CN104367611A - Efficient preparation method for sweet potato leaf polyphenol - Google Patents
Efficient preparation method for sweet potato leaf polyphenol Download PDFInfo
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- CN104367611A CN104367611A CN201410710575.2A CN201410710575A CN104367611A CN 104367611 A CN104367611 A CN 104367611A CN 201410710575 A CN201410710575 A CN 201410710575A CN 104367611 A CN104367611 A CN 104367611A
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- China
- Prior art keywords
- rhizoma dioscoreae
- sweet potato
- extraction
- dioscoreae esculentae
- polyphenol
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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)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/894—Dioscoreaceae (Yam family)
- A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
-
- 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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
-
- 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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
-
- 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
Abstract
The invention relates to an efficient preparation method for sweet potato leaf polyphenol. The method includes: taking sweet potato leaves as raw materials, adopting subcritical water as extraction solvent, controlling the extraction temperature as 140-200 DEG C, extraction pressure as 4-10Mpa and extraction time as 30-120min, preparing rough sweet potato leaf polyphenol extract, and subjecting the rough sweet potato leaf polyphenol extract to centrifugation, concentration and macroporous resin separation and purification prior to vacuum freeze-drying to obtain a sweet potato leaf polyphenol product. The subcritical water is adopted for extraction, and polarity of water can be changed by changing the extraction temperature, so that the sweet potato leaf polyphenol can be extracted selectively, and polyphenol extraction efficiency is improved; as subcritical water extraction is adopted, pure water is used as the extraction solvent, toxic organic solvent is omitted, and no toxicity, environmental protection and safety are realized; high value-added processing of sweet potato leaf resources is realized; the production process and the technique are simple, and business development value is high.
Description
Technical field
The invention belongs to field of natural product extraction, particularly a kind of method efficiently preparing polyphenol from Rhizoma Dioscoreae esculentae leaf.
Background technology
Rhizoma Dioscoreae esculentae (
ipomoea batatas(L.) Lam), formal name used at school Ipomoea batatas Lam., has another name called Radix Ipomoeae, yam, is the seventh-largest cereal crops in the world, one of cereal crops that Ye Shi China is main.Rhizoma Dioscoreae esculentae leaf is one of side-product of Rhizoma Dioscoreae esculentae, and modern study shows that Rhizoma Dioscoreae esculentae leaf has the various health care functions such as antitumor, blood fat reducing, reduction cholesterol, scavenging free radicals, vision protection.In areas such as Japan, Taiwan, Rhizoma Dioscoreae esculentae leaf has become a kind of novel vegetable.Polyphenol, as active component main in Rhizoma Dioscoreae esculentae leaf, has very strong oxidation resistance, and it more and more causes the attention of people to the facilitation of health, and the development and utilization of Rhizoma Dioscoreae esculentae leaf polyphenol product also becomes the focus of modern study.
In prior art, the extracting method of Rhizoma Dioscoreae esculentae leaf polyphenol mainly contains: solvent extraction method, ultrasonic extraction, microwave loss mechanisms.But single extracting method efficiency is low, and inevitably uses organic solvent, has certain toxic.Subcritical water is between its boiling point and critical temperature (100-374 DEG C), and maintains the water of suitable pressure state, can change the polarity of water, surface tension and viscosity by controlling subcritical water pressure and temperature.Especially when the temperature increases, the dielectric constant of water increases, water is nonpolar by polarity transformation gradually, its character is more similar to organic solvent, Subcritical water chromotagraphy is widely used in byproduct for treatment and active components of plants extraction in recent years, and the research that relevant subcritical water technology is applied to the extraction of Rhizoma Dioscoreae esculentae leaf polyphenol has no report.
Therefore, the present invention is the shortcoming overcoming current Rhizoma Dioscoreae esculentae leaf polyphenol extractive technique deficiency, adopt a kind of efficient, environmentally friendly new technique, the polarity of water is controlled by controlling the extracting pressure of subcritical water and temperature, Rhizoma Dioscoreae esculentae leaf polyphenol solvability in water is improved greatly, and then raising extraction efficiency, and by purification by macroporous resin, to obtain the object of high-purity Rhizoma Dioscoreae esculentae leaf polyphenol.
Summary of the invention
The object of this invention is to provide a kind of new method utilizing subcritical water technology to extract Rhizoma Dioscoreae esculentae leaf polyphenol.The advantages such as it has extraction efficiency, purity is high, no solvent residue.
The present invention realizes like this, take Rhizoma Dioscoreae esculentae leaf as raw material, subcritical water technology is adopted to extract polyphenol from Rhizoma Dioscoreae esculentae leaf, the polyphenol extracting solution of gained is again through macroporous resin column chromatography separation and purification, vacuum concentration, lyophilization, obtain Rhizoma Dioscoreae esculentae leaf polyphenol product, and by LC-MS technology for detection product purity.
For solving the problems of the technologies described above, the present invention takes following technical scheme:
1, pretreatment of raw material: the fresh sweet potato leaf surface plucked is removed impurity, clear water rinsed clean, and 50 DEG C of forced air drying 48h, then pulverized 60 mesh sieves, obtained Rhizoma Dioscoreae esculentae leaf powder;
2, Subcritical water chromotagraphy: Rhizoma Dioscoreae esculentae leaf powder is put into subcritical water equipment, the solid-liquid ratio of powder and subcritical water is 1:15-1:30, control extracting pressure 4-10MPa, response time 30-120min, temperature is 140-200 DEG C, starting device, after end to be extracted, open pressure relief valve, obtain extracting solution;
3, be separated concentrated: by extracting solution centrifugal 10min under 4000rpm rotating speed, the supernatant obtained is 55 DEG C of 1/4-1/3 being evaporated to original volume in a rotary evaporator;
4, purification: adsorbed by macroporous resin chromatographic column on concentrated solution, then uses water and 70% ethanol elution successively, collects eluent;
5, dry: eluent concentrating under reduced pressure at 45 DEG C is become paste, and vacuum lyophilization obtains Rhizoma Dioscoreae esculentae leaf polyphenol product;
6, Product checking: product LC-MS carries out detection purity assay, its purity is all greater than 80%, and chromatograph packing material is C18, granularity 5 μm, mobile phase is methanol and the aqueous formic acid containing 0.1%, determined wavelength 320nm, flow velocity is 1 mL/min, and purity computing formula is as follows:
M in formula
1for the gross mass of the aldehydes matter that LC-MS in eluent detects, m
2for the quality of Rhizoma Dioscoreae esculentae leaf polyphenol product.
The present invention has the following advantages: (1) associating Subcritical Water Extraction technology and macroporous resin separating and purifying technology, and carry out high efficiency extraction and purification to Rhizoma Dioscoreae esculentae leaf polyphenol, products obtained therefrom purity is high, and extraction efficiency is apparently higher than conventional organic solvents; (2) whole leaching process avoids toxic organic solvents and uses, green and environmental protection, saves production cost, is applicable to being applied to commercial production, significant to the development and utilization of Rhizoma Dioscoreae esculentae leaf resource.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention.
Detailed description of the invention
Case study on implementation 1
The present invention is achieved like this, and its processing step is:
1, pretreatment of raw material: the fresh sweet potato leaf surface plucked is removed impurity, clear water rinsed clean, and 50 DEG C of forced air drying 48h, then pulverized 60 mesh sieves, obtained Rhizoma Dioscoreae esculentae leaf powder;
2, extract: Rhizoma Dioscoreae esculentae leaf powder is put into subcritical water equipment, and the solid-liquid ratio of powder and subcritical water is 1:20, control extracting pressure 5Mpa, response time 60min, temperature is 150 DEG C, and starting device after end to be extracted, is opened pressure relief valve, obtained extracting solution;
3, separation is concentrated: by extracting solution centrifugal 10min under 4000rpm rotating speed, 55 DEG C are evaporated to 1/4 of original volume in a rotary evaporator;
4, purification: adsorbed by macroporous resin chromatographic column on the concentrated solution of gained, then uses water and 70% ethanol elution successively, collects eluent;
5, dry: eluent concentrating under reduced pressure at 45 DEG C is become paste, and vacuum lyophilization obtains Rhizoma Dioscoreae esculentae leaf polyphenol product;
6, Product checking: product LC-MS carries out detection purity assay.
Case study on implementation 2
The present invention is achieved like this, and its processing step is:
1, pretreatment of raw material: the fresh sweet potato leaf surface plucked is removed impurity, clear water rinsed clean, and 50 DEG C of forced air drying 48h, then pulverized 60 mesh sieves, obtained Rhizoma Dioscoreae esculentae leaf powder;
2, extract: Rhizoma Dioscoreae esculentae leaf powder is put into subcritical water equipment, and the solid-liquid ratio of powder and subcritical water is 1:15, control extracting pressure 8Mpa, response time 80min, temperature is 180 DEG C, and starting device after end to be extracted, is opened pressure relief valve, obtained extracting solution;
3, be separated concentrated: by extracting solution centrifugal 10min under 4000rpm rotating speed, the supernatant obtained is evaporated to 1/3 of original volume at 55 DEG C of temperature in a rotary evaporator;
4, purification: adsorbed by macroporous resin chromatographic column on concentrated solution, then uses water and 70% ethanol elution successively, collects eluent;
5, dry: eluent concentrating under reduced pressure at 45 DEG C is become paste, and vacuum lyophilization obtains Rhizoma Dioscoreae esculentae leaf polyphenol product;
6, Product checking; Detection purity assay is carried out with LC-MS.
Case study on implementation 3
1, pretreatment of raw material: the fresh sweet potato leaf surface plucked is removed impurity, clear water rinsed clean, and 50 DEG C of forced air drying 48h, then pulverized 60 mesh sieves, obtained Rhizoma Dioscoreae esculentae leaf powder;
2, extract: Rhizoma Dioscoreae esculentae leaf powder is put into subcritical water equipment, and the solid-liquid ratio of powder and subcritical water is 1:30, control extracting pressure 10MPa, response time 40min, temperature is 200 DEG C, starting device, after end to be extracted, open pressure relief valve, obtain extracting solution;
3, be separated concentrated: by extracting solution centrifugal 10min under 4000rpm rotating speed, the supernatant obtained in a rotary evaporator 55 DEG C be evaporated to 1/4 of original volume;
4, purification: adsorbed by macroporous resin chromatographic column on concentrated solution, then uses water and 70% ethanol elution successively, collects eluent;
5, dry: eluent concentrating under reduced pressure at 45 DEG C is become paste, and vacuum lyophilization obtains Rhizoma Dioscoreae esculentae leaf polyphenol product;
6, Product checking: carry out detection purity assay with LC-MS.
Claims (2)
1. a high efficiency preparation method for Rhizoma Dioscoreae esculentae leaf polyphenol, is characterized in that:
(1) pretreatment of raw material: the fresh sweet potato leaf surface plucked is removed impurity, clear water rinsed clean, and 50 DEG C of forced air drying 48h, then pulverized 60 mesh sieves, obtained Rhizoma Dioscoreae esculentae leaf powder;
(2) Subcritical water chromotagraphy: Rhizoma Dioscoreae esculentae leaf powder is put into subcritical water equipment and extracts, after end to be extracted, open pressure relief valve, obtain extracting solution;
(3) be separated concentrated: by extracting solution centrifugal 10min under 4000rpm rotating speed, the supernatant obtained in a rotary evaporator 55 DEG C be evaporated to original volume 1/4-1/3;
(4) purification: adsorbed by macroporous resin chromatographic column on concentrated solution, then uses water and 70% ethanol elution successively, collects eluent;
(5) dry: eluent concentrating under reduced pressure at 45 DEG C is become paste, and vacuum lyophilization obtains Rhizoma Dioscoreae esculentae leaf polyphenol product;
(6) Product checking: product LC-MS carries out detection purity assay, its purity is all greater than 80%, and chromatograph packing material is C18, granularity 5 μm, and mobile phase is methanol and the aqueous formic acid containing 0.1%, determined wavelength 320 nm, and flow velocity is 1 mL/min; Purity computing formula is as follows:
M in formula
1for the gross mass of the aldehydes matter that LC-MS in eluent detects, m
2for the quality of Rhizoma Dioscoreae esculentae leaf polyphenol product.
2. the high efficiency preparation method of a kind of Rhizoma Dioscoreae esculentae leaf polyphenol as claimed in claim 1, it is characterized in that: described in step (2), the extraction conditions of Rhizoma Dioscoreae esculentae leaf powder in subcritical water is: the solid-liquid ratio of powder and subcritical water is 1:15-1:30, control extracting pressure 4-10MPa, response time 30min-120min, temperature is 140 DEG C-200 DEG C.
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| CN201410710575.2A CN104367611A (en) | 2014-12-01 | 2014-12-01 | Efficient preparation method for sweet potato leaf polyphenol |
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| CN201410710575.2A CN104367611A (en) | 2014-12-01 | 2014-12-01 | Efficient preparation method for sweet potato leaf polyphenol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (3)
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| CN101912696A (en) * | 2010-09-26 | 2010-12-15 | 祁鲲 | Subcritical extraction method using liquid ammonia as solvent |
| CN102617655A (en) * | 2012-03-12 | 2012-08-01 | 江南大学 | Method for subcritical water extraction of oleuropein |
| CN102746415A (en) * | 2012-07-28 | 2012-10-24 | 江南大学 | Method for simultaneously extracting tea polysaccharide and tea polyphenol with subcritical water |
-
2014
- 2014-12-01 CN CN201410710575.2A patent/CN104367611A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912696A (en) * | 2010-09-26 | 2010-12-15 | 祁鲲 | Subcritical extraction method using liquid ammonia as solvent |
| CN102617655A (en) * | 2012-03-12 | 2012-08-01 | 江南大学 | Method for subcritical water extraction of oleuropein |
| CN102746415A (en) * | 2012-07-28 | 2012-10-24 | 江南大学 | Method for simultaneously extracting tea polysaccharide and tea polyphenol with subcritical water |
Non-Patent Citations (1)
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| 李光 等: "响应曲面法优化红薯叶多酚提取工艺研究", 《广东农业科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Application publication date: 20150225 |