CN110283154A - A kind of method that ultrasound assisted extraction maturation freezes green fruit anthocyanidin - Google Patents
A kind of method that ultrasound assisted extraction maturation freezes green fruit anthocyanidin Download PDFInfo
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- CN110283154A CN110283154A CN201910605381.9A CN201910605381A CN110283154A CN 110283154 A CN110283154 A CN 110283154A CN 201910605381 A CN201910605381 A CN 201910605381A CN 110283154 A CN110283154 A CN 110283154A
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- anthocyanidin
- green fruit
- maturation
- assisted extraction
- ultrasound assisted
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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Abstract
The invention discloses a kind of methods that ultrasound assisted extraction maturation freezes green fruit anthocyanidin, it is related to the extractive technique field of Plant Secondary Metabolites, the described method comprises the following steps: step 1, by it is mature, clean up in the green fruit of jelly of atropurpureus, it is ground broken；Step 2 presses solid-liquid ratio 1:30~1:70, and 40~90% anthocyanidin extractants are added in freezing green fruit；Step 3 is extracted 3~8 minutes in Ultrasonic Cell Disruptor；Step 4, by extracting solution in 10000rmin‑1It is centrifuged 10min under part, takes supernatant.The present invention can be greatly improved the extraction efficiency for freezing anthocyanidin in green ripening fruits, have the advantages that easy to operation, yield is high.
Description
Technical field
The present invention relates to Plant Secondary Metabolites extractive technique field more particularly to a kind of ultrasound assisted extraction maturation jelly are green
The method of fruit anthocyanidin.
Background technique
Freeze green (Rhamnus utilis), it is the red jelly of alias, black dog pellet, mountain plum, green sub, big green etc., it is Rhamnaceae
(Rhamnaceae) machaka of Rhamnus (Rhamnus) or dungarunga.Be distributed widely in Gansu in China, Shaanxi, Henan,
Hebei, Shanxi, Anhui, Jiangsu, Zhejiang, Jiangxi, Fujian, Guangdong, Guangxi, Hubei, Hunan, the ground such as Sichuan, Guizhou, in Korea half
Island and Japanese Science Society are also distributed, and it is big to freeze green hip number.
Freezing green is a kind of dye yielding herb, the pigment rich in such as tender fruit, blade, branch skin, by rubbing dye
The clothes such as silk, cotton can be dyed green by method.Freeze marennin and be referred to as " China is green ", primary pigments are in " Colour Index "
It is compiled respectively as natural green No.1 (Natural Green l) and natural green two (Natural Green 2).Patent document
CN101125963A can extract dye component therein from freezing in green root or bark using 30%~40% ethyl alcohol, heated dense
Contracting, condensing recovery, hig h-speed centrifugal spray drying can be made into natural dye powder.Patent document CN106084879A is to freeze green fruit
For material, filtered after ultrasonication and pectase are decomposed；Ethyl alcohol or extracted by ether are added in filter residue, through high-pressure pulse electric
It extracts, filtering；Filtrate can obtain freezing green dye through purification with macroreticular resin twice.
In addition, freezing green secondary metabolites rich in, for example blade flavones, fruit anthocyanidin are (purple after fruit maturation
Black, anthocyanidin rich in.Anthocyanidin have it is anti-oxidant, put cancer and other effects, it may also be used for foods and cosmetics etc.)
Deng.Some obtains medicinal extract with 95 ℅ EtOH Sonicate assisted extractions, then successively with petroleum to freeze green stem as material in the prior art
Ether, ethyl acetate, n-butanol are extracted, and medicinal extract is made respectively.Wherein alcohol steep object antioxidant activity with higher, second
Acetoacetic ester extract has stronger bacteriostatic activity.Some optimizes concentration of alcohol, liquid material using response phase method in the prior art
Than the influence with extraction time and Extracting temperature to greenery piece extracting flavonoids amount is frozen.Freeze the optimum extraction process of flavones in greenery piece
Are as follows: volume fraction of ethanol 70%, liquid-to-solid ratio 33:1, extraction time 50min and 30 DEG C of Extracting temperature, under this condition extracting flavonoids amount
Up to 35.07mg/g.Also there is the optimum extraction process for optimizing using response phase method and freezing flavones in green fruit in the prior art.In liquid
Under the conditions of material is than 30mL/g, concentration of alcohol 50%, 22 DEG C of Extracting temperature, extraction time 50min, freeze extracting flavonoids amount in green fruit
Up to 60.36mg/g.And patent document CN101411340A freezes green plant drymeal with 4~6 times of petroleum ether extraction, divides at room temperature
Jin Ti not be 2-4 times, 3~5 days every time, conventional vacuum concentration obtained extract.The extract there is poisoning to make tetranychus viennensis
With corrected mortality for 24 hours is 85.72%, LC50 0.52mg/ml.
Up to the present, have all multipair green of jellies, stem, bark, blade and green dye or flavones in young okra fruit reality
The methods and techniques that substance extracts.But the extractive technique about the mature anthocyanidin frozen in green fruit is but rarely reported,
And there are complex steps, time-consuming too long, most cannot quantify to extract for existing associated extraction method.
Therefore, those skilled in the art be dedicated to developing it is a kind of it is easy to operation, yield is high freezes green fruit to maturation
The method that anthocyanidin extracts in reality.
Summary of the invention
In view of the above drawbacks of the prior art, the technical problem to be solved by the present invention is to how quick, efficient, quantitative
Extract the mature anthocyanidin frozen in green fruit.
To achieve the above object, the present invention provides a kind of method that ultrasound assisted extraction maturation freezes green fruit anthocyanidin,
It the described method comprises the following steps:
Step 1, by it is mature, clean up in the green fruit of jelly of atropurpureus, it is ground broken；
Step 2 presses solid-liquid ratio 1:30~1:70, and 40~90% anthocyanidin extractants are added in freezing green fruit；
Step 3 is extracted 3~8 minutes in Ultrasonic Cell Disruptor；
Step 4, by extracting solution in 10000rmin-1Under the conditions of be centrifuged 10min, take supernatant.
Further, it in the step 1, after grinding is broken, is placed in 15mL centrifuge tube.
Further, the solid-liquid ratio in the step 2 is w/v.
Further, the anthocyanidin extractant in the step 2 is acidic methanol.
Further, the acidic methanol includes 1% hydrochloric acid.
Further, the concentration of the acidic methanol is 75%.
Further, the solid-liquid ratio for freezing green fruit and anthocyanidin extractant in the step 2 is 1:60 (g:mL).
Further, the power of Ultrasonic Cell Disruptor is 600W in the step 3.9, ultrasonic wave added as described in claim 1
Extract the mature method for freezing green fruit anthocyanidin, which is characterized in that extraction time is 5 minutes in the step 3.
Further, centrifuging temperature is 4 DEG C in the step 4.
Compared with prior art, the present invention extracts the mature green fruit of jelly by using the method for ultrasonic wave secondary organic solvent
In anthocyanidin, have the advantages that easy to operation, yield is high, substantially increase the extraction for freezing anthocyanidin in green ripening fruits
Efficiency.
It is described further below with reference to technical effect of the attached drawing to design of the invention, specific structure and generation, with
It is fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is method flow schematic diagram of the invention；
Fig. 2 is influence of a preferred embodiment of the present invention methanol concentration to green fruit glycosides recovery rate is frozen；
Fig. 3 is influence of a preferred embodiment of the present invention ultrasonication time to green fruit glycosides recovery rate is frozen；
Fig. 4 is influence of a preferred embodiment of the present invention solid-liquid ratio to green fruit glycosides recovery rate is frozen.
Specific embodiment
The preferred embodiment of the present invention is introduced below with reference to Figure of description, keeps its technology contents more clear and convenient for reason
Solution.The present invention can be emerged from by many various forms of embodiments, and protection scope of the present invention is not limited only to text
In the embodiment mentioned.
In the accompanying drawings, the identical component of structure is indicated with same numbers label, everywhere the similar component of structure or function with
Like numeral label indicates.The size and thickness of each component shown in the drawings are to be arbitrarily shown, and there is no limit by the present invention
The size and thickness of each component.Apparent in order to make to illustrate, some places suitably exaggerate the thickness of component in attached drawing.
As shown in Figure 1, ultrasound assisted extraction maturation of the present invention freezes green fruit anthocyanidin method, specific step is as follows:
Step 1, by it is mature, clean up in the green fruit of jelly of atropurpureus；It is ground broken.
Step 2 presses solid-liquid ratio (w/v) 1:30~1:70, be added in freezing green fruit anthocyanidin extractant 40~
90% acidic methanol (1% hydrochloric acid).
Step 3, in Ultrasonic Cell Disruptor, ultrasonic power be 600W under conditions of extract 3~8 minutes.
Step 4, by extracting solution in 10000rmin-1It is centrifuged 10min, takes supernatant.
Preferably, 75% acidic methanol (1% hydrochloric acid), solid-liquid ratio 1:60 are added in step 2.
Preferably, it is extracted 5 minutes under conditions of ultrasonic power is 600W in step 3.
Embodiment 1
0.2g is weighed respectively and freezes green fruit, and grinding is placed in 15mL centrifuge tube, respectively with 40,50,60,70,80,90%
Acidic methanol (1% hydrochloric acid) be Extraction solvent, at solid-liquid ratio 1:50 (g/mL), extracted under conditions of ultrasonic power is 600W
5min.At 4 DEG C, 10000rmin-1It is centrifuged 10min, takes supernatant.
Show the content of poor method measurement anthocyanidin using pH.Extracting solution 1ml is drawn, it is slow with hydrochloric acid-potassium chloride of pH1.0 respectively
The dilution of the Acetic acid-sodium acetate buffer of fliud flushing and pH4.5 is settled to 3ml.Up to after balance (80min), in maximum absorption wavelength
The absorbance of both measurements at 520nm.With the absorbance at 700nm as correction, distilled water does reference liquid, with corn flower
As anthocyanin standard, the Anthocyanin content measured is indicated element -3- glucoside with Cy-3-G content.
As shown in Figure 2, the results showed that 40% acidic methanol (1% hydrochloric acid) freeze green fruit anthocyanidin recovery rate be 43.2 ±
1.9mg·100g-1Fresh weight；The recovery rate of 50% acidic methanol is 43.0 ± 0.7mg100g-1Fresh weight, 60% recovery rate are
46.3±0.9mg·100g-1Fresh weight, 70% is 54.0 ± 2.1mg100g-1Fresh weight, 80% is 49.7 ± 1.2mg
100g-1Fresh weight, 90% is 43.1 ± 1.0mg100g-1Fresh weight.Wherein 70% acidic methanol recovery rate highest, with its elsewhere
The difference of reason reaches the level of signifiance.
Embodiment 2
0.2g is weighed respectively and freezes green fruit, is placed in 15mL centrifuge tube；Made with 60% acidic methanol (1% hydrochloric acid) solution
For Extraction solvent, solid-liquid ratio 1:50 (g/mL)；3,4,5,6,7,8min are extracted respectively under conditions of ultrasonic power is 600W.In
At 4 DEG C, 10000rmin-1It is centrifuged 10min, takes supernatant.
Show the content of poor method measurement anthocyanidin using pH.Extracting solution 1ml is drawn, it is slow with hydrochloric acid-potassium chloride of pH1.0 respectively
The dilution of the Acetic acid-sodium acetate buffer of fliud flushing and pH4.5 is settled to 3ml.Up to after balance (80min), in maximum absorption wavelength
The absorbance of both measurements at 520nm.With the absorbance at 700nm as correction, distilled water does reference liquid, with corn flower
As anthocyanin standard, the Anthocyanin content measured is indicated element -3- glucoside with Cy-3-G content.
As shown in Figure 3, the results showed that the green fruit anthocyanidin recovery rate of the jelly of ultrasonication 3min is 35.3 ± 1.1mg
100g-1Fresh weight；The recovery rate of ultrasonication 4min is 34.4 ± 1.4mg100g-1Fresh weight, the recovery rate of 5min is 40.6 ±
1.7mg·100g-1Fresh weight, 6min are 48.8 ± 0.9mg100g-1Fresh weight, 7min are 47.4 ± 2.2mg100g-1It is fresh
Weight, 8min is 44.2 ± 1.4mg100g-1Fresh weight.The wherein recovery rate highest of ultrasonication 6min, the difference with other processing
It is different to reach the level of signifiance.
Embodiment 3
0.2g is weighed respectively and freezes green fruit, is placed in 15mL centrifuge tube；Made with 60% acidic methanol (1% hydrochloric acid) solution
For Extraction solvent, solid-liquid ratio is respectively 1:30,1:40,1:50,1:60,1:70 (g/mL)；In the condition that ultrasonic power is 600W
Lower extraction 5min.At 4 DEG C, 10000rmin-1It is centrifuged 10min, takes supernatant.
Show the content of poor method measurement anthocyanidin using pH.Extracting solution 1ml is drawn, it is slow with hydrochloric acid-potassium chloride of pH1.0 respectively
The dilution of the Acetic acid-sodium acetate buffer of fliud flushing and pH4.5 is settled to 3ml.Up to after balance (80min), in maximum absorption wavelength
The absorbance of both measurements at 520nm.With the absorbance at 700nm as correction, distilled water does reference liquid, with corn flower
As anthocyanin standard, the Anthocyanin content measured is indicated element -3- glucoside with Cy-3-G content.
As shown in Figure 4, the results showed that the green fruit anthocyanidin recovery rate of the jelly that solid-liquid ratio is 1:30 is 30.1 ± 0.8mg
100g-1Fresh weight；The recovery rate that solid-liquid ratio is 1:40 is 35.2 ± 0.9mg100g-1Fresh weight, solid-liquid ratio are the recovery rate of 1:50
For 49.3 ± 2.4mg100g-1Fresh weight, solid-liquid ratio are that 1:60 is 40.0 ± 1.6mg100g-1Fresh weight, solid-liquid ratio are 1:70's
For 7.4 ± 1.8mg100g-1Fresh weight.Wherein solid-liquid ratio is the recovery rate highest of 1:50, reaches significant with the difference of other processing
It is horizontal.
Compared with prior art, the present invention presses preferred liquid-to-solid ratio 60:1 (mL:g), is added in freezing green ripening fruits excellent
The acidic methanol (1% hydrochloric acid) of the extractant 75% of choosing only needs 5min in preferred ultrasonic (power 600W) extraction time.Herein
Under the conditions of, the anthocyanidin pick-up rate frozen in green fruit is 54.45 ± 1.17mg100g-1.It substantially increases and freezes green ripening fruits
The extraction efficiency of middle anthocyanidin.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be within the scope of protection determined by the claims.
Claims (10)
1. a kind of method that ultrasound assisted extraction maturation freezes green fruit anthocyanidin, which is characterized in that the method includes following steps
It is rapid:
Step 1, by it is mature, clean up in the green fruit of jelly of atropurpureus, it is ground broken；
Step 2 presses solid-liquid ratio 1: 30~1: 70, and 40~90% anthocyanidin extractants are added in freezing green fruit；
Step 3 is extracted 3~8 minutes in Ultrasonic Cell Disruptor；
Step 4, by extracting solution in 10000rmin-1Under the conditions of be centrifuged 10min, take supernatant.
2. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
In 1, after grinding is broken, it is placed in 15mL centrifuge tube.
3. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
Solid-liquid ratio in 2 is w/v.
4. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
Anthocyanidin extractant in 2 is acidic methanol.
5. the method that ultrasound assisted extraction maturation as claimed in claim 4 freezes green fruit anthocyanidin, which is characterized in that the acidity
Methanol includes 1% hydrochloric acid.
6. the method that ultrasound assisted extraction maturation as claimed in claim 4 freezes green fruit anthocyanidin, which is characterized in that the acidity
The concentration of methanol is 75%.
7. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
The solid-liquid ratio for freezing green fruit and anthocyanidin extractant in 2 is 1:60 (g:mL).
8. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
The power of Ultrasonic Cell Disruptor is 600W in 3.
9. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
Extraction time is 5 minutes in 3.
10. the method that ultrasound assisted extraction maturation as described in claim 1 freezes green fruit anthocyanidin, which is characterized in that the step
Centrifuging temperature is 4 DEG C in rapid 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704598A (en) * | 2020-08-04 | 2020-09-25 | 河南白云牧港生物科技有限公司 | Method for extracting anthocyanin from Chinese yam root bark |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020055471A1 (en) * | 2000-08-31 | 2002-05-09 | Bailey David T. | Efficient method for producing compositions enriched in anthocyanins |
| CN103601770A (en) * | 2013-12-02 | 2014-02-26 | 上海交通大学 | Ultrasonic-assisted extraction method for anthocyanin in hibiscus syriacus petals |
-
2019
- 2019-07-05 CN CN201910605381.9A patent/CN110283154A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020055471A1 (en) * | 2000-08-31 | 2002-05-09 | Bailey David T. | Efficient method for producing compositions enriched in anthocyanins |
| CN103601770A (en) * | 2013-12-02 | 2014-02-26 | 上海交通大学 | Ultrasonic-assisted extraction method for anthocyanin in hibiscus syriacus petals |
Non-Patent Citations (1)
| Title |
|---|
| 全月澳 等: "《果树营养诊断法》", 31 March 1982, 农业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704598A (en) * | 2020-08-04 | 2020-09-25 | 河南白云牧港生物科技有限公司 | Method for extracting anthocyanin from Chinese yam root bark |
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