CN104644815A - Method for extracting total flavonoids of Chinese wampee leaves employing two-phase aqueous system and ultrasonic integration - Google Patents
Method for extracting total flavonoids of Chinese wampee leaves employing two-phase aqueous system and ultrasonic integration Download PDFInfo
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- CN104644815A CN104644815A CN201510116170.0A CN201510116170A CN104644815A CN 104644815 A CN104644815 A CN 104644815A CN 201510116170 A CN201510116170 A CN 201510116170A CN 104644815 A CN104644815 A CN 104644815A
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Abstract
The invention discloses a method for extracting total flavonoids of Chinese wampee leaves employing a two-phase aqueous system and ultrasonic integration. The method comprises the following steps: firstly, crushing the Chinese wampee leaves, and adding a certain concentration of isopropanol and ammonium sulfate water solution to form the two-phase aqueous system; and ultrasonically extracting total flavonoids in the Chinese wampee leaves. According to the method, an orthogonal test is designed on the basis of a single factor experiment result; extraction technological conditions of the total flavonoids are selected out; the optimal extraction conditions that the ultrasound time of 40% isopropanol solution of which the ammonium sulfate concentration is 310mg/mL is 20 minutes and the feed-to-liquid ratio is 1 to 40 are determined. The method disclosed by the invention is simple and convenient to operate; and the extraction efficiency is effectively improved.
Description
Technical field
The invention belongs to the technical field extracting total flavones, a kind of particularly method utilizing isopropyl alcohol-ammonium sulfate double-aqueous phase system and ultrasonic integrated extraction Folium clausenae lansii total flavones.
Background technology
Clausena lansium (Lour.) Skeels [Clausena lansium (Lour.) Skeels] belongs to Rutaceae Aurantiae plant, for the large shrub of perennial evergreen or dungarunga, originate in south China, Taiwan, Fujian, Guangdong, Hainan, Guangxi, South of Guizhou, Yunnan and Sichuan Valley of Jinsha River all have cultivation.Branch and leaf can do medical material, have heat radiation of inducing sweat, pleasantly to reduce phlegm, sterilize, the effect such as hemostasis.Flavone compound is extensively present in plant tissue, containing abundant flavone compound in Folium clausenae lansii.Flavone compound can prevent the burst of numerous disease, as cardiovascular disease etc.The method that tradition extracts flavone in plant has supercritical CO
2extraction, solvent extraction method etc.Aqueous two-phase extraction (Aqueous two-phase extraction, ATPE) technology is a kind of new separation technology, its method is that one or more materials are dissolved in water with suitable concentration, the immiscible aqueous solution system formed under certain condition, extraction object is reached according to the difference of pre-separation material distribution in double-aqueous phase system (Aqueous two-phase system, ATPS).ATPE have easy and simple to handle, mild condition, product purity are high, bioaffinity good, solvent easily reclaims, be easy to and the advantages such as other Integration ofTechnology.
CN103211926A proposes the method for total flavones in a kind of double-aqueous phase system extraction Semen Vitis viniferae, the method first extracts plant component with extractant, extracting solution is obtained after filtration, in extracting solution, add ethanol, ammonium sulfate or propanol again, ammonium sulfate forms double-aqueous phase system, extraction, separatory obtain main component, step is many, and the time is long.
For the deficiencies in the prior art, the present invention proposes a kind of method of extraction Folium clausenae lansii total flavones newly, direct isopropyl alcohol and a certain amount of ammonium sulfate are made into double-aqueous phase system solution, extract plant component as extractant, extraction limit, limit extracts, and step is few, the time is short, efficiency is high.
Summary of the invention
The invention discloses a kind of method utilizing isopropyl alcohol-ammonium sulfate double-aqueous phase system and ultrasonic integrated extraction Folium clausenae lansii total flavones, said method comprising the steps of:
S100: fresh Folium clausenae lansii is pulverized after drying in the shade, cross 40 mesh sieves, sealed type storage is for subsequent use;
S200: add double-aqueous phase system in the Folium clausenae lansii pulverized;
S300: with total flavones in supersound extraction Folium clausenae lansii, orthogonal test is designed on single factor experiment result basis, selects the extracting factor of total flavones.
In described step S200, double-aqueous phase system is the double-aqueous phase system that inorganic salt and isopropyl alcohol form.
Described inorganic salt is preferably any one in ammonium sulfate, sodium sulfate, sodium chloride, sodium carbonate, ammonium carbonate, is preferably ammonium sulfate.
In described double-aqueous phase system, the concentration of described inorganic salt is preferably 200-400mg/mL, and described isopropyl alcohol is preferably 20-40% isopropanol water solution.
In described step S300, ultrasound wave rated power is 250W, and the supersound extraction time is at 20min.
The volume ratio of described Folium clausenae lansii quality and double-aqueous phase system is 1: 30.
Described inorganic salt concentration 310mg/mL, described isopropyl alcohol is 40% isopropanol water solution, the solid-liquid ratio 1: 40 (g/mL) of Folium clausenae lansii and double-aqueous phase system, ultrasonic time 20min.
Method of the present invention is directly made into double-aqueous phase system solution with isopropyl alcohol and a certain amount of ammonium sulfate, extracts plant component as extractant, and extraction limit, limit extracts, and step is few, the time is short, efficiency is high.
Extract Folium clausenae lansii composition by method of the present invention, get isopropyl alcohol part after filtration, separatory, low-temperature evaporation dries to obtain total extract, weighs, and analyzing wherein flavones content is 71.34%.
Accompanying drawing explanation
Fig. 1 is that the double-aqueous phase system that forms of different salt and isopropyl alcohol is on the impact of Folium clausenae lansii extracting flavonoids rate; In figure: a is (NH
4)
2sO
4, b is Na
2sO
4, c is (NH
4)
2cO
3, d is NaCl, e is Na
2cO
3;
Fig. 2 is the impact of ammonium sulfate concentrations on extracting flavonoids rate;
Fig. 3 is the impact of isopropyl alcohol concentration on extracting flavonoids rate;
Fig. 4 is the impact of ultrasonic time on extracting flavonoids rate;
Fig. 5 is the impact of solid-liquid ratio on extracting flavonoids rate.
Detailed description of the invention
Embodiment 1
Utilize a method for isopropyl alcohol-ammonium sulfate double-aqueous phase system and ultrasonic integrated extraction Folium clausenae lansii total flavones, said method comprising the steps of:
S100: fresh Folium clausenae lansii is pulverized after drying in the shade, cross 40 mesh sieves, sealed type storage is for subsequent use; Folium clausenae lansii, picks up from Liuzhou Sha Tangzhen, is accredited as the fresh leaf of Clausena Rutaceae Aurantiae plant through doctor Qin Yiming.
S200: add double-aqueous phase system in the Folium clausenae lansii pulverized; Accurately take Folium clausenae lansii powder 1.00g and be placed in 100mL round-bottomed flask, the ammonium sulfate of the aqueous isopropanol and variable concentrations that add variable concentrations by certain solid-liquid ratio respectively forms isopropyl alcohol-ammonium sulfate aqueous two-phase solution.
S300: with total flavones in supersound extraction Folium clausenae lansii, orthogonal test is designed on single factor experiment result basis, selects the extracting factor of total flavones.
By the described ultrasonic certain hour of aqueous two-phase solution containing Folium clausenae lansii, filtered by Folium clausenae lansii, filtrate is placed in separatory funnel and leaves standstill 2h, gets upper solution, be settled to 25mL, shake up with 30% isopropyl alcohol after separatory.
Embodiment 2
The present invention presses formulae discovery total flavones extraction ratio
Quality (g) × 100% of total flavones extraction ratio (%)=total flavones quality (g)/Folium clausenae lansii powder
Embodiment 3
The selection of salt
Get the aqueous isopropanol of 30mL 30%, ammonium sulfate, sodium sulfate, sodium chloride, sodium carbonate, ammonium carbonate solid is added respectively by 300mg/mL, concussion is dissolved, form double-aqueous phase system, accurately take Folium clausenae lansii powder 1.00g, supersound extraction 15min, filter, a small amount of 30% aqueous isopropanol of filtering residue washs several times, collects filtrate and is placed in the standing 2h of separatory funnel, get upper solution, be settled to 25mL with 30% isopropyl alcohol, shake up, measure flavones content by the method for embodiment 2, calculate the extraction ratio of flavone, experimental result is shown in Fig. 1.
Result shows, high than other four kinds of salt as the extraction ratio of extracting solution flavone with the double-aqueous phase system of ammonium sulfate and isopropyl alcohol composition, its extracting flavonoids rate is 2.68%, therefore tests and selects ammonium sulfate and isopropyl alcohol to form double-aqueous phase system to extract flavone.
Embodiment 4
Experiment of single factor
Ammonium sulfate consumption is on the impact of extraction ratio
Accurately take Folium clausenae lansii powder 1.00g 5 parts, get the aqueous isopropanol of 30mL 30%, respectively by 240,260,280,300,320mg/mL adds ammonium sulfate solids, concussion is dissolved, and forms stable double-aqueous phase system, ultrasonic 15min, filter, wash several times with a small amount of 30% aqueous isopropanol, collect filtrate and be placed in the standing 2h of separatory funnel, get upper solution, 25mL is settled to 30% isopropyl alcohol, shake up, measure flavones content by the method for embodiment 2, calculate extracting flavonoids rate.
Isopropyl alcohol concentration is on the impact of extraction ratio
Take 6 parts, 1.00g Folium clausenae lansii powder, be that 300mg/mL adds ammonium sulfate by concentration respectively, be 1: 30 aqueous isopropanol adding 20%, 25%, 30%, 35%, 40%, 45% respectively with solid-liquid ratio (m: V), ultrasonic time 15min, filter, wash several times with a small amount of 30% aqueous isopropanol, collect filtrate and be placed in the standing 2h of separatory funnel, get upper solution, 25mL is settled to 30% isopropyl alcohol, shake up, measure flavones content by the method for embodiment 2, calculate extracting flavonoids rate.
Ultrasonic time is on the impact of extraction ratio
Take 6 parts, 1.00g Folium clausenae lansii powder, be 1: 30 aqueous isopropanol adding 40% by solid-liquid ratio (m: V) respectively, respectively ultrasonic 5,10,15,20,25,30min, filter, with a small amount of 30% aqueous isopropanol washing several times, collect filtrate and be placed in the standing 2h of separatory funnel, divide and get upper solution, be settled to 25mL with 30% isopropyl alcohol, shake up, measure flavones content by the method for embodiment 2, calculate extracting flavonoids rate.
Solid-liquid ratio is on the impact of extraction ratio
Take 7 parts, 1.00g Folium clausenae lansii powder, add the double-aqueous phase system solution of 40% aqueous isopropanol and 300mg/mL ammonium sulfate composition respectively by 1: 15,1: 20,1: 25,1: 30,1: 35,1: 40,1: 45, ultrasonic 20min, filters, wash several times with a small amount of 30% aqueous isopropanol, collect filtrate and be placed in the standing 2h of separatory funnel, separatory, gets upper solution, 25mL is settled to 30% isopropyl alcohol, shake up, measure flavones content by the method for embodiment 2, calculate extracting flavonoids rate.
Experiment of single factor result
Ammonium sulfate concentrations is on the impact of extracting flavonoids rate
Experimental result as shown in Figure 2.
Fig. 2 shows, total flavones extraction ratio first increases rear decline with ammonium sulfate concentrations, ammonium sulfate concentrations is between 240 ~ 300mg/mL, total flavones extraction ratio increases along with the increase of ammonium sulfate concentrations, and after ammonium sulfate concentrations reaches 320mg/mL, total flavones extraction ratio starts to reduce, and when can find out that ammonium sulfate concentrations is about 300mg/mL, total flavones extraction ratio is maximum.
Isopropyl alcohol concentration is on the impact of extracting flavonoids rate
Experimental result as shown in Figure 3.
As seen from Figure 3, with the increase of isopropyl alcohol concentration, total flavones extracts and takes the lead in subtracting after increasing; Its concentration is 20% ~ 40% time, and total flavones extraction ratio increases with isopropyl alcohol concentration and increases; When isopropyl alcohol is 45%, total flavones extraction ratio declines.Therefore, experimental selection 40% isopropyl alcohol effect is better.
Ultrasonic time is on the impact of extracting flavonoids rate
Experimental result as shown in Figure 4.
As seen from Figure 4, with the increase of ultrasonic time, total flavones extraction ratio progressively increases, and increase very fast in 5 ~ 20min, after 20min, increasing degree is less, this is because extracting flavonoids is close to complete, therefore ultrasonic time is for be advisable at about 20min.
Solid-liquid ratio is on the impact of extracting flavonoids rate
Experimental result as shown in Figure 5.
As seen from Figure 5, solid-liquid ratio increases soon 1: 15 ~ 1: 30 time, starts to decline after 1: 35, and can find out that total flavones extraction ratio is maximum solid-liquid ratio 1: 30 time, therefore solid-liquid ratio is that 1: 30 extraction effect is better.
Embodiment 5
Orthogonal experiment
According to experiment of single factor result, use L
9(3
4) table design arranges orthogonal experiment, empirical factor level in table 1, orthogonal experiment arrangement and the results are shown in Table 2.
Table 1 orthogonal experiment factor level table
From experiment of single factor in embodiment 4, during ultrasonic-aqueous two-phase integrated extraction Folium clausenae lansii total flavones, its extraction ratio is undertaken by ammonium sulfate concentrations, isopropyl alcohol concentration, ultrasonic time, solid-liquid ratio four factors, for optimizing further extracting flavonoids condition further, carry out the orthogonal experiment of 4 factor 3 levels, orthogonal experiment factor level in table 1, experimental establishment and the results are shown in Table 2.
The arrangement of table 2 orthogonal experiment and experimental result
Each factor can be obtained according to the extreme difference R of Orthogonal experiment results and B > C > D > A is followed successively by from big to small to the primary and secondary of total flavones extraction ratio, i.e. isopropyl alcohol concentration > solid-liquid ratio > ultrasonic time > ammonium sulfate consumption; Be A according to k value size determination optimum extraction condition
3b
3c
3d
3, i.e. 40% isopropyl alcohol, solid-liquid ratio 1: 40, ultrasonic time 20min, ammonium sulfate concentrations 310mg/mL.
Embodiment 6
The assay method of flavones content:
Accurately take 10.00mg control substance of Rutin, add methanol 10mL, slight fever is dissolved, be cooled to room temperature, be transferred to 50mL volumetric flask, use methanol solution standardize solution, shake up, obtaining concentration is 0.20mg/mL control substance of Rutin solution, pipette 0.0, 2.0, 4.0, 6.0, 8.0, 10.0mL control substance of Rutin solution is in 25mL volumetric flask, add water to about 10ml, add 5%NaNO21.00mL, shake up, place 5min, add 10%Al (NO3) 31.0mL, shake up, place 5min, add 4%NaOH 10mL, add water to graduation mark, shake up, place 15min, take blank as reference, absorbance is surveyed at maximum absorption wavelength 510nm place.With the concentration of rutin standard solution for vertical coordinate, take absorbance A as abscissa, drawing standard curve, return with method of least square, obtain the regression equation of the concentration c (mg/mL) of absorbance and rutin standard solution: c=0.1825A+0.001, correlation coefficient r=0.9973, this shows that the method has good linear relationship in 0.00-0.08mg/mL concentration range, can be used for the mensuration of general flavone content in Folium clausenae lansii.
Measure need testing solution a certain amount of, add solution respectively as stated above and measure absorbance, absorbance is substituted into total flavones quality in regression equation calculation total flavones concentration and sample, calculate total flavones extraction ratio by example 2 method.
Embodiment 7
Utilize a method for isopropyl alcohol-ammonium sulfate double-aqueous phase system and ultrasonic integrated extraction Folium clausenae lansii total flavones, under several different condition, total flavones extracts the comparison of yield:
S100: accurately take Folium clausenae lansii powder and be placed in 100mL round-bottomed flask;
S200: ammonium sulfate finite concentration (20% ~ 45%) isopropanol water solution is made into double-aqueous phase system solution (concentration is 240 ~ 320mg/mL);
S300: accurately measure double-aqueous phase system solution by certain solid-liquid ratio (between 1: 15 to 1: 40), pour in above-mentioned round-bottomed flask and mix with Folium clausenae lansii powder;
S400: supersound extraction certain hour (5 ~ 30min), after filtration, separatory, recording total flavones extraction yield is 1.62%.
Change ammonium sulfate concentrations, isopropyl alcohol concentration, solid-liquid ratio and ultrasonic time, under recording different condition, several result is as follows:
Under table 3 different condition, total flavones extracts the comparison of yield
Note: experiment 5 is the extraction effect of this method optimal conditions.
Claims (8)
1. utilize a method for double-aqueous phase system and ultrasonic integrated extraction Folium clausenae lansii total flavones, it is characterized in that, said method comprising the steps of:
S100: pulverize after being dried in the shade by fresh Folium clausenae lansii, sealed type storage is for subsequent use;
S200: add double-aqueous phase system in the Folium clausenae lansii pulverized;
S300: by the ultrasonic certain hour of aqueous two-phase solution containing Folium clausenae lansii, filters Folium clausenae lansii, and filtrate is placed in separatory funnel and leaves standstill 2h, gets upper solution, obtain Folium clausenae lansii total flavones after separatory.
2. method according to claim 1, is characterized in that, preferably, in described step S300, the extraction ratio computing formula of total flavones is as follows:
Quality (g) × 100% of total flavones extraction ratio (%)=total flavones quality (g)/Folium clausenae lansii powder.
3. method according to claim 1, is characterized in that, in described step S200, double-aqueous phase system is the double-aqueous phase system that inorganic salt and isopropyl alcohol form.
4. method according to claim 3, described inorganic salt is any one in ammonium sulfate, sodium sulfate, sodium chloride, sodium carbonate, ammonium carbonate, is preferably ammonium sulfate.
5. the method according to claim 3 or 4, is characterized in that, in described double-aqueous phase system, the concentration of described inorganic salt is 200-400mg/mL, and described isopropyl alcohol is 20-40% isopropanol water solution.
6. method according to claim 1, is characterized in that, in described step S300, the supersound extraction time is at 20min.
7. method according to claim 1, is characterized in that, the volume ratio of described Folium clausenae lansii quality and double-aqueous phase system is 1
:30.
8. method according to claim 5, is characterized in that, described inorganic salt concentration 310mg/mL, and described isopropyl alcohol is 40% isopropanol water solution, the solid-liquid ratio 1: 40 (g/mL) of Folium clausenae lansii and double-aqueous phase system, ultrasonic time 20min.
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| CN110818667A (en) * | 2019-10-22 | 2020-02-21 | 西安医学院 | Method for extracting flavone from pomegranate waste based on ionic liquid and semi-bionic enzymatic method |
| CN112876443A (en) * | 2021-02-05 | 2021-06-01 | 许昌学院 | Method for extracting flavonoid active substances in honey |
| CN114796331A (en) * | 2022-04-07 | 2022-07-29 | 福建师范大学 | Method for preparing total flavonoids of fructus aurantii |
| CN115590905A (en) * | 2022-10-26 | 2023-01-13 | 贵州省草业研究所（Cn） | Extraction separation method for improving flavone and polyphenol content in wild buckwheat stem and leaf extract |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818667A (en) * | 2019-10-22 | 2020-02-21 | 西安医学院 | Method for extracting flavone from pomegranate waste based on ionic liquid and semi-bionic enzymatic method |
| CN112876443A (en) * | 2021-02-05 | 2021-06-01 | 许昌学院 | Method for extracting flavonoid active substances in honey |
| CN112876443B (en) * | 2021-02-05 | 2023-02-03 | 许昌学院 | Method for extracting flavonoid active substances in honey |
| CN114796331A (en) * | 2022-04-07 | 2022-07-29 | 福建师范大学 | Method for preparing total flavonoids of fructus aurantii |
| CN115590905A (en) * | 2022-10-26 | 2023-01-13 | 贵州省草业研究所（Cn） | Extraction separation method for improving flavone and polyphenol content in wild buckwheat stem and leaf extract |
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