CN105535041A - Extraction method of total flavonoids in leaves of turpinia arguta seem - Google Patents
Extraction method of total flavonoids in leaves of turpinia arguta seem Download PDFInfo
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- 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)
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- 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
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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
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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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
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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Abstract
The invention provides an extraction method of total flavonoids in leaves of turpinia arguta seem. The extraction method is characterized by comprising the following steps: a, taking the leaves of the turpinia arguta seem and crushing the leaves for later use; b, carrying out ultrasonic extraction on medicinal powder with ethanol, and filtering an extracting solution so as to obtain the total flavonoids, wherein the ratio of liquid to materials is 20:1 to 30:1, the ethanol concentration is 40 to 60% v/v, the extraction temperature is 50-70 DEG C, and the extraction time is 40 to 60 minutes. The extraction process disclosed by the invention is easy and simple to operate, low in energy consumption and cost, good in reproducibility, and accurate and reliable in results, thereby providing a theoretical basis for further development of leaf resources of the turpinia arguta seem, and having very important significance to the development and application of the turpinia arguta seem.
Description
Technical field
The present invention relates to a kind of extracting method of leaf of Turpinia pomifera (Roxb) D O. total flavones.
Background technology
Leaf of Turpinia pomifera (Roxb) D O. is beaten also known as seven cun of nails, Turpinia arguta Seem, thousand, is the dried leaves of Staphyleaceae plant Turpinia pomifera(Roxb) D O. TurpiniaargutaSeem., originates in Southern Jiangxi area, is version " Chinese Pharmacopoeia " the local conventional crude drugs that records in 2015.This product is cold in nature, bitter in the mouth, has effect of heat-clearing and toxic substances removing, relieving sore throat and diminishing swelling, promoting blood circulation and stopping pain, is mainly used in the diseases such as treatment laryngopharynx swelling and pain, tonsillitis sore throat, sore swollen toxin.Modern study shows, total flavones is that it plays the main matter of curative effect, have antiinflammatory, antibacterial, strengthen the pharmacological actions such as immunity and analgesia.
At present, the extracting method of leaf of Turpinia pomifera (Roxb) D O. total flavones has: ethanol reflux extraction, microwave―assisted extraction, ethanol percolate extraction method.Zeng Xian, Chen Shihua, Deng. the research [J] of Turpinia pomifera(Roxb) D O. total flavone extracting process. R&D of modern TCM and practice, 2015,29 (5): 46-48 disclose a kind of extraction process adopting alcohol reflux restricted-access media Turpinia pomifera(Roxb) D O. total flavones, and its optimum extraction process is: Extracting temperature 60 DEG C, time 1.5h, volume fraction of ethanol 90%, solid-liquid ratio 1:50, extraction time 4 times.This extraction process solvent consumption is large, and length consuming time, energy consumption are large, production cost is high.Therefore, find a kind of easy and simple to handle, save energy consumption and cost, favorable reproducibility, result accurately and reliably the development and application tool of extraction process to leaf of Turpinia pomifera (Roxb) D O. be of great significance.
At present, the relevant report adopting ultrasonic extraction process to extract leaf of Turpinia pomifera (Roxb) D O. total flavones is had no.
Summary of the invention
Technical scheme of the present invention there is provided a kind of new process for extracting of leaf of Turpinia pomifera (Roxb) D O. total flavones.
The invention provides a kind of extracting method of leaf of Turpinia pomifera (Roxb) D O. total flavones: it comprises the steps:
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 20:1-30:1, and concentration of alcohol is 40-60%v/v, and Extracting temperature is 50-70 DEG C, and extraction time is 40-60min.
Preferably, liquid ratio is: 25:1.
Preferably, concentration of alcohol is 50%v/v.
Preferably, Extracting temperature is 50 DEG C.
Preferably, extraction time is 50min.
Present invention also offers extract prepared by said extracted method.
The present invention select from numerous influence factors of ultrasonic extraction process concentration of alcohol, liquid ratio, Extracting temperature, extraction time 4 factors investigate, filter out the optimal parameter scope of each factor, from each parameter area, random selecting parameter value combines, optimize optimum extraction process: concentration of alcohol 50%, liquid ratio 25:1, Extracting temperature 50 DEG C, extraction time 50min, with this understanding, leaf of Turpinia pomifera (Roxb) D O. total flavones extraction ratio is 3.34%.
Extraction process of the present invention is easy and simple to handle, solvent load is few, save energy consumption and cost, favorable reproducibility, result accurately and reliably, for the exploitation of going deep into further of leaf of Turpinia pomifera (Roxb) D O. resource is provided fundamental basis, the development and application tool of leaf of Turpinia pomifera (Roxb) D O. is of great significance.
Accompanying drawing explanation
Fig. 1 apigenin reference substance solution canonical plotting
Fig. 2 concentration of alcohol is on the impact of total flavones extraction ratio
Fig. 3 liquid ratio is on the impact of total flavones extraction ratio
Fig. 4 Extracting temperature is on the impact of total flavones extraction ratio
Fig. 5 extraction time is on the impact of total flavones extraction ratio
Below by way of detailed description of the invention, the present invention is described in further detail, but do not limit the present invention, the various change that those skilled in the art make according to the present invention and replacement, only otherwise depart from spirit of the present invention, all should belong to the scope of claims of the present invention.
Detailed description of the invention
Embodiment 1 extracting method of the present invention
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 25:1, and concentration of alcohol is 50%v/v, and Extracting temperature is 50 DEG C, and extraction time is 50min.
Embodiment 2 extracting method of the present invention
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 20:1, and concentration of alcohol is 40%v/v, and Extracting temperature is 50 DEG C, and extraction time is 40min.
Embodiment 3 extracting method of the present invention
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 30:1, and concentration of alcohol is 60%v/v, and Extracting temperature is 70 DEG C, and extraction time is 60min.
Embodiment 4 extracting method of the present invention
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 25:1, and concentration of alcohol is 40%v/v, and Extracting temperature is 60 DEG C, and extraction time is 50min.
Embodiment 5 extracting method of the present invention
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 25:1, and concentration of alcohol is 50%v/v, and Extracting temperature is 70 DEG C, and extraction time is 40min.
Beneficial effect of the present invention is proved below by way of specific experiment.
Experimental example 1
1 instrument and material
1.1 instrument UV-6100 ultraviolet-uisible spectrophotometers (Shanghai Mei Puda Instrument Ltd.);
PS-60A type ultrasonic cleaner (Chengdu Ya Rong experimental apparatus company limited, 40kHz, 350W); BP211DAG type electronic balance (100,000/, German Satorius); UPT-I-10T type Superpure water machine (Chengdu Ultra Pure Science & Technology Co., Ltd).
1.2 material apigenin reference substance (lot number MUST-15032610; Man Site bio tech ltd, Chengdu); Leaf of Turpinia pomifera (Roxb) D O. (purchased from Jiangxi QingFeng Pharmacy Co., Ltd); 95% ethanol (Chengdu Ke Long chemical reagent factory), all the other are analytical pure.
2 methods and result
2.1 surfactants-supersonic synergic extracting method
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, add the alcoholic solution of suitable concentration by fixed proportion, heat supersound extraction certain hour at a certain temperature, filter, obtain need testing solution.
The mensuration of 2.2 leaf of Turpinia pomifera (Roxb) D O. general flavone contents
2.2.1 the preparation of reference substance solution
Precision takes apigenin 5.10mg in 50mL measuring bottle, first adds that a small amount of methanol is ultrasonic makes dissolving, then with methanol constant volume to scale, shakes up, the solution of obtained 0.102mg/mL.
2.2.2 the selection of wavelength is measured
Dilute reference substance solution and need testing solution respectively, between 200 ~ 500nm, carry out length scanning, result shows: both all have absorption maximum at 268.5nm place, therefore selects 268.5nm for measuring wavelength.
2.2.3 the preparation of standard curve
Measure appropriate reference substance solution, be configured to the standard solution that mass concentration is 2.04 μ g/mL, 4.08 μ g/mL, 6.12 μ g/mL, 8.16 μ g/mL, 10.20 μ g/mL respectively, absorbance is measured in 268.5nm place, with standard substance mass concentration (C) for abscissa, absorbance (A) carries out linear regression (as Fig. 1) for vertical coordinate, obtain equation A=0.0767C+0.0288, r=0.9996.
2.2.4 the mensuration of total flavones
Measure extracting solution appropriate and be diluted to finite concentration, measure A value in 268.5nm wavelength place, according to the content of standard curve calculating leaf of Turpinia pomifera (Roxb) D O. total flavones.
2.3 concentration of alcohol are investigated
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, fixing liquid ratio 20:1, Extracting temperature 50 DEG C, extraction time 30min, add the ethanol that concentration is 30%, 40%, 50%, 60%, 70% respectively, extract leaf of Turpinia pomifera (Roxb) D O. total flavones with this understanding, extraction ratio result is as Fig. 2.
Result shows, along with the increase of concentration of alcohol, total flavones extracts and takes the lead in increasing rear reduction, the highest with 50% total ethanol extracting flavonoids rate.
2.4 liquid ratios are investigated
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, fixing concentration of alcohol 50%, Extracting temperature 50 DEG C, extraction time 30min, investigates liquid ratio 10:1,15:1,20:1,25:1,30:1, and extract leaf of Turpinia pomifera (Roxb) D O. total flavones with this understanding, extraction ratio result is as Fig. 3.
Result shows, along with the increase of solvent load, total flavones extracts and takes the lead in increasing rear reduction, the highest with liquid ratio 25:1 total flavones extraction ratio.
2.5 Extracting temperature are investigated
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, fixing concentration of alcohol 50%, liquid ratio 25:1, extraction time 30min, investigates different Extracting temperature 40,50,60,70,80 DEG C, and extract leaf of Turpinia pomifera (Roxb) D O. total flavones with this understanding, extraction ratio result is as Fig. 4.
Result shows, along with the rising of temperature, total flavones extraction ratio increases gradually, and when temperature reaches after 60 DEG C, the trend that extraction ratio increases obviously slows down.
2.6 extraction times were investigated
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, fixing concentration of alcohol 50%, liquid ratio 25:1, Extracting temperature 60 DEG C, investigate different extraction time 20,30,40,50,60min, extract leaf of Turpinia pomifera (Roxb) D O. total flavones with this understanding, extraction ratio result is as Fig. 5.
Result shows, when extraction time is 50min, leaf of Turpinia pomifera (Roxb) D O. total flavones extraction ratio is maximum.
Test draws, concentration of alcohol optimum range: 40-60%, liquid ratio optimum range: 20:1-30:1, Extracting temperature optimum range: 50-70 DEG C, extraction time optimum range: 40-60min.
2.7 leaf of Turpinia pomifera (Roxb) D O. total flavone extracting process are optimized
1 laboratory sample
Within the scope of the optimal parameter of concentration of alcohol, liquid ratio, Extracting temperature, extraction time, random selecting parameter value combines, and obtains following sample:
Sample 1: concentration of alcohol 40%, liquid ratio 20:1, Extracting temperature 50 DEG C, extraction time 40min
Sample 2: concentration of alcohol 40%, liquid ratio 25:1, Extracting temperature 60 DEG C, extraction time 50min
Sample 3: concentration of alcohol 40%, liquid ratio 30:1, Extracting temperature 70 DEG C, extraction time 60min
Sample 4: concentration of alcohol 50%, liquid ratio 20:1, Extracting temperature 60 DEG C, extraction time 60min
Sample 5: concentration of alcohol 50%, liquid ratio 25:1, Extracting temperature 70 DEG C, extraction time 40min
Sample 6: concentration of alcohol 50%, liquid ratio 30:1, Extracting temperature 50 DEG C, extraction time 50min
Sample 7: concentration of alcohol 60%, liquid ratio 20:1, Extracting temperature 70 DEG C, extraction time 50min
Sample 8: concentration of alcohol 60%, liquid ratio 25:1, Extracting temperature 50 DEG C, extraction time 60min
Sample 9: concentration of alcohol 60%, liquid ratio 30:1, Extracting temperature 60 DEG C, extraction time 40min
Sample 10: concentration of alcohol 50%, liquid ratio 25:1, Extracting temperature 50 DEG C, extraction time 50min
2 experimental procedures:
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 1.00g, carry out supersound extraction according to above-mentioned process conditions, calculate leaf of Turpinia pomifera (Roxb) D O. total flavones extraction ratio.
3 experimental results, in table 1.
Table 1 leaf of Turpinia pomifera (Roxb) D O. total flavones extraction ratio
Experimental result shows that the extraction efficiency of sample 10 is the highest, and energy consumption is saved, cost is low, determines that optimum extraction process is: concentration of alcohol 50%, liquid ratio 25:1, Extracting temperature 50 DEG C, extraction time 50min.
4 demonstration tests
Take leaf of Turpinia pomifera (Roxb) D O. coarse powder 3 parts, every part of 1.00g, extract total flavones by above-mentioned optimised process, carry out 3 batches of demonstration tests, result is as table 2.
Table 2 demonstration test result
As seen from the experiment, the total flavones average recoveries of three batches of tests is 3.34%, RSD < 2.0%, and show that the extraction process of screening is stablized feasible, repeatability is good, can carry out the extraction of leaf of Turpinia pomifera (Roxb) D O. total flavones.
To sum up, the present invention investigates Extraction technique, obtain best extraction process, with this understanding, leaf of Turpinia pomifera (Roxb) D O. total flavones extraction ratio is obviously better than other conditions of supersound extraction, illustrate that liquid ratio, concentration of alcohol, extraction time and Extracting temperature are not more high better, find the best of breed scheme of multiple conditional parameter can save energy consumption and cost, best extraction effect can be reached again.Extraction process of the present invention is easy and simple to handle, save energy consumption and cost, favorable reproducibility, result accurately and reliably, for the exploitation of going deep into further of leaf of Turpinia pomifera (Roxb) D O. resource is provided fundamental basis, the development and application tool of leaf of Turpinia pomifera (Roxb) D O. is of great significance.
Claims (6)
1. the extracting method of a leaf of Turpinia pomifera (Roxb) D O. total flavones: it is characterized in that: it comprises the steps:
A, get leaf of Turpinia pomifera (Roxb) D O. pulverize after, for subsequent use;
B, medicated powder is carried out supersound extraction with ethanol, extracting liquid filtering, to obtain final product; Wherein, liquid ratio is 20:1-30:1, and concentration of alcohol is 40-60%v/v, and Extracting temperature is 50-70 DEG C, and extraction time is 40-60min.
2. extracting method according to claim 1, is characterized in that: liquid ratio is: 25:1.
3. extracting method according to claim 1, is characterized in that: concentration of alcohol is 50%v/v.
4. extracting method according to claim 1, is characterized in that: Extracting temperature is 50 DEG C.
5. extracting method according to claim 1, is characterized in that: extraction time is 50min.
6. the extract that described in claim 1-5 any one prepared by extracting method.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279459A (en) * | 2016-08-25 | 2017-01-04 | 湖南中医药大学 | The extracting method of polysaccharide and application thereof in a kind of leaf of Turpinia pomifera (Roxb) D O. |
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| CN101862357A (en) * | 2010-04-13 | 2010-10-20 | 江西山香药业有限公司 | Acute turpinia leaf general flavone ethanol reflux extract, and preparation method and application thereof |
| CN102920751A (en) * | 2010-04-13 | 2013-02-13 | 江西山香药业有限公司 | Turpinia arguta leaf total flavonoid ethanol reflux extract, preparation method and uses thereof |
| CN102935098A (en) * | 2010-04-13 | 2013-02-20 | 江西山香药业有限公司 | Acute turpinia leaf general flavone ethanol reflux extract, and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101862357A (en) * | 2010-04-13 | 2010-10-20 | 江西山香药业有限公司 | Acute turpinia leaf general flavone ethanol reflux extract, and preparation method and application thereof |
| CN102920751A (en) * | 2010-04-13 | 2013-02-13 | 江西山香药业有限公司 | Turpinia arguta leaf total flavonoid ethanol reflux extract, preparation method and uses thereof |
| CN102935098A (en) * | 2010-04-13 | 2013-02-20 | 江西山香药业有限公司 | Acute turpinia leaf general flavone ethanol reflux extract, and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279459A (en) * | 2016-08-25 | 2017-01-04 | 湖南中医药大学 | The extracting method of polysaccharide and application thereof in a kind of leaf of Turpinia pomifera (Roxb) D O. |
| CN106279459B (en) * | 2016-08-25 | 2018-09-04 | 湖南中医药大学 | The extracting method of polysaccharide and its application in a kind of acute turpinia leaf |
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Application publication date: 20160504 |