CN109865005A - A kind of extraction process of Ammonium alum method leaf flavonoids - Google Patents
A kind of extraction process of Ammonium alum method leaf flavonoids Download PDFInfo
- Publication number
- CN109865005A CN109865005A CN201910237744.8A CN201910237744A CN109865005A CN 109865005 A CN109865005 A CN 109865005A CN 201910237744 A CN201910237744 A CN 201910237744A CN 109865005 A CN109865005 A CN 109865005A
- Authority
- CN
- China
- Prior art keywords
- ammonium alum
- alum method
- general flavone
- leaf
- method leaf
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of extraction processes of Ammonium alum method leaf flavonoids, comprising the following steps: Step 1: the preparation of Ammonium alum method leaf dried powder；Step 2: the extraction of Ammonium alum method leaf flavonoids；Step 3: the calculating of Ammonium alum method leaf flavonoids yield；Step 4: Ammonium alum method leaf extracts the fractional extraction of concentrate.Ammonium alum method leaf flavonoids extraction process provided by the invention has easy to operate, various solvents used are all recyclable to be used again, it is at low cost, general flavone can be carried out a degree of enrichment by fractional extraction, facilitate the further exploitation of Ammonium alum method leaf flavonoids, the present invention provides a reference for the development and utilization of Ammonium alum method resource.
Description
Technical field
The present invention relates to a kind of extraction process of Ammonium alum method leaf, it is more particularly related to which a kind of use water as molten
The extraction process of agent extraction Ammonium alum method leaf flavonoids.
Background technique
Ammonium alum method also known as banyan tree, Huang Geshu are one of Moraceae Ficus class plants.Originate in Southwestern China, south China
Area, it is in the majority with Sichuan, Chongqing region.Ammonium alum method is flourishing, and vitality is indomitable, high temperature resistant but also can not only keep out the cold.Banyan
Leaf has the medicinal efficacies such as antibacterial, anti-inflammatory, inducing diaphoresis, heat-clearing and dampness elimination, can be used for bronchitis, asthma, malaria, cough, acute
The prevention and treatment of the diseases such as enteritis and bacillary dysentery." medium-height grass pharmacological property is standby to be wanted " and " national Chinese herbal medicine compilation " all have recorded Moraceae Ficus
The medical value of plant Ammonium alum method leaf, dispelling wind and removing obstruction in the meridians, activating blood circulation and reducing swelling, antipruritic sore.Cure mainly arthralgia and myalgia, tearing against wind skin
Itch, ulcer on the shank, traumatic injury and fracture.Studies have shown that smallfruit fig leaf glycosides containing triterpene, flavonoid glycoside, acidic resins and tannin etc..Flavones
The effective components such as class and terpene lactones are in treatment cardiovascular and cerebrovascular disease, the nervous system disease and eliminate free radical, antibacterial, anticancer etc.
Aspect has remarkable result.Flavone compound is using 2- phenyl chromone as the polyphenols of mother nucleus structure, as plant
Secondary metabolite is present in various plants with glycoside forms mostly.Flavone compound pharmacological action is significant, have antibacterial,
Anti-inflammatory, decompression, anti-oxidant, anti-mutation, anticancer, calmness, it is clearing heat and detoxicating the effects of, be widely used in field of medicaments.
Summary of the invention
It is an object of the present invention to provide a kind of extraction processes of Ammonium alum method leaf flavonoids.
In order to realize purpose according to the present invention, a kind of extraction process of Ammonium alum method leaf flavonoids is provided, including following
Step:
Step 1: Ammonium alum method leaf is cleaned, crushed after being dried, 20~100 meshes are crossed, Ammonium alum method leaf coarse powder is obtained；
Step 2: according to Ammonium alum method leaf coarse powder quality (g): water volume (mL) is that deionization is added in the solid-liquid ratio of 1:20~80
Water carries out the refluxing extraction that bath temperature is 50~95 DEG C of 0.5~10.0h by a definite date；
Step 3: extracting solution filters while hot, 1/5th of original volume are concentrated under reduced pressure into, 95% second of two volumes is added
Alcohol is stood overnight, and next day filtering measures absorbance value, calculates general flavone yield after taking filtrate to develop the color.
Step 4: concentrating filtrate to the 10% of original volume, petroleum ether, ethyl acetate and the positive fourth of water saturation are successively used
Alcohol is successively extracted as extractant, is compared to each section extract liquor absorbance value, and discovery water-saturated n-butanol extracts part
The content of middle general flavone is maximum.
In the extraction process of above-mentioned Ammonium alum method leaf flavonoids, it is preferred that in the step 2, it is dry to accurately weigh Ammonium alum method leaf
500mL deionized water, the refluxing extraction 2.0h in 95 DEG C of water-baths is added according to the solid-liquid ratio of 1:50 in dry powder 10.0g；
In the extraction process of aforementioned Ammonium alum method leaf flavonoids, it is preferred that in the step 3, calculate Ammonium alum method leaf flavonoids
Yield method particularly includes:
Step a, extracting solution is filtered while hot, is concentrated under reduced pressure into 1/5th of original volume, the 95% of two volumes is added
Ethyl alcohol is stood overnight, and next day filtering is calculated the concentration of general flavone in filtrate by formula (1)；
Y=0.0097X+0.0054 (1)
In formula:
Absorbance value at Y: λ=510nm；
X: the concentration of determinand, unit are micrograms per millilitre.
Step b, flavones yield (%)=extract concentration × volume × extension rate/material quality × 100 are pressed, are calculated total
Flavones yield.
The present invention is include at least the following beneficial effects:
Extraction process provided by the invention has easily operated, simple and feasible feature；To the several factors for influencing yield
It is investigated；Solvent used in technique is all recyclable to be recycled, economic and environment-friendly；The present invention is to general flavone in Ammonium alum method leaf
Extract the effective use for helping to realize Ammonium alum method resource.
Other advantages, target and feature of the invention will be reflected by the following instructions respectively.
Detailed description of the invention
Fig. 1 is the influence curve figure of liquid-to-solid ratio of the invention to yield, and abscissa is liquid-to-solid ratio in figure, and ordinate is to extract
Rate/%.
Fig. 2 is the influence curve figure of extraction time of the invention to yield, and abscissa is extraction time/h, ordinate in figure
For recovery rate/%.
Fig. 3 is the influence curve figure of Extracting temperature of the invention to yield, in figure abscissa be Extracting temperature/DEG C, indulge sit
It is designated as recovery rate/%.
Specific embodiment
Below with reference to embodiment, a specific embodiment of the invention is further described.Following embodiment is for saying
The bright present invention, but be not used in and limit the scope of the invention.
<embodiment>
1 instrument
UV detector, Rotary Evaporators, water-bath.
2 materials and reagent
Ammonium alum method leaf (yellow fallen leaves), picks up from Medical University Of Chongqing campus, dry, pulverize after cleaning in 65 DEG C of baking ovens
It crosses 40 meshes and is placed in drier and store for future use；Ultrapure water, by Medical University Of Chongqing's original new drug and auxiliary material analytical technology platform
It provides；95% ethyl alcohol is provided by Sichuan Kingsoft pharmaceutical Co. Ltd；NaNO2, Al3(NO3)3·9H2O, NaOH, by Chengdu
Cologne Chemical Company provides；Control substance of Rutin (99%, pharmaceutical chemistry teaching and research room, pharmaceutical college, Medical University Of Chongqing).
3 methods
The extraction of 3.1 Ammonium alum method leaf flavonoids
Precision weighs Ammonium alum method leaf dried powder 1.0g, the deionized water of certain volume is added, under certain bath temperature
It extracts after a certain period of time, by filtrate, rotary evaporation is concentrated into the 20% of original volume in 65 DEG C of water-baths after filtering, and twice of body is added
95% long-pending ethyl alcohol is stood overnight, and filtrate is added water to 30mL after next day filtering, measures extinction after taking 1.0mL to carry out chromogenic reaction
Angle value, calculated result.
The drafting of 3.2 rutin standard curves
Precision weighs 0.1g rutin in 100mL volumetric flask, and 60% ethyl alcohol is added and dissolves and be settled to scale, obtains 1.0mg/
ML rutin stock solution.0.20,0.30,0.40,0.60,0.80 and 1.0mL of rutin standard solution is drawn respectively in 25mL volumetric flask
In, ultrapure water 6.0mL is added, mixes, 5% sodium nitrite solution 1.0mL is added, shakes up, stands 6min, then plus 10% aluminum nitrate
1.0mL shakes up, and stands 6min and adds 5% sodium hydroxide 10.0mL again, after ultrapure water constant volume, stands 15min, suction is surveyed in 510nm at
Luminosity.Using the concentration of reference substance as abscissa, corresponding absorbance is that ordinate draws standard curve.The linear of standard curve returns
Return equation are as follows: y=0.0097x+0.0054, R2=0.0983, rutin concentration and absorbance within the scope of 8.0~40.0 μ g/mL
In good linear relationship.
The screening of 3.3 extraction conditions
3.3.1 the influence of solid-liquid ratio, extraction time, Extracting temperature to Ammonium alum method leaf flavonoids yield is investigated.
It is respectively 1:20,1:30,1:40,1:50,1:60,1:70 and 1:80 (g/mL) that solid-liquid ratio, which is arranged, and precision weighs
7 parts of 1.0g Ammonium alum method leaf dried powder, in the deionized water that respective volume in round-bottomed flask, is added, are flowed back in 95 DEG C of water-baths and are mentioned
2.0h is taken, filtrate water constant volume measures absorbance simultaneously at λ=510nm after taking 1.0mL extracting solution to develop the color to 100mL after filtering
Content is calculated, influence of the solid-liquid ratio to Ammonium alum method leaf flavonoids yield, the result is shown in Figure 1 are investigated.As can be seen from the figure work as feed liquid
When than for 1:50 (g/mL), the content highest of general flavone in Ammonium alum method leaf extract.
3.3.2 influence of the extraction time to Ammonium alum method leaf flavonoids yield is investigated
Setting extraction time is respectively 0.5h, 1.0h, 1.5h, 2.0h, 3.0h, 4.0h, 6.0h, 8.0h and 10.0h, precision
9 parts of 1.0g Ammonium alum method leaf dried powder are weighed in round-bottomed flask, 50mL deionized water, the refluxing extraction in 95 DEG C of water-baths is added
Corresponding time, filtering measure absorbance at λ=510nm and calculate content, when investigating extraction after taking 1.0mL extracting solution to develop the color
Between influence to Ammonium alum method leaf flavonoids yield, as a result see Fig. 2.As can be seen from the figure upon extracting between be 2.0h when, yellow square rafter
The content highest of general flavone in leaf extracting solution.
3.3.3 influence of the Extracting temperature to Ammonium alum method leaf flavonoids yield is investigated
It is respectively 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C and 95 DEG C that Extracting temperature, which is arranged, and precision weighs 1.0g Ammonium alum method leaf
6 parts of dried powder, in round-bottomed flask, are added 50mL deionized water, and 2h is extracted in water-bath at the corresponding temperature, takes 1.0mL after filtering
Absorbance value is measured after extracting solution colour developing at λ=510nm and calculates content, Extracting temperature is investigated and Ammonium alum method leaf flavonoids is obtained
The influence of rate, is as a result shown in Fig. 3.As can be seen from the figure when Extracting temperature is 95 DEG C, general flavone in Ammonium alum method leaf extract
Content highest.
3.4 each polar solvents are to Ammonium alum method leaf extract effect of extracting
Filtrate 600mL after alcohol precipitation is concentrated into 60mL, then is extracted twice with petroleum ether (1:1, v/v), combining extraction liquid,
About 120mL extract liquor is rotated into recycling petroleum ether, residue 50mL95% ethyl alcohol dissolves, measures and inhale at λ=510nm after colour developing
Luminosity.Water layer after petroleum ether extraction is used ethyl acetate (1:1, v/v) again, and three times, other operate same petroleum ether for extraction；Water layer is most
After be saturated with water butanol solution (1:1, v/v) extraction three times, remaining operates same ethyl acetate, measures total Huang of each extraction part
Ketone content, discovery developed the color with petroleum ether portion after at λ=510nm substantially without absorption, ethyl acetate and the positive fourth of water saturation
Concentration of the alcohol extract liquor in same volume is respectively 102.06 μ g/mL, 456.70 μ g/mL, as can be known from the results, with opposed polarity
Solvent, which carries out fractional extraction, to be helped for general flavone to be enriched with, so that separating-purifying later is more easier.
Claims (4)
1. the extraction process of general flavone in Ammonium alum method leaf, which is characterized in that comprise the following steps that:
Step 1: Ammonium alum method leaf is cleaned, crushed after being dried, 20~100 meshes are crossed, Ammonium alum method leaf coarse powder is obtained；
Step 2: according to Ammonium alum method leaf coarse powder quality (g): water volume (mL) be 1:20~80 solid-liquid ratio be added deionized water into
Row bath temperature is the refluxing extraction of 50~95 DEG C of 0.5~10.0h by a definite date；
Step 3: extracting solution filters while hot, 1/5th of original volume are concentrated under reduced pressure into, 95% ethyl alcohol of two volumes is added,
It stands overnight, filters, measurement absorbance value calculates general flavone yield after taking filtrate to develop the color.
Step 4: 1/10th of original volume are concentrated the filtrate to, it is successively molten with petroleum ether, ethyl acetate and water-saturated n-butanol
Agent extraction, by the comparison to each section absorbance value, final determine is saturated with water containing for general flavone in n-butanol portion
Amount is maximum.
2. the extraction process of general flavone in Ammonium alum method leaf as described in claim 1, which is characterized in that Ammonium alum method in step 2
What leaf extracted method particularly includes:
Ammonium alum method leaf dried powder 10.0g is accurately weighed, 500mL deionized water is added according to the solid-liquid ratio of 1:50, in 95 DEG C of water
It goes back to extract 2.0h in bath.
3. the extraction process of general flavone in Ammonium alum method leaf as described in claim 1, which is characterized in that yellow to calculating in step 3
General flavone yield in square rafter leaf method particularly includes:
Step a, extracting solution is filtered while hot, filtrate rotary evaporation is concentrated under reduced pressure into 1/5th of original volume, in concentrate
Two volumes are added in 95% ethyl alcohol of concentrate, stand overnight, next day filtering, by general flavone in formula (1) measurement filtrate
Concentration；
Y=0.0097X+0.0054 (1)
In formula:
Absorbance value at Y: λ=500nm；
X: the concentration of determinand, unit are micrograms per millilitre；
Step b, general flavone is calculated by flavones yield (%)=extract concentration × volume × extension rate/material quality × 100
Yield.
4. the extraction process of general flavone in Ammonium alum method leaf as described in claim 1, which is characterized in that each polarity in step 4
Solvent successively extracts Ammonium alum method leaf and extracts concentrate method particularly includes: gained filtrate decompression after ethanol precipitation is concentrated into substance
Long-pending 10%, then successively extracted with petroleum ether, ethyl acetate and water-saturated n-butanol solution, each extract liquor is collected, is measured respectively
The content of general flavone in each extract liquor finds that the amount of contained general flavone in water-saturated n-butanol solution is most.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910237744.8A CN109865005A (en) | 2019-03-27 | 2019-03-27 | A kind of extraction process of Ammonium alum method leaf flavonoids |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910237744.8A CN109865005A (en) | 2019-03-27 | 2019-03-27 | A kind of extraction process of Ammonium alum method leaf flavonoids |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109865005A true CN109865005A (en) | 2019-06-11 |
Family
ID=66921377
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910237744.8A Pending CN109865005A (en) | 2019-03-27 | 2019-03-27 | A kind of extraction process of Ammonium alum method leaf flavonoids |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109865005A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637503A (en) * | 2009-08-19 | 2010-02-03 | 大连中植环境生物科技有限公司 | Total flavonoids of broussonetia papyrifera extract and preparation method and application thereof |
-
2019
- 2019-03-27 CN CN201910237744.8A patent/CN109865005A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101637503A (en) * | 2009-08-19 | 2010-02-03 | 大连中植环境生物科技有限公司 | Total flavonoids of broussonetia papyrifera extract and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 董兰岚等: "黄桷树叶中总黄酮的乙醇超声提取工艺研究", 《应用化工》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103961381B (en) | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract | |
| CN101637486B (en) | Angelica dahurica coumarin extract as well as preparation method and quality control method thereof | |
| CN105130796A (en) | Diterpenoid compound and preparing method and application thereof | |
| CN103804443A (en) | Flavonoid glycoside compound and preparation method thereof | |
| CN103739586A (en) | Method for extracting diterpenoid compounds from Blumea aromatic DC. | |
| CN103191041A (en) | Chinese yew branch and leaf extractive with anti-oxidative effect as well as extraction method and application of yew branch and leaf extractive | |
| CN104163755A (en) | Method for preparing magnolol and honokiol from Mangnolia officinalis leaves | |
| EP2650301B1 (en) | Method for preparing albiflorin and paeoniflorin | |
| CN101647828A (en) | Method for separating total alkaloid from sophora flavescens ait by using ion exchange resin | |
| CN102552371B (en) | Gynostemma pentaphylla extractive and application thereof to preparing medicine for treating tumor | |
| CN108299453A (en) | A method of detaching psoralen, Isopsoralen and Bakuchiol from psoralea corylifolia | |
| CN103006754B (en) | Manaplant alhagi extract and preparation method thereof | |
| CN102050851A (en) | Liquiritin and preparation method thereof | |
| CN103830306A (en) | Preparation method of honey suckle leaf effective extract product | |
| CN105963342A (en) | An antiallergic compound flavone composition, and a preparing method and applications thereof | |
| CN101732421A (en) | Method for preparing total flavonoids, total tannins and galic acid compounds of polygonum capitatum | |
| CN101698059A (en) | Method for separating dendrobium total alkaloids by ion exchange resin | |
| CN1332969C (en) | Flavonoid glycoside compound and its preparing process | |
| CN101941961A (en) | Method for extracting and separating kaempferol from impatiens balsamina | |
| CN109865005A (en) | A kind of extraction process of Ammonium alum method leaf flavonoids | |
| CN102172361A (en) | Method for separating traditional Chinese medicine total alkaloids by ion exchange resin | |
| CN103655744B (en) | Preparation method for Fukean tablet and application of Fukean tablet in preparation of drug used for inhibiting proliferation of mouse lymphoma cell YAC-1 | |
| Banerjee et al. | Pharmacognostical, physiochemical and phytochemical evaluation of leaf, Stem and Root of Orchid Dendrobium Ochreatum | |
| CN103214553A (en) | Method for extracting onion osteogenic peptide | |
| CN103351373A (en) | Method for extracting Schisandrin B from Schisandra chinensis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190611 |
|
| RJ01 | Rejection of invention patent application after publication |