CN106187977A - A kind of method extracting Garcinia mangostana shell procyanidins - Google Patents
A kind of method extracting Garcinia mangostana shell procyanidins Download PDFInfo
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- CN106187977A CN106187977A CN201610529520.0A CN201610529520A CN106187977A CN 106187977 A CN106187977 A CN 106187977A CN 201610529520 A CN201610529520 A CN 201610529520A CN 106187977 A CN106187977 A CN 106187977A
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- garcinia mangostana
- mangostana shell
- procyanidins
- extraction
- shell
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
Abstract
The invention discloses a kind of method extracting Garcinia mangostana shell procyanidins, belong to the technical field that agricultural product active substance extracts, with Garcinia mangostana shell as raw material, solvent additional high pressure pulsed electric field methods is used to extract the procyanidin in Garcinia mangostana shell, first the method is that Garcinia mangostana shell is dried, pulverizes, is sieved, obtain Garcinia mangostana shell powder, again through slightly carrying, high voltage pulse electric field processing, extraction, purification, drying and other steps extract the procyanidin in Garcinia mangostana shell, the invention improves upon the efficiency extracting procyanidin at present from Garcinia mangostana shell, there is important economic worth.
Description
Technical field
The invention belongs to agricultural product active substance procyanidin extractive technique field, be specifically related to a kind of extraction in Garcinia mangostana shell
The method of procyanidin.
Background technology
Procyanidin (being called for short PC) is a kind of polyphenol substance mixture being widely present in nature in plant, rufous
Powder, feeble QI, puckery, it is dissolved in water and most organic solvent, there is the strongest in vivo bioactivity, be recognized in the world
High-efficiency antioxidant agent, it is possible to protection human body is from the damage of free radical.Procyanidin is applied quite varied in daily life, as
In terms of skin protection, procyanidin is added in skin care item to be effectively improved elasticity of skin, plays defying age, whitening and uvioresistant etc.
Effect, then can be used as lipstick on Cosmetic Market；Health care aspect, procyanidin makes health product energy enhancing human body immunity
Power, has blood fat reducing, suppression colon cancer cell, prevention cardiovascular and cerebrovascular disease and atherosclerosis；Therefore procyanidin is protecting
The fields such as skin, cosmetic industry, medicines and health protection, functional food have broad application prospects.
Procyanidin is planted the beans such as Fructus Vitis viniferae, Sorghum vulgare Pers., Fructus Mali pumilae, cacao bean and wild fruit such as Rosehips, Fructus Pruni pseudocerasi, Fructus Fragariae Ananssae etc.
In thing widely distributed, along with the expansion of plant research scope, increasing research display Garcinia mangostana shell there is also procyanidin.
At present, the method about extraction procyanidin mainly has following several: conventional organic solvents extraction, aqueous solution carry
Follow the example of, supercritical fluid extraction, microwave-assisted extraction etc., but organic solvent extraction is by reagent selection, raw material size, material
The impact of the many factors such as liquor ratio, and organic solvent toxic and side effects is big and product extraction ratio is low, extraction time is long, and destructible heat is steady
Qualitative more weak composition, impurity content is high, pollutes environment；Extraction with aqueous solution method selects water as extractant, and extraction is time-consuming long, temperature
Degree height, easily causes the loss of procyanidin, and the polarity of water is relatively big simultaneously, and dissolution impurity is more, and DNA purity is relatively low；Shooting flow
Body extraction cost is high, and the requirement to operating condition is higher.
To sum up, generally there is the low problem such as unstable with anthocyanidin of extraction efficiency in procyanidin traditional extraction process, therefore,
Exploring new extractive technique to improve the extraction efficiency of anthocyanidin and stability is the development side that procyanidin extracts research from now on
To.
Summary of the invention
In place of it is an object of the invention to overcome above-mentioned the deficiencies in the prior art, it is provided that one extracts former cyanine from Garcinia mangostana shell
The method of element.The procyanidin utilizing the method to be extracted can be widely applied to skin care item industry, medicines and health protection and functional food
The fields such as product.
The present invention is a kind of procyanidin utilized in solvent additional high pressure pulsed electric field methods extraction Garcinia mangostana shell, and raw material is
Garcinia mangostana shell.
The method be first bosom branch is shelled after peel be dried, pulverize, sieve, receive Garcinia mangostana shell powder, then will
Garcinia mangostana shell powder through slightly carrying, high voltage pulse electric field processing, extraction, purification, drying and other steps extract the procyanidin in Garcinia mangostana shell.
The invention improves upon the efficiency extracting procyanidin at present from Garcinia mangostana shell, there is important economic and social benefit.
The technical scheme that the present invention provides is:
A kind of method extracting Garcinia mangostana shell procyanidins, described method comprises the following steps:
1) being dried by Garcinia mangostana shell, liquid nitrogen crosses 40～80 mesh sieves after pulverizing, and loads container, and it is standby that sealing is stored in 4 DEG C of refrigerators；
2) weigh Garcinia mangostana shell, add ethanol water with the feed liquid weight ratio of 1:10～15, then press 150U/mL addition fiber
Element enzyme, is 4～8 slightly to extract 0.5～1.5h at pH value, filter, reduce pressure, concentrate after obtain concentrated solution, add ether and remove
Lipoid substance, again with methanol extracts with ethyl acetate mixture, adds after water and reduces pressure, removes organic solvent and i.e. obtain
Crude extract；
3) crude extract is added mass fraction 30% glacial acetic acid aqueous solution by weight 1:10～20, by crude extract and ice vinegar
Aqueous acid is positioned in high-pressure pulse electric extraction 1～2 hour, obtains extracting solution；
4) purification: by extracting solution filtration under diminished pressure, after recycling design, separates through macroporous adsorbent resin, and uses 10 times of weights
Distilled water and 60% mass fraction ethanol water carry out eluting；
5) it is dried: eluent being placed in 50～60 DEG C of vacuum and concentrates, last lyophilization becomes powder, is produced
Thing.
Preferably, step 2) in thick Extracting temperature be 35～45 DEG C, ethanol water mass fraction is 60～70%.
Preferably, step 2) described in methanol and ethyl acetate weight ratio be 1:4.
Preferably, step 2) described in ether, methanol, ethyl acetate concentration mass fraction more than 99%, ether with
The weight ratio of concentrated solution is 1: 1, and methanol is 2: 1 with the weight ratio of ethyl acetate mixture with concentrated solution.
Preferably, step 3) described in high-pressure pulse electric electric field intensity be 20～30kV/cm, umber of pulse be 6～
8。
Preferably, step 3) mesohigh impulse electric field equipment extracts 2 hours.
Preferably, step 4) described in macroporous adsorbent resin be AB-8.
The present invention at least includes following beneficial effect:
(1) solvent additional high pressure impulse electric field extract separate mainly according to the existence of the effective ingredient in material,
One novel extraction procyanidin technique of the design such as polarity, dissolubility, has low cost, small investment, extraction time are short, extract
Efficiency high, during extracting, the process of high-pressure pulse electric does not results in the rising of material temperature, can be effectively
The physiologically active of protection procyanidin extract, it is ensured that the stability of product, has the biggest application value.
(2) method extracting procyanidin from Garcinia mangostana shell that the present invention provides, than general procyanidin extraction process
Yield is high, is about 2.5 times of conventional organic solvent method, about 1.6 times of microwave assisting method, and about 1.4 times of ultrasonic assistant method carry
Take temperature low, the activity of procyanidin can be kept very well, it is to avoid the noise of ultrasonic assistant method is big, treating capacity is little lacks
Fall into, it is possible to continuous processing sample, be suitable to industrialization large-scale production.
(3) use the method disclosed in the present, filled up currently with solvent additional high pressure impulse electric field from Garcinia mangostana shell
The technological gap of middle extraction procyanidin.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will be by this
Invention research and practice and be understood by the person skilled in the art.
Detailed description of the invention
In conjunction with the following example, the present invention is described in further detail, to make those skilled in the art with reference to description
Word can be implemented according to this.
Embodiment 1
The method extracting Garcinia mangostana shell procyanidins comprises the following steps:
1) being dried by Garcinia mangostana shell, liquid nitrogen crosses 40 mesh sieves after pulverizing, and loads container, and it is standby that sealing is stored in 4 DEG C of refrigerators；
2) weighing Garcinia mangostana shell, the feed liquid weight ratio with 1: 10 adds ethanol water, then presses 150U/mL addition cellulose
Enzyme, is 4 slightly to extract 0.5h at pH value, filter, reduce pressure, concentrate after obtain concentrated solution, add ether and remove lipoid substance,
Again with methanol extracts with ethyl acetate mixture, adds after water and reduces pressure, removes organic solvent and i.e. obtain crude extract；
3) crude extract is added mass fraction 30% glacial acetic acid aqueous solution by weight 1: 10, by crude extract and glacial acetic acid water
Solution is positioned in high-pressure pulse electric extraction 1 hour, obtains extracting solution；
4) purification: by extracting solution filtration under diminished pressure, after recycling design, separates through macroporous adsorbent resin, and uses 10 times of weights
Distilled water and 60% mass fraction ethanol water carry out eluting；
5) it is dried: eluent being placed in 50 DEG C of vacuum and concentrates, last lyophilization becomes powder, obtains product.
Embodiment 2
The method extracting Garcinia mangostana shell procyanidins comprises the following steps:
1) being dried by Garcinia mangostana shell, liquid nitrogen crosses 80 mesh sieves after pulverizing, and loads container, and it is standby that sealing is stored in 4 DEG C of refrigerators；
2) weighing Garcinia mangostana shell, it is 60% ethanol water that the feed liquid weight ratio with 1: 15 adds mass fraction, then presses 150U/
ML adds cellulase, is 8 at pH value, and temperature is 35 DEG C, slightly extracts 1.5h, filter, reduce pressure, concentrate after concentrated
Liquid, adds ether and removes lipoid substance, and again with methanol extracts with ethyl acetate mixture, reduces pressure, goes after adding water
I.e. obtain crude extract except organic solvent, described ether, methanol, ethyl acetate concentration mass fraction are more than 99%, and ether is with dense
The weight ratio of contracting liquid is 1: 1, and methanol is 2: 1 with the weight ratio of ethyl acetate mixture with concentrated solution, described methanol and second
Acetoacetic ester weight ratio is 1: 4；
3) crude extract is added mass fraction 30% glacial acetic acid aqueous solution by weight 1: 20, by crude extract and glacial acetic acid water
It is to extract 2 hours in 20kV/cm high-pressure pulse electric that solution is positioned over electric field intensity, and umber of pulse is 6, obtains extracting solution；
4) purification: by extracting solution filtration under diminished pressure, after recycling design, separates through AB-8 macroporous adsorbent resin, and uses 10
Distilled water and the 60% mass fraction ethanol water of times weight carry out eluting；
5) it is dried: eluent being placed in 50 DEG C of vacuum and concentrates, last lyophilization becomes powder, obtains product.
Embodiment 3
The method extracting Garcinia mangostana shell procyanidins comprises the following steps:
1) being dried by Garcinia mangostana shell, liquid nitrogen crosses 60 mesh sieves after pulverizing, and loads container, and it is standby that sealing is stored in 4 DEG C of refrigerators；
2) weighing Garcinia mangostana shell, it is 70% ethanol water that the feed liquid weight ratio with 1: 12 adds mass fraction, then presses 150U/
ML adds cellulase, is 6 at pH value, and temperature is 45 DEG C, slightly extracts 1.0h, filter, reduce pressure, concentrate after concentrated
Liquid, adds ether and removes lipoid substance, and again with methanol extracts with ethyl acetate mixture, reduces pressure, goes after adding water
I.e. obtain crude extract except organic solvent, described ether, methanol, ethyl acetate concentration mass fraction are more than 99%, and ether is with dense
The weight ratio of contracting liquid is 1: 1, and methanol is 2: 1 with the weight ratio of ethyl acetate mixture with concentrated solution, described methanol and second
Acetoacetic ester weight ratio is 1: 4；
3) crude extract is added mass fraction 30% glacial acetic acid aqueous solution by weight 1: 15, by crude extract and glacial acetic acid water
It is to extract 1.5 hours in 30kV/cm high-pressure pulse electric that solution is positioned over electric field intensity, and umber of pulse is 8, obtains extracting solution；
4) purification: by extracting solution filtration under diminished pressure, after recycling design, separates through AB-8 macroporous adsorbent resin, and uses 10
Distilled water and the 60% mass fraction ethanol water of times weight carry out eluting；
5) it is dried: eluent being placed in 55 DEG C of vacuum and concentrates, last lyophilization becomes powder, obtains product.
600g Garcinia mangostana shell is divided into 6 groups be respectively adopted embodiment 1-3 method and organic solvent method, microwave assisting method,
Ultrasonic assistant method contrast test extracts procyanidin, uses Semen Vitis viniferae grasp seed procyanidins as standard substance, configuration standard solution, adopts
Make standard curve by iron salt catalytic colorimetry colorimetric at 550nm, measure and extract product procyanidins content, and by following
Formula calculates yield and purity,
Yield (%)=(product procyanidins quality/Garcinia mangostana chitin amount) × 100%
Purity (%)=(product procyanidins quality/product quality) × 100%
Extract Garcinia mangostana shell procyanidin yield and purity be as shown in the table:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Organic solvent method | Microwave assisting method | Ultrasonic assistant method | |
| Yield | 4.12% | 4.20% | 4.09% | 1.65% | 2.59% | 2.95% |
| Purity | 99.0% | 98.5% | 98.8% | 92.5.3% | 95.6.0% | 97.6% |
Conclude that the purity of product that the method that the present invention provides draws is than organic solvent method, microwave from test result
It is high that auxiliary law, ultrasonic assistant method extract the product purity obtained, constant product quality, and extracts than general procyanidin
Technique yield is high, is about 2.5 times of conventional organic solvent method, about 1.6 times of microwave assisting method, about the 1.4 of ultrasonic assistant method
Times.
Although embodiment of the present invention are disclosed as above, but it is not restricted in description and embodiment listed
Using, it can be applied to various applicable the field of the invention completely, for those skilled in the art, and can be easily
Realizing other amendment, therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention does not limit
In specific details with shown here as the embodiment with description.
Claims (7)
1. the method extracting Garcinia mangostana shell procyanidins, it is characterised in that described method comprises the following steps:
1) being dried by Garcinia mangostana shell, liquid nitrogen crosses 40～80 mesh sieves after pulverizing, and loads container, and it is standby that sealing is stored in 4 DEG C of refrigerators；
2) weighing Garcinia mangostana shell, the feed liquid weight ratio with 1: 10～15 adds ethanol water, then presses 150U/mL addition cellulose
Enzyme, is 4～8 slightly to extract 0.5～1.5h at pH value, filter, reduce pressure, concentrate after obtain concentrated solution, add ether and go grease removal
Compounds, again with methanol extracts with ethyl acetate mixture, adds after water and reduces pressure, removes organic solvent and i.e. obtain slightly
Extract；
3) crude extract is added mass fraction 30% glacial acetic acid aqueous solution by weight 1: 10～20, by crude extract and glacial acetic acid water
Solution is positioned in high-pressure pulse electric extraction 1～2 hour, obtains extracting solution；
4) purification: by extracting solution filtration under diminished pressure, after recycling design, separates through macroporous adsorbent resin, and uses 10 times of heavy steamings
Distilled water and 60% mass fraction ethanol water carry out eluting；
5) it is dried: eluent being placed in 50～60 DEG C of vacuum and concentrates, last lyophilization becomes powder, obtains product.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, is characterized in that: step 2) in slightly extract temperature
Degree is 35～45 DEG C, and ethanol water mass fraction is 60～70%.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, it is characterised in that step 2) described in
Methanol and ethyl acetate weight ratio are 1: 4.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, it is characterised in that step 2) described in
Ether, methanol, ethyl acetate concentration mass fraction are more than 99%, and ether is 1: 1 with the weight ratio of concentrated solution, methanol and acetic acid second
Ester mixed solution is 2: 1 with the weight ratio of concentrated solution.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, it is characterised in that step 3) described in
High-pressure pulse electric electric field intensity is 20～30kV/cm, and umber of pulse is 6～8.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, it is characterised in that step 3) mesohigh arteries and veins
Rush in electric field equipment and extract 2 hours.
The method of extraction Garcinia mangostana shell procyanidins the most according to claim 1, it is characterised in that step 4) described in
Macroporous adsorbent resin is AB-8.
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Cited By (7)
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| CN108991330A (en) * | 2018-06-27 | 2018-12-14 | 广西驰胜农业科技有限公司 | A kind of Siraitia grosvenorii medicine materical crude slice and its preparation method and application |
| CN109362967A (en) * | 2018-11-05 | 2019-02-22 | 华中农业大学 | It is a kind of to alleviate pig oxidative stress, the plant extract feed additive of improvement meat and application |
| CN109678834A (en) * | 2019-01-20 | 2019-04-26 | 林燕 | A kind of preparation method for extracting anthocyanidin from mangosteen peel |
| CN112535237A (en) * | 2020-12-02 | 2021-03-23 | 广州立达尔生物科技股份有限公司 | Mangosteen fermentation extract, preparation method and application |
| WO2022262456A1 (en) * | 2021-06-16 | 2022-12-22 | 河南工业大学 | Method for extracting proanthocyanidins from buckwheat hulls |
| WO2023133660A1 (en) * | 2022-01-11 | 2023-07-20 | 广州工商学院 | Mangosteen shell active substance extraction apparatus and separation method |
| CN116762864A (en) * | 2023-08-17 | 2023-09-19 | 内蒙古蒙牛乳业（集团）股份有限公司 | Yoghurt and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991330A (en) * | 2018-06-27 | 2018-12-14 | 广西驰胜农业科技有限公司 | A kind of Siraitia grosvenorii medicine materical crude slice and its preparation method and application |
| CN109362967A (en) * | 2018-11-05 | 2019-02-22 | 华中农业大学 | It is a kind of to alleviate pig oxidative stress, the plant extract feed additive of improvement meat and application |
| CN109678834A (en) * | 2019-01-20 | 2019-04-26 | 林燕 | A kind of preparation method for extracting anthocyanidin from mangosteen peel |
| CN112535237A (en) * | 2020-12-02 | 2021-03-23 | 广州立达尔生物科技股份有限公司 | Mangosteen fermentation extract, preparation method and application |
| WO2022262456A1 (en) * | 2021-06-16 | 2022-12-22 | 河南工业大学 | Method for extracting proanthocyanidins from buckwheat hulls |
| WO2023133660A1 (en) * | 2022-01-11 | 2023-07-20 | 广州工商学院 | Mangosteen shell active substance extraction apparatus and separation method |
| CN116762864A (en) * | 2023-08-17 | 2023-09-19 | 内蒙古蒙牛乳业（集团）股份有限公司 | Yoghurt and preparation method thereof |
| CN116762864B (en) * | 2023-08-17 | 2023-11-14 | 内蒙古蒙牛乳业（集团）股份有限公司 | Yoghurt and preparation method thereof |
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Application publication date: 20161207 |