CN106146582A - A kind of method using micro-cutting to help interaction technology assisted extraction Hesperidin - Google Patents
A kind of method using micro-cutting to help interaction technology assisted extraction Hesperidin Download PDFInfo
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- CN106146582A CN106146582A CN201610563918.6A CN201610563918A CN106146582A CN 106146582 A CN106146582 A CN 106146582A CN 201610563918 A CN201610563918 A CN 201610563918A CN 106146582 A CN106146582 A CN 106146582A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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Abstract
The invention discloses a kind of method using micro-cutting to help interaction technology assisted extraction orange skin glycosides up till now, including: orange peel is carried out pretreatment, use micro-cutting help interaction technology carry out mixed grinding, carry out ethanol extraction at single stage type continuous flow upstream ultrasonic extractor, loading resin chromatography post, eluent are dried, and obtain described Hesperidin.Compared with prior art, the inventive method uses micro-cutting interaction technology assisted extraction Hesperidin, can be effectively improved Hesperidin dissolubility in ethanol solution under superfine powder state, improves the eduction rate of Hesperidin further；During Hesperidin ethanol extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate Hesperidin and extract the speed that process infiltration is dissolved and spread, shorten extraction time, solvent usage amount can be reduced again, be a kind of high efficiency, low consumed Hesperidin extracting method.
Description
Technical field
The invention belongs to effective ingredients in plant extractive technique field, be specifically related to a kind of employing micro-cutting and help interaction technology to assist
The method extracting Hesperidin.
Background technology
Natural plants is because its aboundresources, toxic and side effects are little, without Drug resistance, be increasingly subject to people without advantages such as hazard residues
Favor.Composition contained by natural plants is extremely complex, is divided into effective ingredient, invalid components and toxic component, wherein, fiber
Element, chlorophyll, natural gum and inorganic salt etc. are considered as invalid components, pigment, alkaloid, flavone, coumarin, water quality element, terpenoid,
Glycoside, organic acid and trace element etc. are effective ingredient.The extracting method of natural plants effective active composition is a lot, and it is traditional
Extracting method mainly has decocting method, infusion process, reflux extraction etc..Decocting method is convenient and easy, but the impurity in fried liquid is more,
Easily go mouldy, corrupt, some are thermo-labile or volatile ingredient is more easily damaged, volatilizees and loses during decocting.Leaching
Stain method is a kind of method that comparison is easy and conventional, it is adaptable to the volatile medical material with destructible of effective ingredient heat, but operation
Time is long, and effective ingredient is often difficult to leach completely.Reflux extraction can be divided into backflow hot dipping and circulating reflux cold
Leaching method, is with volatile organic solvent extraction medicinal ingredients such as ethanol, leachate is added thermal distillation, and wherein volatile solvent evaporates
It is condensed again after going out, repeats to flow back to infuser extracts medical material, until effective ingredient reflux, extract, method completely.
In the last few years, the technique of plant effective active constituents extraction was constantly groped with excellent by many Chinese scholars
Changing, some new extractions and isolation technics constantly emerge in large numbers appearance, such as microwave, ultrasound wave, micronizing, supercritical etc., although
These new techniques have significantly progressive than conventional art, but the low problem of effective ingredient poorly water-soluble, availability is not also from root
Have been resolved on Ben, and some technology is special due to equipment, be also only limitted to laboratory research, and may not apply to industry metaplasia
Produce practice.Visible, the imperfection of extractive technique always govern plant effective active composition deeper into research and exploitation and
The key issue of application.Therefore, improve effective ingredient extraction efficiency, reduce cost, the Maturity that develops skill thus reach work
The exploitation of the new technique of the industry production requirement target that always people pursue and direction.
Summary of the invention
The purpose of the present invention aims to provide a kind of method using micro-cutting to help interaction technology assisted extraction Hesperidin.
Concrete, employing micro-cutting of the present invention helps the method for interaction technology assisted extraction Hesperidin, with orange peel is
Raw material, comprises the following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 30～60 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate are put into by weight 95～99:1～5 planetary mills or vibromill are ground 10～
30min, obtains admixed finepowder；
(3) by admixed finepowder and 50～65% ethanol put into single stage type continuous flow upstream ultrasonic extraction by solid-liquid ratio 1g:8～15ml
In machine, frequency be 20～80KHz, power be 300～500w, temperature be 20～50 DEG C ul-trasonic irradiation under ultrasonic adverse current carry
Take 10～30min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2～3 times, repeated
Filter, finally merges all filtrate, obtains total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to resin chromatography post loading, successively use distilled water and 5～10% ethanol aqueous wash removing
Decontamination, then with 50～65% ethanol water eluting obtain eluent, flow speed control is 20～50mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Further illustrating as the present invention, resin used by described resin chromatography post is D901 type macroporous adsorbent resin.
The Citrus resource of China is the abundantest, but the current utilization to Citrus is also limited to the utilization to citrusfruit
Outward, other fail to be fully used such as orange peel.Orange peel accounts for the 20% of whole fruit weight, and common processing method is
Being discarded, this causes the biggest waste, also causes pollution to environment simultaneously.Except containing moisture, fiber in orange peel
Outside element, lignin, orange peel is possibly together with abundant pigment, pectin, Hesperidin, essential oil etc..Therefore, orange peel utilizes
One of main path is just around the extraction of its ingredient and launches, as therefrom extracted pigment, pectin, Hesperidin, essence
Oil, dietary fiber etc..Wherein Hesperidin is the one of flavone compound, discovered in recent years its there is blood pressure lowering, antiallergic, fall
Low bone density, cholesterol, the internal enzymatic activity of change, improve microcirculation, antibacterial, antiinflammatory, anti-hepatitis, the pharmacological action such as anticancer, be
Treatment hypertension and the medicine of myocardial infarction, is used as the raw material of pharmacy in medical industry, be Chinese patent medicine beniol mainly comprise it
One.
The employing micro-cutting interaction technology of the present invention, is to utilize mechanochemical effect produced by the grinding of high intensity, can make
Obtain Pericarpium Citri junoris powder and reach micronizing state, thus improve its cell-wall breaking ratio, promote the exposure of effective ingredient Hesperidin further
With release, changing its micro-property, surface can increase, and surface area increases, and adsorptivity and polarity increase, for chemical assistant sodium carbonate
And occur adsorption to provide in advance condition between effective ingredient Hesperidin, improve molten in ethanol solution of effective ingredient Hesperidin
Xie Xing, improves the eduction rate of Hesperidin further.
Further, under the effect of ultrasound wave, accelerate the infiltration of extraction process and dissolve and the speed of diffusion, shorten extraction
Time；Meanwhile, using Continuous Countercurrent Extraction technology, keep the most uninterrupted reverse flow state in extraction tube, each section realizes
Big trial gradient, uses minimum solvent to obtain the dissolubility of maximum, reduces solvent load, and whole process uses pipeline closed
Produce, reduce solvent loss.
Ultrasound wave refers to that frequency is 2 × 104～109The sound wave of Hz.Owing to ultrasound wave has that wavelength is short, beam strong and easily
In by focusing on the feature concentrating energy, therefore the effect between it and ature of coal can be divided into calorifics mechanism, Mechanics of Machinery machine-processed and empty
Change mechanism 3 kinds.Its action principle is the cavitation effect and mechanical effect utilizing ultrasound wave to produce, and increases solvent and enters plant cell
Permeability, strengthen extract mass transfer rate between plant cell and Extraction medium；And the cavitation that ultrasonic activation produces
Bubble formation shearing force, forms local assault ripple during the collapse of this bubble and high-speed jet can make the plant cell rupture, accelerate
The release of cellular content.
Compared with prior art, the inventive method uses micro-cutting interaction technology assisted extraction Hesperidin, in superfine powder state
Hesperidin dissolubility in ethanol solution can be effectively improved down, improve the eduction rate of Hesperidin further；At Hesperidin ethanol
During extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate Hesperidin and extract process infiltration
Dissolve and the speed of diffusion, shorten extraction time, solvent usage amount can be reduced again, be a kind of high efficiency, low consumed Pericarpium Citri junoris
Glycosides extracting method.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, the present embodiment be only the present invention is made clearer
Illustrate rather than limitation of the present invention.It should be pointed out that, for the person of ordinary skill of the art, without departing from this
On the premise of bright design, it is also possible to make some deformation and improvement, within these all fall within protection scope of the present invention.
Embodiment 1
Use the micro-cutting method that helps interaction technology assisted extraction Hesperidin, with orange peel as raw material, specifically include following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 40 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate 95:5 by weight are put in planetary mills or vibromill and be ground 20min, must mix micro-
Powder；
(3) admixed finepowder and 55% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:12ml,
Frequency is 50KHz, power is 350w, temperature is ultrasonic countercurrent extraction 20min under the ul-trasonic irradiation of 35 DEG C, filters extracting solution,
Collection obtains filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain and always filter
Liquid；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 10% ethanol water successively
Eluant solution removes impurity, then obtains eluent with 55% ethanol water eluting, and flow speed control is 35mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Embodiment 2
Use the micro-cutting method that helps interaction technology assisted extraction Hesperidin, with orange peel as raw material, specifically include following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 50 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate 98:2 by weight are put in planetary mills or vibromill and be ground 10min, must mix micro-
Powder；
(3) admixed finepowder and 50% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:15ml,
Frequency is 80KHz, power is 350w, temperature is ultrasonic countercurrent extraction 20min under the ul-trasonic irradiation of 20 DEG C, filters extracting solution,
Collection obtains filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2 times, repeats to filter, finally merge all filtrate, obtain and always filter
Liquid；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 5% ethanol water successively
Eluant solution removes impurity, then obtains eluent with 65% ethanol water eluting, and flow speed control is 50mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Embodiment 3
Use the micro-cutting method that helps interaction technology assisted extraction Hesperidin, with orange peel as raw material, specifically include following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 60 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate 99:1 by weight are put in planetary mills or vibromill and be ground 10min, must mix micro-
Powder；
(3) admixed finepowder and 60% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8ml, at frequency
Rate is 20KHz, power is 500w, temperature is ultrasonic countercurrent extraction 30min under the ul-trasonic irradiation of 20 DEG C, filters extracting solution, receives
Collection obtains filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain and always filter
Liquid；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 5% ethanol water successively
Eluant solution removes impurity, then obtains eluent with 55% ethanol water eluting, and flow speed control is 30mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Embodiment 4
Use the micro-cutting method that helps interaction technology assisted extraction Hesperidin, with orange peel as raw material, specifically include following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 30 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate 93:7 by weight are put in planetary mills or vibromill and be ground 30min, must mix micro-
Powder；
(3) admixed finepowder and 55% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:10ml,
Frequency is 50KHz, power is 350w, temperature is ultrasonic countercurrent extraction 15min under the ul-trasonic irradiation of 25 DEG C, filters extracting solution,
Collection obtains filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain and always filter
Liquid；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 8% ethanol water-soluble successively
Liquid eluting removes impurity, then obtains eluent with 55% ethanol water eluting, and flow speed control is 40mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Claims (2)
1. using the method that micro-cutting helps interaction technology assisted extraction Hesperidin, with orange peel for raw material as raw material, it is special
Levy and be, comprise the following steps:
(1) take orange peel to clean, be dried the most under vacuum, control dried orange peel water content below 5%,
Then dried orange peel is pulverized, cross 30～60 mesh sieves, obtain Pericarpium Citri junoris powder；
(2) Pericarpium Citri junoris powder and sodium carbonate are put into by weight 95～99:1～5 planetary mills or vibromill are ground 10～
30min, obtains admixed finepowder；
(3) by admixed finepowder and 50～65% ethanol put into single stage type continuous flow upstream ultrasonic extraction by solid-liquid ratio 1g:8～15ml
In machine, frequency be 20～80KHz, power be 300～500w, temperature be 20～50 DEG C ul-trasonic irradiation under ultrasonic adverse current carry
Take 10～30min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2～3 times, repeated
Filter, finally merges all filtrate, obtains total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is added to resin chromatography post loading, successively use distilled water and 5～10% ethanol aqueous wash removing
Decontamination, then with 50～65% ethanol water eluting obtain eluent, flow speed control is 20～50mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Hesperidin.
Use the method that micro-cutting helps interaction technology assisted extraction Hesperidin the most according to claim 1, it is characterised in that described
Resin used by resin chromatography post is D901 type macroporous adsorbent resin.
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Cited By (9)
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| CN106581318A (en) * | 2016-12-20 | 2017-04-26 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode |
| CN106699915A (en) * | 2016-12-20 | 2017-05-24 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of polysaccharide of grapeseed extract through pressure-shear induced chemical transition |
| CN106728480A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract polyphenol dissolution rate using micro- |
| CN106728481A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract saponin(e dissolution rate using micro- |
| CN108383886A (en) * | 2018-05-08 | 2018-08-10 | 湘西华方制药有限公司 | The aurantiamarin that continuous countercurrent technique extracts the method for aurantiamarin from the dried immature fruit of citron orange and extraction obtains |
| CN111362994A (en) * | 2020-04-17 | 2020-07-03 | 严格生物科技产业发展有限公司 | Novel process method for extracting hesperidin by using countercurrent |
| CN111979049A (en) * | 2020-08-26 | 2020-11-24 | 云南中烟工业有限责任公司 | Component directional preparation method |
| CN112402504A (en) * | 2020-11-17 | 2021-02-26 | 哈工大机器人南昌智能制造研究院 | Method for continuously preparing citrus flavonoid |
| CN113150869A (en) * | 2021-04-02 | 2021-07-23 | 江南大学 | Method for continuously extracting essential oil, pectin and hesperidin from orange peel |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106581318A (en) * | 2016-12-20 | 2017-04-26 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of grape seed extract flavones in press-shear assisted interaction mode |
| CN106699915A (en) * | 2016-12-20 | 2017-05-24 | 大连赛姆生物工程技术有限公司 | Method for improving dissolution rate of polysaccharide of grapeseed extract through pressure-shear induced chemical transition |
| CN106728480A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract polyphenol dissolution rate using micro- |
| CN106728481A (en) * | 2016-12-20 | 2017-05-31 | 大连赛姆生物工程技术有限公司 | It is a kind of to cut the method for helping interaction mode to improve grape seed extract saponin(e dissolution rate using micro- |
| CN108383886A (en) * | 2018-05-08 | 2018-08-10 | 湘西华方制药有限公司 | The aurantiamarin that continuous countercurrent technique extracts the method for aurantiamarin from the dried immature fruit of citron orange and extraction obtains |
| CN108383886B (en) * | 2018-05-08 | 2021-06-18 | 湘西华方制药有限公司 | Method for extracting hesperidin from immature bitter orange by continuous countercurrent method and hesperidin obtained by extraction |
| CN111362994A (en) * | 2020-04-17 | 2020-07-03 | 严格生物科技产业发展有限公司 | Novel process method for extracting hesperidin by using countercurrent |
| CN111362994B (en) * | 2020-04-17 | 2023-12-22 | 严格生物科技产业发展有限公司 | Process method for extracting hesperidin by utilizing countercurrent |
| CN111979049A (en) * | 2020-08-26 | 2020-11-24 | 云南中烟工业有限责任公司 | Component directional preparation method |
| CN112402504A (en) * | 2020-11-17 | 2021-02-26 | 哈工大机器人南昌智能制造研究院 | Method for continuously preparing citrus flavonoid |
| CN113150869A (en) * | 2021-04-02 | 2021-07-23 | 江南大学 | Method for continuously extracting essential oil, pectin and hesperidin from orange peel |
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