CN102988605A - Method for extracting lycium barbarum extract by supercritical CO2 - Google Patents
Method for extracting lycium barbarum extract by supercritical CO2 Download PDFInfo
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- CN102988605A CN102988605A CN2012104596236A CN201210459623A CN102988605A CN 102988605 A CN102988605 A CN 102988605A CN 2012104596236 A CN2012104596236 A CN 2012104596236A CN 201210459623 A CN201210459623 A CN 201210459623A CN 102988605 A CN102988605 A CN 102988605A
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- extraction
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- plant extract
- lycium barbarum
- lycium
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to an extraction method for lycium barbarum polysaccharide, and particularly relates to a method for extracting a lycium barbarum extract by supercritical CO2, which is used for achieving the purpose of high-efficiency extraction for lycium barbarum polysaccharide. The method comprises the following steps of: a, drying and crushing lycium barbarum, and then placing the lycium barbarum in an extraction kettle; b, injecting CO2 in a supercritical state in the extraction kettle, and extracting for 3.5-4.5 hours in the conditions of a temperature of 45-55 DEG C, a pressure of 1.2-2.0 Mpa and a CO2 flow velocity of 0.10-0.15 L/min; and c, conveying a CO2 fluid dissolved with the lycium barbarum plant extract in a separation kettle to separate a CO2 gas, compressing the CO2 gas, and then conveying the CO2 gas in the extraction kettle for cycle use. The content of lycium barbarum polysaccharide in the lycium barbarum plant extract obtained by extraction adopting the method for extracting a lycium barbarum extract by supercritical CO2 is up to 17%.
Description
Technical field
The present invention relates to a kind of extracting method of lycium barbarum polysaccharide, particularly a kind of supercritical CO
2The method of extraction wolfberry fruit extract.
Background technology
Dry mature fruit for the plant Fructus Lycii.Ovalize or cylindrical, two ends are point slightly, and long 1-1.5 centimetre, diameter 3-5 millimeter.Surface cerise or kermesinus, the irregular wrinkle of tool, tarnish.Matter is soft and slightly moisten, built-in most seeds, in most amber seeds are arranged, flat like kidney-shaped.Fructus Lycii is famous and precious medical material and tonic, edible or make Fructus Lycii tea.Modern study, Fructus Lycii have blood sugar lowering, lipotropy, and can atherosclerosis.Contain a small amount of precious function nutrition composition lycium barbarum polysaccharide in the Fructus Lycii, can't be soluble in water, can not well keep, can well keep this part function nutrition material in the wolfberry fruit extract how to obtain is the emphasis of our current research.Disclose a lot of technical literatures in the prior art, passed through supercritical CO
2The extraction Fructus Lycii obtains different extracts, application number: 200410080382.X provides a kind of method of extracting active component from Chinese wolfberry fruit.Extract in addition pigment, carotene, Fructus Lycii wet goods technology.Existing lycium barbarum polysaccharide is extracted the research field that mainly concentrates on water extraction and alcohol extraction and column chromatography extraction etc., and extraction ratio is not high.
Summary of the invention
The problem that the present invention extracts for the high efficiency that solves lycium barbarum polysaccharide provides a kind of supercritical CO
2The method of extraction wolfberry fruit extract.
Technical scheme of the present invention is a kind of supercritical CO
2The method of extraction lycium plant extract, step is as follows:
A, will put into extraction kettle after the Fructus Lycii drying and crushing;
B, with the CO of supercriticality
2Injecting extraction kettle, is 45～55 ℃ in temperature, and pressure is 1.2～2.0Mpa, CO
2Flow velocity is: under the condition of 0.10～0.15L/min, extract 3.5～4.5 hours;
C, be dissolved with the CO of lycium plant extract
2Fluid enters separating still, the lycium plant extract is separated CO by regulating 48-60 ℃ of temperature and pressure 2.0Mpa～3.0Mpa
2Gas enters after compression extraction kettle and recycles.
Above-mentioned supercritical CO
2The method of extraction lycium plant extract, wherein, described supercritical CO
2The preferred temperature of extraction is 50 ℃, and pressure is 1.7Mpa, CO
2Flow velocity is 0.12L/min.
The method of above-mentioned SCF-CO 2 lycium plant extract, wherein, described drying is carried out in temperature is lower than 80 ℃ baking oven, and dry 1.5～2 hours, the Fructus Lycii moisture after the drying was lower than 10%.
Above-mentioned supercritical CO
2The method of extraction lycium plant extract, the content of the lycium barbarum polysaccharide in the lycium plant extract of extraction gained reaches 17%.
Supercritical CO of the present invention
2The method of extraction lycium plant extract first with the Fructus Lycii drying and crushing, has overcome because the Fructus Lycii appearance is hard CO before extracting
2Fluid can't penetrate its appearance and the incomplete defective of extraction that causes, has increased Fructus Lycii and CO
2The contact area of fluid was pulverized Fructus Lycii 40 mesh sieves simultaneously, and its granularity is just so that CO
2Fluid is circulate in extraction process, contacts more fully with Fructus Lycii, thereby has further improved the extraction efficiency of lycium plant extract.
Supercritical CO of the present invention
2Used CO in the method for extraction lycium plant extract
2Purity is more than or equal to 99%, CO
2Be noble gas, can operate at normal temperatures, can effectively prevent oxidation and the decomposition of thermal sensitivity composition and chemically unstable composition, utilize CO
2Be in the large character of the high density, low viscosity and the diffusion coefficient that have under the supercriticality and extract effective ingredient in the Fructus Lycii, then will be dissolved in CO in the method that heats up with blood pressure lowering
2Solute in the fluid separates, and plays the dual function that extracts and distill, and can finish a leaching process in 2.5～4 hours.The method operation cycle is short, extraction efficiency is high, can avoid the residual of organic solvent simultaneously, in addition, because CO
2Cheap and easy to get, general recyclable about 80%, saved the energy, simultaneously because CO
2Without flammability, use safety and environmentally safe.
Supercritical CO of the present invention
2The method technique of extraction lycium plant extract is simple, easy to operate, greatly improved production efficiency, lycium plant extract with the method extraction, avoided the residual of organic solvent, shortened extraction time, improve the extraction efficiency of Fructus Lycii, especially greatly improved the content of lycium barbarum polysaccharide in the lycium plant extract.The content of the lycium barbarum polysaccharide in the lycium plant extract of extraction gained reaches 17%, and effect of extracting is obvious.
The specific embodiment
The plant extract object detecting method
Instrument and reagent
Instrument: ultraviolet-visible spectrophotometer
Reagent: 5% phenol solution, concentrated sulphuric acid, alcoholic solution
Sample determination
1. the reference substance solution preparation is accurate takes by weighing 105 ℃ of about 50mg of anhydrous glucose that are dried to constant weight, puts in the 50mL volumetric flask, and standardize solution is dissolved in water.
2. the preparation precision of standard curve is measured reference substance solution 1.0,2.0,3.0,4.0,5.0mL and is placed respectively the 50mL volumetric flask, adds the water standardize solution, is the reference substance test liquid.Respectively get reference substance test liquid 1.0mL in 25mL tool plug scale test tube in addition, add respectively 5% phenol solution 1.0mL, shake up, add concentrated sulphuric acid 5.0mL and (when adding concentrated sulphuric acid, do not add along wall.Pipet should be suspended from the test tube mouth makes concentrated sulphuric acid vertically pour liquid level), shake up immediately.In boiling water bath, heat 10min, take out in the rearmounted ice-water bath cooling and be placed to room temperature.Do reference with reagent blank and measure trap at the wavelength place of 485nm, take trap as vertical coordinate, concentration (ug/mL) is abscissa, the drawing standard curve.
3. the preparation precision of sample solution takes by weighing the about 300mg of lycium barbarum polysaccharide sample, put in the 100mL volumetric flask, add alcoholic solution 80mL, sonic oscillation 60min is placed to room temperature, filter, residue washes residue in the former 100mL volumetric flask with a small amount of boiling water after washing 2～3 times with alcoholic solution, adds altogether about 80mL of boiling water, sonic oscillation 60min dissolving is placed to the room temperature standardize solution.Shake up filtration, get subsequent filtrate 2.0mL and put the 50mL volumetric flask and add the water standardize solution, be test sample solution.By operating under the standard curve preparation, try to achieve the test sample solution concentration by standard curve.
The result calculates
In the formula: P: sample liquid concentration of glucose (ug/ml)
D: diluted sample factor
F: conversion factor
M: sample quality (ug)
Embodiment 1, below in conjunction with example the present invention is described in detail.
Supercritical CO
2The method of extraction lycium plant extract, wherein, the step of described method is as follows: Fructus Lycii was dried by the fire 1.5 hours in 80 ℃ baking oven, Fructus Lycii water content after the drying is 10%, dried Fructus Lycii was pulverized 40 mesh sieves, and the Fructus Lycii after then will sieving is put into supercritical extraction reactor and extracts.Be 50 ℃ in temperature, pressure is 1.7Mpa, CO
2Flow velocity is under the condition of 0.12L/min, extracts 4 hours, and the lycium plant extract is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Lycium plant extract in the fluid is separated CO
2Recycle.
Detect the effective ingredient in the lycium plant extract, the content of the lycium barbarum polysaccharide in the lycium plant extract of this technique extraction gained is:
Embodiment 2, supercritical CO
2The method of extraction lycium plant extract, wherein, the step of described method is as follows: Fructus Lycii was dried by the fire 2 hours in 70 ℃ baking oven, and the Fructus Lycii water content after the drying is 6%, dried Fructus Lycii was pulverized 40 mesh sieves, and the Fructus Lycii after then will sieving is put into supercritical extraction reactor and extracts.Be 45 ℃ in temperature, pressure is 2.0Mpa, CO
2Flow velocity is under the condition of 0.10L/min, extracts 4 hours, and the lycium plant extract is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Lycium plant extract in the fluid is separated CO
2Recycle.
Detect the effective ingredient in the lycium plant extract, the content of the lycium barbarum polysaccharide in the lycium plant extract of this technique extraction gained is: 17.1%.
Embodiment 3
Supercritical CO
2The method of extraction lycium plant extract, wherein, the step of described method is as follows: Fructus Lycii was dried by the fire 1.7 hours in 70 ℃ baking oven, Fructus Lycii water content after the drying is 5%, dried Fructus Lycii was pulverized 40 mesh sieves, and the Fructus Lycii after then will sieving is put into supercritical extraction reactor and extracts.Be 55 ℃ in temperature, pressure is 1.2Mpa, CO
2Flow velocity is under the condition of 0.15L/min, extracts 2.5 hours, and the lycium plant extract is dissolved in supercritical CO
2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making
2Lycium plant extract in the fluid is separated CO
2Recycle.
Detect the effective ingredient in the lycium plant extract, the content of the lycium barbarum polysaccharide in the lycium plant extract of this technique extraction gained is: 17.2%.
Here description of the invention and application is illustrative, is not to want that therefore, the present invention is not subjected to the restriction of present embodiment with scope restriction of the present invention in the above-described embodiments, and the technical scheme that the replacements such as any employing obtain is all in the scope of protection of the invention.
Claims (4)
1. supercritical CO
2The method of extraction lycium plant extract is characterized in that step is as follows:
A, will put into extraction kettle after the Fructus Lycii drying and crushing;
B, with the CO of supercriticality
2Injecting extraction kettle, is 45～55 ℃ in temperature, and pressure is 1.2～2.0Mpa, CO
2Flow velocity is: under the condition of 0.10～0.15L/min, extract 3.5～4.5 hours;
C, be dissolved with the CO of lycium plant extract
2Fluid enters separating still, the lycium plant extract is separated CO by regulating 48-60 ℃ of temperature and pressure 2.0Mpa～3.0Mpa
2Gas enters after compression extraction kettle and recycles.
2. supercritical CO according to claim 1
2The method of extraction lycium plant extract is characterized in that described supercritical CO
2The preferred temperature of extraction is 50 ℃, and pressure is 1.7Mpa, CO
2Flow velocity is 0.12L/min.
3. supercritical CO according to claim 1
2The method of extraction lycium plant extract is characterized in that, described drying is carried out in temperature is lower than 80 ℃ baking oven, and dry 1.5～2 hours, the Fructus Lycii moisture after the drying was lower than 10%.
4. supercritical CO according to claim 1
2The method of extraction lycium plant extract is characterized in that Fructus Lycii was pulverized 40 mesh sieves.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356683A (en) * | 2014-10-23 | 2015-02-18 | 西安莹朴生物科技股份有限公司 | Preparation method of wolfberry red pigment |
| CN104623095A (en) * | 2015-02-11 | 2015-05-20 | 唐泽光 | Extraction method for FructusLycii active ingredient |
| CN106317243A (en) * | 2016-08-30 | 2017-01-11 | 宁夏沃福百瑞枸杞产业股份有限公司 | Preparation method of lycium barbarum polysaccharides |
| CN109662938A (en) * | 2019-02-14 | 2019-04-23 | 重庆市洲仨科技发展有限公司 | A kind of plant polyose moisturizing factor and the preparation method and application thereof |
| CN112931813A (en) * | 2021-02-24 | 2021-06-11 | 中国热带农业科学院农产品加工研究所 | Polysaccharide dry pulp superfine powder and preparation method thereof |
| CN115364014A (en) * | 2022-09-02 | 2022-11-22 | 广州弗恩生物科技有限公司 | Multi-effect moisturizing factor and preparation method thereof |
| CN115813999A (en) * | 2022-11-16 | 2023-03-21 | 南京农业大学 | Method for preparing anhydrous chrysanthemum and wolfberry puree based on polysaccharide extraction |
-
2012
- 2012-11-15 CN CN2012104596236A patent/CN102988605A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356683A (en) * | 2014-10-23 | 2015-02-18 | 西安莹朴生物科技股份有限公司 | Preparation method of wolfberry red pigment |
| CN104623095A (en) * | 2015-02-11 | 2015-05-20 | 唐泽光 | Extraction method for FructusLycii active ingredient |
| CN106317243A (en) * | 2016-08-30 | 2017-01-11 | 宁夏沃福百瑞枸杞产业股份有限公司 | Preparation method of lycium barbarum polysaccharides |
| CN109662938A (en) * | 2019-02-14 | 2019-04-23 | 重庆市洲仨科技发展有限公司 | A kind of plant polyose moisturizing factor and the preparation method and application thereof |
| CN112931813A (en) * | 2021-02-24 | 2021-06-11 | 中国热带农业科学院农产品加工研究所 | Polysaccharide dry pulp superfine powder and preparation method thereof |
| CN115364014A (en) * | 2022-09-02 | 2022-11-22 | 广州弗恩生物科技有限公司 | Multi-effect moisturizing factor and preparation method thereof |
| CN115813999A (en) * | 2022-11-16 | 2023-03-21 | 南京农业大学 | Method for preparing anhydrous chrysanthemum and wolfberry puree based on polysaccharide extraction |
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Application publication date: 20130327 |