidant phenolic acid is extracted in the slag from jacket |
| CN104490977A (en) * | 2014-11-28 | 2015-04-08 | 桂林市和胤祥新型材料有限公司 | Method for extracting olive polyphenol from olive leaves |
| CN104367611A (en) * | 2014-12-01 | 2015-02-25 | 江西师范大学 | Efficient preparation method for sweet potato leaf polyphenol |
| CN104771930A (en) * | 2015-04-02 | 2015-07-15 | 江苏大学 | Subcritical water extraction agent and method for extracting polyphenol substances from lotus solid wastes |
| CN106668116A (en) * | 2016-12-27 | 2017-05-17 | 云南中烟工业有限责任公司 | Supercritical extraction method for improving oleuropein flavor quality |
| CN107177638A (en) * | 2017-05-19 | 2017-09-19 | 惠州嘉联生物科技开发有限公司 | The highly enriched fermentation process and its active product of Yunnan olive polyphenol |
| CN107308033A (en) * | 2017-05-22 | 2017-11-03 | 福建省亚热带植物研究所 | A kind of preparation method of olive fruits high-purity polyphenol and its application in cosmetics |
| CN108815401A (en) * | 2018-06-22 | 2018-11-16 | 江苏大学 | A kind of method of total polyphenols in Subcritical Water Extraction sorghum bran |
| CN111991432A (en) * | 2020-09-03 | 2020-11-27 | 昆明理工大学 | Method for extracting mango leaf polyphenol |
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Application publication date: 20120801 |