CN104547204A - Method for extracting polyphenol substances from litchi pericarp - Google Patents
Method for extracting polyphenol substances from litchi pericarp Download PDFInfo
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- CN104547204A CN104547204A CN201410752424.3A CN201410752424A CN104547204A CN 104547204 A CN104547204 A CN 104547204A CN 201410752424 A CN201410752424 A CN 201410752424A CN 104547204 A CN104547204 A CN 104547204A
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- litchi
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/77—Sapindaceae (Soapberry family), e.g. lychee or soapberry
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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Abstract
The invention relates to a method for extracting polyphenol substances from litchi pericarp, and belongs to the technical field of active substance extraction of agricultural products. The preparation method comprises the following steps: treating raw materials, extracting, purifying, drying and the like. According to the method, the polyphenol substances in the litchi pericarp are subjected to alcohol extraction by combination of low-temperature liquid nitrogen crushing and a surfactant serving as an assistant, so that the extraction rate on the polyphenol substances is improved; the extraction time is shortened; the extraction temperature is reduced; the activity of the polyphenol substances is kept; and the method is efficient in extraction process, free of pollution and low in cost.
Description
Technical field
The present invention relates to a kind of method extracting polyphenol substance, be specifically related to a kind of method extracting polyphenol substance from Fructus Litchi, belong to agricultural product active substance extractive technique field.
Background technology
Fructus Litchi is Sapindaceae, Fructus Litchi belongs to aiphyllium, it is tropical, that subtropical zone is important fruit tree, the cultivation history of more than 2000 year is had in China, cultivated area and output account for more than 80% of the world, be the maximum fruit tree of South China's cultivated area, be mainly distributed in the ground such as Guangdong, Guangxi, Fujian, Hainan and Taiwan.Because it is nutritious, the sweet meat of taste is tender, and quality is extremely excellent and be described as " treasure of China ".
In the suitability for industrialized production of Fructus Litchi, a large amount of Fructus Litchi does not obtain effective development and utilization as side-product, is usually used as garbage and abandons, and litchi rind also has very high biochemical activity in fact.CN201110339166.2 discloses a kind of Fructus Litchi extract and preparation method thereof and the application in Medicated cigarette.The present invention is first by petroleum ether backflow lixiviate litchi corium farinosum, collect the solid residue after backflow lixiviate, determine the enzymatic hydrolysis condition be suitable for, carry out enzymolysis to carrying residue at the beginning of Fructus Litchi and be further purified, obtained Fructus Litchi extract adds to after in Medicated cigarette, with the fragrance of Medicated cigarette with jealous there is good matching, contribute to the flavouring upgrading of Medicated cigarette, fall thorn remove impurity and reduce the burst size of harmful components, have certain facilitation to the lifting of Medicated cigarette integrated quality.CN201410180985.0 discloses a kind of preparation method of high-purity phloretin, take litchi rind as raw material, hot preparation litchi rind extracting solution is added with high-purity weak polar solvent, gained extracting solution contains aqueous two-phase extraction through liquid-liquid extraction, separation, the purification process step such as membrane technology separation, obtain high-purity phloretin.
Active component also containing picture polyphenol substance in Fructus Litchi.Plant polyphenol is the polyphenol compound that a class is extensively present in plant, content in vascular plant is only second to cellulose, hemicellulose and lignin, extensively be present in the skin of plant, root, leaf, fruit, there is antioxidation, strengthening blood vessel wall, promote gastrointestinal disturbances, reduce blood fat, with increase passive protective physical fitness, and prevent arteriosclerosis, thrombotic effect; Can also diuresis, blood pressure lowering, anti-bacteria and growth of cancer cells, and help digest, health care is good.CN200510093663.3 discloses a kind of method extracting lichee polyphenol from Fructus Litchi, it be a kind of with litchi rind and/or Semen Litchi for raw material, extract through extracting solvent, concentrated, separation and purification, dry extraction litchi rind polyphenol method, it using water or low-carbon alcohols if methanol, ethanol, propanol, isopropyl alcohol, butanols, amylalcohol etc. are as solvent; The method extracted adopts water or low-carbon alcohols heating extraction, also can adopt ultrasonic extraction or microwave extraction; Separation and purification can adopt column chromatographic isolation and purification.In extract, lichee polyphenol weight content is more than 70%, can effectively remove peroxidating material.But extraction process is complicated, and extraction ratio also needs to be further improved.
Summary of the invention
The present invention is directed to prior art Problems existing, a kind of method extracting polyphenol substance from Fructus Litchi is provided, the method is utilize low temperature liquid nitrogen to pulverize mating surface activating agent to assist polyphenol substance in alcohol extraction Fructus Litchi, reach improve polyphenol substance extraction ratio, reduce extraction time and temperature, the object of the activity of maintenance polyphenol substance, and leaching process is efficient, pollution-free, low cost.
In order to solve the problem, the technical solution adopted in the present invention is:
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, low temperature liquid nitrogen is pulverized, and crosses 80 ~ 120 mesh sieves;
B. extract: by litchi corium farinosum 5 ~ 9 parts, volume fraction is the alcoholic solution 20 ~ 30 parts of 60% ~ 80%, 0.1 ~ 0.5 part, surfactant, extract 60 ~ 90 minutes at 50 ~ 70 DEG C; Described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
Described steps A, the condition that low temperature liquid nitrogen is pulverized is nitrogen feed amount is 2 ~ 4mL/s, and Fructus Litchi inlet amount is 3 ~ 5g/s; Pulverizing temperature is-10 ~ 0 DEG C;
Described step B, surfactant is cationic surface active agent.
The present invention relative to the beneficial effect of prior art is:
(1) surfactant can by showing at it or the adsorption at interface or the molecule aggregation body that formed in the solution and change these compositions dissolubility in the solution, the extraction efficiency of material can be improved, reduce extraction cost, have save time, efficiently, electricity-saving lamp advantage, therefore surfactant plays an important role in assisted extraction active component.Low temperature liquid nitrogen crushing technology is mechanical crushing equipment under the state below cooled with liquid nitrogen to 0 DEG C by the operating unit of crushing material.Compared with other breaking methods, because nitrogen is produced by air separation, rich content, low production cost, pre-cooling required time is short, effectively can prevent Heat sensitive active composition recurring structure changeization ﹑ content in crushing process from falling low ﹑ effect and decline.。The present invention utilizes low temperature liquid nitrogen to pulverize mating surface activating agent and assists polyphenol substance in alcohol extraction Fructus Litchi, and adopt low temperature liquid nitrogen crushing technology to pulverize Fructus Litchi, reach improve polyphenol substance extraction ratio, reduce extraction time and temperature, the object of the activity of maintenance polyphenol substance, and leaching process is efficient, pollution-free, low cost.
(2) method extracting polyphenol substance from Fructus Litchi provided by the invention, than general ethanol extraction technology, the extraction ratio of polyphenol substance improves more than 40%, and the in vitro anti-oxidation of polyphenol substance is higher.
Accompanying drawing explanation
Fig. 1 surfactant Assisted Ethanol extracts the impact on polyphenol substance extraction ratio;
Fig. 2 surfactant Assisted Ethanol extracts the impact of polyphenol substance being removed to DPPH free radical.
Detailed description of the invention
Be described in further details the present invention below by embodiment, these embodiments are only used for the present invention is described, do not limit the scope of the invention.
embodiment 1
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, carries out low temperature liquid nitrogen pulverizing, and nitrogen feed amount is 2mL/s, and Fructus Litchi inlet amount is that 3g/s pulverizing temperature is-10 DEG C, crosses 80 mesh sieves after pulverizing;
B. extract: by litchi corium farinosum 5 parts, volume fraction is the alcoholic solution 20 parts of 60%, 0.1 part, surfactant, extract 60 minutes at 50 DEG C, number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
embodiment 2
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, carries out low temperature liquid nitrogen pulverizing, and nitrogen feed amount is 4mL/s, and Fructus Litchi inlet amount is 5g/s pulverizing temperature is 0 DEG C, crosses 120 mesh sieves after pulverizing;
B. extract: by litchi corium farinosum 9 parts, volume fraction is the alcoholic solution 30 parts of 80%, 0.5 part, surfactant, extract 90 minutes at 70 DEG C; Described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
embodiment 3
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, carries out low temperature liquid nitrogen pulverizing, and nitrogen feed amount is 3mL/s, and Fructus Litchi inlet amount is that 4g/s pulverizing temperature is-5 DEG C, crosses 100 mesh sieves after pulverizing;
B. extract: by litchi corium farinosum 7 parts, volume fraction is the alcoholic solution 25 parts of 70%, 0.3 part, surfactant, extract 75 minutes at 60 DEG C; Described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
embodiment 4
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, carries out low temperature liquid nitrogen pulverizing, and nitrogen feed amount is 2.5mL/s, and Fructus Litchi inlet amount is that 3.5g/s pulverizing temperature is-3 DEG C, crosses 90 mesh sieves after pulverizing;
B. extract: by litchi corium farinosum 6 parts, volume fraction is the alcoholic solution 23 parts of 65%, 0.2 part, surfactant, extract 65 minutes at 55 DEG C; Described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
embodiment 5
Extract a method for polyphenol substance from Fructus Litchi, comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, carries out low temperature liquid nitrogen pulverizing, and nitrogen feed amount is 3.5mL/s, and Fructus Litchi inlet amount is that 4.5g/s pulverizing temperature is-9 DEG C, crosses 110 mesh sieves after pulverizing;
B. extract: by litchi corium farinosum 8 parts, volume fraction is the alcoholic solution 27 parts of 75%, 0.35 part, surfactant, extract 80 minutes at 65 DEG C; Described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
embodiment 6
Naturally, after being dried by Fructus Litchi, mechanical activation comminution, crosses 80 mesh sieves; By litchi corium farinosum 5 parts, volume fraction is the alcoholic solution 20 parts of 60%, extracts 60 minutes (described number is parts by weight) at 50 DEG C; After recycling design, adopt column chromatographic isolation and purification; Eluent lyophilization powdered.Polyphenol substance extraction ratio (see figure 1) and scavenging ability of DPPH free radical (see figure 2) is compared with embodiment 1.Comparative result is known, and low temperature liquid nitrogen crushing technology and surfactant auxiliary extraction technology can make the extraction ratio of polyphenol substance improve more than 40%, and the in vitro anti-oxidation of polyphenol substance is higher.
Claims (3)
1. extract a method for polyphenol substance from Fructus Litchi, it is characterized in that: comprise the following steps:
A. Feedstock treating: after Fructus Litchi dries naturally, low temperature liquid nitrogen is pulverized, and crosses 80 ~ 120 mesh sieves;
B. extract: by litchi corium farinosum 5 ~ 9 parts, volume fraction is the alcoholic solution 20 ~ 30 parts of 60% ~ 80%, 0.1 ~ 0.5 part, surfactant, extract 60 ~ 90 minutes at 50 ~ 70 DEG C, described number is parts by weight;
C. purification: after recycling design, adopts column chromatographic isolation and purification;
D. dry: eluent lyophilization powdered.
2. a kind of method extracting polyphenol substance from Fructus Litchi according to claim 1, is characterized in that: the condition that the low temperature liquid nitrogen described in steps A is pulverized is nitrogen feed amount is 2 ~ 4mL/s, and Fructus Litchi inlet amount is 3 ~ 5g/s; Pulverizing temperature is-10 ~ 0 DEG C.
3. a kind of method extracting polyphenol substance from Fructus Litchi according to claim 1, is characterized in that: the surfactant described in step B is cationic surface active agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410752424.3A CN104547204A (en) | 2014-12-11 | 2014-12-11 | Method for extracting polyphenol substances from litchi pericarp |
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| CN201410752424.3A CN104547204A (en) | 2014-12-11 | 2014-12-11 | Method for extracting polyphenol substances from litchi pericarp |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722069A (en) * | 2017-10-31 | 2018-02-23 | 桂林纽泰生物科技有限公司 | The extraction process of litchi rind polyphenol |
| CN110652008A (en) * | 2019-11-08 | 2020-01-07 | 深圳市清生元生物技术股份有限公司 | Ultrasonic-assisted aqueous two-phase extraction method for litchi polyphenol |
-
2014
- 2014-12-11 CN CN201410752424.3A patent/CN104547204A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722069A (en) * | 2017-10-31 | 2018-02-23 | 桂林纽泰生物科技有限公司 | The extraction process of litchi rind polyphenol |
| CN110652008A (en) * | 2019-11-08 | 2020-01-07 | 深圳市清生元生物技术股份有限公司 | Ultrasonic-assisted aqueous two-phase extraction method for litchi polyphenol |
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