CN108619243A - A kind of solid acid strengthens hydro-thermal reaction collaboration and obtains through refining ramulus mori（Leaf）The method of middle active constituent - Google Patents
A kind of solid acid strengthens hydro-thermal reaction collaboration and obtains through refining ramulus mori（Leaf）The method of middle active constituent Download PDFInfo
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Abstract
The invention belongs to active constituent extractive technique fields in natural products, and in particular to Catalyzed by Phosphotungstic Acid, hydro-thermal reaction regulate and control method.Ramulus mori（Leaf）With efficient pharmacological action, the industries such as food, medicine and skin care item, ramulus mori are had been widely used for（Leaf）The pharmacological action shown and its active constituent are closely related, improve ramulus mori（Leaf）Extraction efficiency and the recycling value of middle active constituent are worth with research significance and applied economics.The present invention is directed to existing ramulus mori（Leaf）The deficiency of extraction process of active component, a kind of method of Catalyzed by Phosphotungstic Acid hydro-thermal regulation and control extraction is provided, both phosphorus heteropoly tungstic acid acid catalysis and hydro-thermal reaction Synergistic degradation plant tissue, destroy the hydrogen bond between cellulose and hemicellulose, destroy cell wall compact texture, reduce the mass transfer barrier between cell wall and cytoplasm, be conducive to being fully dissolved out for active constituent, realize extraction conditions operating procedure is few and simple, environmental pollution is small, energy consumption and it is at low cost the features such as.
Description
Technical field
The invention belongs to active constituent extractive technique fields in natural products, and in particular to Catalyzed by Phosphotungstic Acid, hydro-thermal
Response regulatory method.
Background technology
Mulberry leaf are rich in multivitamin（The 670 μ g containing retinol in 100g mulberry leaf dry products, 7440 μ g of carotene,
VB10.59mg, VB21.35mg VC31.6mg）And amino acid（Containing as many as 18 kinds, the 10.10% of dry weight is accounted for, wherein required amino
Acid content accounts for 3.281%, and vegetable protein the first limiting amino acid lysine accounts for 0.454%, and semi-dispensable amino acid accounts for 1.843%）；Mulberry
Leaf extract has good hypoglycemic, reducing blood lipid, anti-inflammatory, anti-aging, filaricide sick, antitumor.And contain polyhydroxy in ramulus mori
Base alkaloid, flavone compound, mulberry leaf polysaccharide, phytosterol, Polyphenols isoreactivity ingredient；With inhibition serum cholesterol liter
The pharmacological actions such as high and atherosclerosis, anti-bacteria and anti-virus.It is proved through modern medicine and Nutritional studies, ramulus mori（Leaf）
The efficient pharmacological action shown and its contained active constituent are closely related.The health care pharmacological action of mulberry leaf, makes it be eaten
The products such as mulberry tea, mulberry leaf noodle, mulberry leaf biscuit, mulberry leaf wine, mulberry vinegar, mulberry leaf sauce have been developed in the favor of product industry, keep people logical
Diet is crossed to achieve the purpose that prevent disease, promote longevity；With the continuous deepening of research, mulberry leaf are expected to become some diseases
The especially treatment drug and health product of geriatric disease and chronic disease, and have extensively in beauty and skin care, herding etc.
Wealthy foreground.
Existing ramulus mori（Leaf）Extraction process of active component mainly has reflux extraction, ultrasonic extraction, Enzymatic Extraction, surpasses and face
Boundary's fluid extraction etc..Wherein, circumfluence method extracting solution heated time is longer, because long-time is heated, the bioactivity of ingredient in raw material
It is easily damaged, and solvent-oil ratio is big, has limited to the production application of this method；The Enzymatic Extraction reaction time is long, and enzyme is albumen
Matter easily causes filtering sugar solution difficulty；Ultrasonic extracting method is easy to operate, but its extraction efficiency can be less than other methods sometimes；
Supercritical fluid extraction is greatly enhanced in extraction efficiency, but the equipment that its method requires is complicated, and solvent range of choice is narrow,
High pressure force container and high-pressure pump are needed, therefore cost of investment is higher.These methods more or less influence to extract product quality, cause environment
The problems such as pollution.Therefore, carry out the research of mulberry leaf active ingredient highly effective extraction method, improve ramulus mori（Leaf）Middle active constituent carries
It takes efficiency and recycling to be worth to be worth with research significance and applied economics.
Existing invention disclosed patent CN201610569828.8 in 2 days November in 2016 " a kind of hydro-thermal method extraction tea is more
The method of sugar ", the invention are to extract tea polysaccharide using hydro-thermal method in high-temperature high-pressure reaction kettle, that is, utilize the solution of high temperature and pressure
Make Tea Polysaccharides quickly complete molten extraction Tea Polysaccharides, can effectively extract Tea Polysaccharides, but there are still deficiencies below：（1）Only
The fine and close reticular structure of complexity of plant cell wall is destroyed by the pyrolysis of hydro-thermal reaction；（2）The invention is only extracted tea polysaccharide
A kind of substance；（3）Water cannot be fully dissolved out as extractant, other substances such as Tea Polyphenols in Tea, amino acid and protein, not
It can realize the maximization of the utilization of resources.Existing ramulus mori（Leaf）The extracting method of middle active constituent, as disclosed in 27 days January in 2016
" extracting method of active material in medicine mulberry leaf " of Publication No. CN201711354749.6, disclosed method is：Weigh drying
6.0L petroleum ethers are added by 1 ﹕, 20 solid-liquid ratios in medicine Mulberry Leaf 300.0g, and after 70 DEG C of reflux 4h filterings, filter residue presses 1 ﹕ 20 of solid-liquid ratio
6.0L65% ethyl alcohol is added, impregnates one day night, filtering, filtrate decompression is concentrated to give mulberry extract；Mulberry extract is by resin point
From purifying, three kinds of crude extracts of alkaloid, flavones and polysaccharide are respectively obtained.This method extraction active material chemical composition and
Though content is stablized, there are still deficiencies below：（1）Entire extraction process takes longer；（2）Petroleum ether and ethanol consumption are larger
Respectively 6.0L；（3）The inflammable and explosive property and chronic toxicity of petroleum ether threaten to health and environment, increase safety
Production cost.
Invention content
The object of the present invention is to be directed to existing ramulus mori（Leaf）It is miscellaneous to provide a kind of phosphorus tungsten for the deficiency of extraction process of active component
The method of polyacid catalysis-hydro-thermal regulation and control extraction, realizes that extraction conditions operating procedure is few and simple, environmental pollution is small, energy consumption
And the features such as at low cost.
Mechanism of the present invention is：The reticular structure for the complexity densification that plant cell wall is made of lignin, in outer force effect
Lower its compact texture of destruction, can just make hydrogen bond and breaking of covalent bonds, accelerate the dissolution of compound.β-O-4 the ehter bonds of lignin connect
The mode of connecing is that content is most and most important structural unit in lignin, while its bond energy minimum also most easy fracture, and lignin
Hydrolysis can occur under hydrothermal conditions, main process is the fracture of ehter bond.And phosphorus heteropoly tungstic acid acid catalysis and water
Both thermal responses Synergistic degradation plant tissue mainly utilizes surface that there is the acid sites of catalytic activity and heteropoly acid to aoxidize
Reduction carrier（E and II+）Diffusion and biomass in plant tissue occur oxidation under hydrothermal conditions, hydrolysis and acid
Both catalysed oxidns cooperate with, and destroy the hydrogen bond between cellulose and hemicellulose, and degrading plant fibr tissue destroys cell wall
Compact texture reduces the mass transfer barrier between cell wall and cytoplasm, is conducive to being fully dissolved out for active constituent.
Realizing the technical solution of goal of the invention is：A kind of solid acid strengthens hydro-thermal reaction collaboration and obtains through refining ramulus mori（Leaf）Middle activity
The method of ingredient in hydro-thermal reaction pot systems, through phosphorus heteropoly tungstic acid acid catalyzed degradation, centrifugation, is determined using Mulberry Leaf as raw material
Hold, and analysis is detected using efficient liquid phase.The method is as follows：
（1）Pretreatment of raw material
The new fresh mulberry leaf of picking is used in 50~70 DEG C of baking ovens and dries 4~6h, the mulberry leaf after drying are crushed through pulverizer, are sieved
60~100 mesh are packed into hermetic bag, for use.
（2）Solid acid strengthens hydro-thermal reaction and handles raw material
The（1）After the completion of step, the pretreated Mulberry Leafs of 2g are first weighed in hydrothermal reaction kettle, Quality of Mulberry Leaves is then added
（g）4~6 ‰ phosphorus heteropoly tungstic acid, finally according to absolute ethyl alcohol volume（ml）With Mulberry Leaf quality（g）Than for 3~11 ﹕ 1
Ratio, measure 6~22ml absolute ethyl alcohols pour into hydrothermal reaction kettle.Then reaction kettle is put into 170~190 DEG C of baking oven
React 90~130min.
（3）Active Components detect
The（2）After the completion of step, reaction kettle taking-up is cooled to room temperature, is poured into centrifuge tube, in 2000~4000r/min of rotating speed
Lower centrifugation 10-20min, pours out supernatant, is settled in 25nl volumetric flasks.1ml Mori folium extracts are pipetted in sample bottle, are being flowed
Dynamic phase acetonitrile（ml）﹕ water（ml）65~50 ﹕ 50 of=35 ﹕, 25~40 DEG C of temperature, 5~20 μ L of sample size, flow velocity are 0.6~1ml/
It is detected under conditions of min.
（4）Active constituent product is obtained through refining
Again by（3）The centrifugal clear liquid that step is collected is positioned in a rotary evaporator, is 0.4~0.6Mpa, temperature in vacuum pressure
Degree is at 80~100 DEG C, carries out being concentrated under reduced pressure into thick mulberry-leaf extract semifinished product；Then, according to mulberry-leaf extract system
The quality of product（g）: the volume of ethyl alcohol（ml）The ratio between be 1: 8~10 ratio, mulberry-leaf extract and second are added in leaching vessel
Alcoholic solution, mixed dissolution are uniform；Finally, by rotary evaporator, vacuum pressure is 0.4~0.6Mpa, temperature is 80~100
At DEG C, carries out that repetition 2~4 times is concentrated under reduced pressure, mulberry-leaf extract product is made.
The present invention is after adopting the above technical scheme, mainly there is following Xiao Guo ﹕
（1）The present invention carries out catalysis reaction by phosphorus heteropoly tungstic acid, due to its unique strong protonic acid, high hydrothermal stability,
It is multi-functional（Acid, oxygen, photocatalysis）, be easy to the molecular structure of modulation and unique " quasi- liquid phase " behavior, have to mulberry leaf good
Catalytic degradation effect.
（2）The present invention using ethyl alcohol replace water hydro-thermal reaction extraction mulberry leaf in active constituent, realize hydro-thermal reaction with
Alcohol extracting, which synchronizes, to be carried out, and absolute ethyl alcohol is used only in extraction process, successfully avoids the use of other poisonous and harmful solvents, increases experiment
The safety of process is conducive to the protection of environment, and easy to operate.
（3）The present invention uses discarded mulberry leaf for raw material, after pretreatment, is extracted with the method for the present invention and is slightly carried product,
Analysis detects three kinds of different dry measure used in former times skin glycosides, astragalin and chlorogenic acid active constituents.When mulberry leaf sieve through 80 mesh, are dried in 60 DEG C of baking ovens
After being pre-processed when 5h, wherein 5 ‰ heteropoly acid and 22 ml absolute ethyl alcohols is added, reaction temperature is 180 DEG C, the reaction time is
110 min, extraction effect is best, shows that heteropoly acid is applied to the extraction of active constituent in mulberry leaf and realizes its recycling to reach
Using there is critically important realistic meaning.
The present invention is further described With reference to embodiment.A kind of hydro-thermal reaction collaboration solid acid catalysis is obtained through refining
Ramulus mori（Leaf）The method of middle active constituent is as follows：
Embodiment 1
（1）Pretreatment of raw material
The new fresh mulberry leaf of picking is used in 60 DEG C of baking ovens and dries 5h, it is powder, sieving that the mulberry leaf after drying are crushed through pulverizer
80 mesh are packed into hermetic bag, for use.
（2）Solid acid strengthens hydro-thermal reaction and handles raw material
The（1）After the completion of step, the pretreated Mulberry Leafs of 2g are first weighed in hydrothermal reaction kettle, Quality of Mulberry Leaves is then added
（g）5 ‰ i.e. 0.01g phosphorus heteropoly tungstic acid, finally according to absolute ethyl alcohol volume（ml）With Mulberry Leaf quality（g）Than for 9 ﹕ 1
Ratio, measure 18ml absolute ethyl alcohols pour into hydrothermal reaction kettle.Then reaction kettle is put into 180 DEG C of baking oven and is reacted
110min。
（3）Active Components detect
The（2）After the completion of step, reaction kettle taking-up is cooled to room temperature, pours into centrifuge tube, is centrifuged at rotating speed 4000r/min
15min pours out supernatant, is settled in 25nl volumetric flasks.1ml Mori folium extracts are pipetted in sample bottle, in mobile phase acetonitrile
（ml）﹕ water（ml）=40 ﹕ 60,25 DEG C of temperature are detected under conditions of sample size 10 μ L, flow velocity 0.6ml/min, at this time mulberry leaf
Middle active material is fully dissolved out, and peak area is shown according to liquid phase testing result（mAu*s）Up to 23769.7.
（4）Active constituent product is obtained through refining
The（3）After the completion of step, the centrifugal clear liquid of collection is positioned in a rotary evaporator, is 0.5Mpa, temperature in vacuum pressure
Degree is at 90 DEG C, carries out being concentrated under reduced pressure into thick mulberry-leaf extract semifinished product；Then, according to the matter of mulberry-leaf extract product
Amount（g）The volume of ﹕ ethyl alcohol（ml）The ratio between be 1 ﹕ 9 ratio, mulberry-leaf extract and ethanol solution, mixing are added in leaching vessel
It is uniformly dissolved；Finally, reduced pressure repetition is carried out in the case where vacuum pressure is 0.5Mpa, temperature is 90 DEG C by rotary evaporator
3 times, mulberry-leaf extract product is made.
Embodiment 2
A kind of solid acid strengthens hydro-thermal reaction collaboration and obtains through refining ramulus mori（Leaf）The method of middle active constituent, with embodiment 1, wherein：
The（1）In step, oven temperature is 50 DEG C, drying time 6h, and be sieved 60 mesh.
The（2）In step, the quality of phosphorus heteropoly tungstic acid（g）For Quality of Mulberry Leaves（g）4 ‰, absolute ethyl alcohol（ml）With mulberry leaf powder
Last quality（g）The ratio between be 7 ﹕ 1, reaction temperature be 170 DEG C, reaction time 130min.
The（3）In step, rotating speed 2000r/min, centrifugation time 20min.Acetonitrile（ml）With water（ml）The ratio between be 35 ﹕
65, temperature is 30 DEG C, sample size 5 μ L, flow velocity 0.8ml/min, peak area（mAu*s）It is 19738.334.
The（4）In step, vacuum pressure 0.4Mpa, temperature are the quality of mulberry-leaf extract product at 80 DEG C（g）With ethyl alcohol
Volume（ml）The ratio between be 1 ﹕ 8, be concentrated under reduced pressure number of repetition be 4 times.
Embodiment 3
A kind of solid acid strengthens hydro-thermal reaction collaboration and obtains through refining ramulus mori（Leaf）The method of middle active constituent, with embodiment 1, wherein：
The（1）In step, oven temperature is 70 DEG C, drying time 4h, and be sieved 100 mesh.
The（2）In step, the quality of phosphorus heteropoly tungstic acid（g）For Quality of Mulberry Leaves（g）6 ‰, absolute ethyl alcohol（ml）With mulberry leaf powder
Last quality（g）The ratio between be 11 ﹕ 1, reaction temperature be 190 DEG C, reaction time 90min.
The（3）In step, rotating speed 3000r/min, centrifugation time 15min；Acetonitrile（ml）With water（ml）The ratio between be 50 ﹕
50, temperature is 40 DEG C, sample size 20 μ L, flow velocity 1ml/min, peak area（mAu*s）It is 18549.287.
The（4）In step, vacuum pressure 0.6Mpa, temperature are the quality of mulberry-leaf extract product at 100 DEG C（g）﹕ ethyl alcohol
Volume（ml）The ratio between be 1 ﹕ 10, be concentrated under reduced pressure number of repetition be 2 times.
Experimental result
1, different condition extract and prepare mulberry-leaf extract experimental result it is as follows：
Influence of the table 1-1 different temperatures to mulberry-leaf extract
| Serial number | Temperature（℃） | Mulberry leaf amount（g） | Peak area |
| 1 | 150 | 2.0005 | 4952.58206 |
| 2 | 160 | 2.0002 | 5957.05733 |
| 3 | 170 | 2.0004 | 6633.87159 |
| 4 | 180 | 2.0005 | 7278.36817 |
| 5 | 190 | 2.0001 | 4767.52964 |
Table 1-2 different solids compare the influence of mulberry-leaf extract
| Serial number | Solid-to-liquid ratio | Mulberry leaf amount（g） | Peak area |
| 1 | 1 ﹕ 3 | 2.0005 | 3994.49018 |
| 2 | 1 ﹕ 5 | 2.0002 | 4179.25257 |
| 3 | 1 ﹕ 7 | 2.0004 | 5305.81655 |
| 4 | 1 ﹕ 9 | 2.0005 | 9335.01751 |
| 5 | 1 ﹕ 11 | 2.0001 | 8241.60411 |
Influence of the table 1-3 different times to mulberry-leaf extract
| Serial number | Time（min） | Mulberry leaf amount（g） | Peak area |
| 1 | 70 | 2.0005 | 9197.33561 |
| 2 | 90 | 2.0002 | 9850.28037 |
| 3 | 110 | 2.0004 | 23769.7 |
| 4 | 130 | 2.0005 | 8074.78674 |
| 5 | 150 | 2.0001 | 7530.05743 |
It was found from above-mentioned experiment：The present invention discards the active constituent in mulberry leaf using the extraction of solid acid concerted catalysis hydro-thermal reaction,
When mulberry leaf sieve through 80 mesh, dry 5h in 60 DEG C of baking ovens after pretreatment, wherein 5 ‰ heteropoly acid and 18 ml absolute ethyl alcohols is added,
Reaction temperature is 180 DEG C, the reaction time is 110 min, and extraction effect is best, according to efficient liquid phase the results show that peak area reaches
To 23769.7, active constituent can be dissolved out adequately in mulberry leaf, and analysis detects different dry measure used in former times skin glycosides, resveratrol and chlorogenic acid
Three kinds of active constituents show that heteropoly acid is applied to the extraction of active constituent in mulberry leaf and realizes that the utilization of its recycling has very to reach
Important realistic meaning.And in extraction process, absolute ethyl alcohol is used only, successfully avoids the use of other poisonous and harmful solvents, carries
High security performance, increases the safety of experimentation, is conducive to the protection of environment, and easy to operate.
Claims (3)
1. a kind of hydro-thermal reaction collaboration solid acid catalysis obtains through refining ramulus mori（Leaf）The method of middle active constituent, it is characterised in that the side
Method concrete operation step is as follows：
（1）Pretreatment of raw material
（1）In step, the new fresh mulberry leaf of picking is used in 60 DEG C of baking ovens and dries 5h, the mulberry leaf after drying are through pulverizer powder
Broken is powder, and be sieved 80 mesh, is packed into hermetic bag, for use；
（2）Solid acid strengthens hydro-thermal reaction and handles raw material
The（1）After the completion of step, the pretreated Mulberry Leafs of 2g are first weighed in hydrothermal reaction kettle, Quality of Mulberry Leaves is then added
（g）5 ‰ i.e. 0.01g phosphorus heteropoly tungstic acid, finally according to absolute ethyl alcohol volume（ml）With Mulberry Leaf quality（g）Than for 9 ﹕ 1
Ratio, measure 18ml absolute ethyl alcohols pour into hydrothermal reaction kettle, then reaction kettle is put into 180 DEG C of baking oven and is reacted
110min；
（3）Active Components detect
The（2）After the completion of step, reaction kettle taking-up is cooled to room temperature, pours into centrifuge tube, is centrifuged at rotating speed 4000r/min
15min pours out supernatant, is settled in 25nl volumetric flasks, 1ml Mori folium extracts is pipetted in sample bottle, in mobile phase acetonitrile
（ml）﹕ water（ml）=40 ﹕ 60,25 DEG C of temperature are detected under conditions of sample size 10 μ L, flow velocity 0.6ml/min, at this time mulberry leaf
Middle active material is fully dissolved out, and peak area is shown according to liquid phase testing result（mAu*s）Up to 23769.7；
（4）Active constituent product is obtained through refining
The（3）After the completion of step, the centrifugal clear liquid of collection is positioned in a rotary evaporator, is 0.5Mpa, temperature in vacuum pressure
Degree is at 90 DEG C, carries out being concentrated under reduced pressure into thick mulberry-leaf extract semifinished product；Then, according to the matter of mulberry-leaf extract product
Amount（g）The volume of ﹕ ethyl alcohol（ml）The ratio between be 1 ﹕ 9 ratio, mulberry-leaf extract and ethanol solution, mixing are added in leaching vessel
It is uniformly dissolved；Finally, reduced pressure repetition is carried out in the case where vacuum pressure is 0.5Mpa, temperature is 90 DEG C by rotary evaporator
3 times, mulberry-leaf extract product is made.
2. a kind of preparation method and application of weak water-soluble supported catalyst according to claim 1, feature
It is that the method concrete operation step is as follows：
The（1）In step, oven temperature is 50 DEG C, drying time 6h, and be sieved 60 mesh；
The（2）In step, the quality of phosphorus heteropoly tungstic acid（g）For Quality of Mulberry Leaves（g）4 ‰, absolute ethyl alcohol（ml）With Mulberry Leaf matter
Amount（g）The ratio between be 7 ﹕ 1, reaction temperature be 170 DEG C, reaction time 130min；
The（3）In step, rotating speed 2000r/min, centrifugation time 20min, acetonitrile（ml）With water（ml）The ratio between be 35 ﹕ 65, temperature
Degree is 30 DEG C, sample size 5 μ L, flow velocity 0.8ml/min, peak area 19738.334；
The（4）In step, vacuum pressure 0.4Mpa, temperature are the quality of mulberry-leaf extract product at 80 DEG C（g）With the body of ethyl alcohol
Product（ml）The ratio between be 1 ﹕ 8, be concentrated under reduced pressure number of repetition be 4 times.
3. a kind of preparation method and application of weak water-soluble supported catalyst according to claim 1, feature
It is that the method concrete operation step is as follows：
The（1）In step, oven temperature is 70 DEG C, drying time 4h, and be sieved 100 mesh；
The（2）In step, the quality of phosphorus heteropoly tungstic acid（g）For Quality of Mulberry Leaves（g）6 ‰, absolute ethyl alcohol（ml）With Mulberry Leaf matter
Amount（g）The ratio between be 11 ﹕ 1, reaction temperature be 190 DEG C, reaction time 90min；
The（3）In step, rotating speed 3000r/min, centrifugation time 15min；Acetonitrile（ml）With water（ml）The ratio between be 50 ﹕ 50, temperature
Degree is 40 DEG C, sample size 20 μ L, flow velocity 1ml/min, peak area 18549.287；
The（4）In step, vacuum pressure 0.6Mpa, temperature are the quality of mulberry-leaf extract product at 100 DEG C（g）The body of ﹕ ethyl alcohol
Product（ml）The ratio between be 1 ﹕ 10, be concentrated under reduced pressure number of repetition be 2 times.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110551229A (en) * | 2019-09-19 | 2019-12-10 | 重庆工商大学 | Method for extracting natural product by catalyzing and activating mulberry twigs with heteropoly acid solution |
| CN114539132A (en) * | 2022-04-13 | 2022-05-27 | 重庆工商大学 | Method for performing DNJ (deoxyribose nucleic acid) extraction on mulberry leaves by hydrothermal acid control |
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| CN107282106A (en) * | 2017-06-28 | 2017-10-24 | 重庆工商大学 | A kind of weak water-soluble supported catalyst preparation method and application |
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