CN106189351A - A kind of process extracting safflower yellow from Flos Carthami - Google Patents
A kind of process extracting safflower yellow from Flos Carthami Download PDFInfo
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- CN106189351A CN106189351A CN201610564085.5A CN201610564085A CN106189351A CN 106189351 A CN106189351 A CN 106189351A CN 201610564085 A CN201610564085 A CN 201610564085A CN 106189351 A CN106189351 A CN 106189351A
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- flos carthami
- safflower yellow
- ethanol
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having no double bonds between ring members or between ring members and non-ring members
- C07D309/08—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D309/10—Oxygen atoms
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of process extracting safflower yellow from Flos Carthami, including: Flos Carthami 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 safflower yellow.Compared with prior art, the inventive method uses micro-cutting interaction technology assisted extraction safflower yellow, can be effectively improved safflower yellow dissolubility in ethanol solution under superfine powder state, improves the eduction rate of safflower yellow further；During safflower yellow ethanol extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate safflower yellow 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 safflower yellow extracting method.
Description
Technical field
The invention belongs to effective ingredients in plant extractive technique field, be specifically related to a kind of from Flos Carthami, extract safflower yellow
Process.
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 process extracting safflower yellow from Flos Carthami.
Concrete, the process extracting safflower yellow from Flos Carthami of the present invention, comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 30～60 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami 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 30～45% 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 safflower yellow.
Further illustrating as the present invention, resin used by described resin chromatography post is D901 type macroporous adsorbent resin.
Flos Carthami, for the dry flower of feverfew Flos Carthami Carthamus tinctorius L..Summer flower by xanthochromia red time adopt
Pluck, dry in the shade or dry.Extensively there is cultivation all parts of the country.There is promoting blood circulation to restore menstrual flow, effect of eliminating stasis to stop pain.For amenorrhea, dysmenorrhea, lochia
Not all right, lump in the abdomen mass in the abdomen, obstruction of qi in the chest and cardialgia, the stagnant stomachache of the stasis of blood, breast side of body twinge, injury from falling down, skin infection swells and ache.Safflower yellow is from Flos Carthami
The flavone compound extracted, lists the national drug standards in using the new drug as treatment cardiovascular and cerebrovascular disease, is a kind of toxicity pole
Natural pigment low, that strong coloring force, tone are stable, is the reason of various refreshment drink, cake, confection, varieties of food items and cosmetics
Keep in mind toner, there is the advantages such as beautiful in colour, high-low temperature resistant, high pressure resistant, fast light, acidproof, reducing resistance and antimicrobial, have
The highest use use value and DEVELOPMENT PROSPECT.
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 Flos Carthami powder and reach micronizing state, thus improve its cell-wall breaking ratio, promote the sudden and violent of effective ingredient safflower yellow further
Dew and release, change its micro-property, and surface can increase, and surface area increases, and adsorptivity and polarity increase, for chemical assistant carbonic acid
Occur adsorption to provide condition in advance between sodium and effective ingredient safflower yellow, improve effective ingredient safflower yellow at ethanol solution
In dissolubility, improve further the eduction rate of safflower yellow.
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 safflower yellow, at ultra micro powdery
Safflower yellow dissolubility in ethanol solution can be effectively improved under state, improve the eduction rate of safflower yellow further；At Flos Carthami
During flavin ethanol extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate safflower yellow and carry
Take process infiltration to dissolve and the speed of diffusion, shorten extraction time, solvent usage amount can be reduced again, be a kind of high efficiency, low
The safflower yellow extracting method consumed.
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
A kind of process extracting safflower yellow from Flos Carthami, specifically includes following steps:
Concrete, the process extracting safflower yellow from Flos Carthami of the present invention, comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 30 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami powder and sodium carbonate 96:4 by weight are put in planetary mills or vibromill and be ground 15min, 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 30KHz, power is 500w, temperature is ultrasonic countercurrent extraction 15min 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 8% ethanol water successively
Eluant solution removes impurity, then obtains eluent with 35% ethanol water eluting, and flow speed control is 35mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain safflower yellow.
Embodiment 2
A kind of process extracting safflower yellow from Flos Carthami, specifically includes following steps:
Concrete, the process extracting safflower yellow from Flos Carthami of the present invention, comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 40 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami powder and sodium carbonate 98:2 by weight are put in planetary mills or vibromill and be ground 25min, 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 60KHz, power is 350w, temperature is ultrasonic countercurrent extraction 20min under the ul-trasonic irradiation of 30 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 10% ethanol water successively
Eluant solution removes impurity, then obtains eluent with 30% ethanol water eluting, and flow speed control is 50mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain safflower yellow.
Embodiment 3
A kind of process extracting safflower yellow from Flos Carthami, specifically includes following steps:
Concrete, the process extracting safflower yellow from Flos Carthami of the present invention, comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 50 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami powder and sodium carbonate 99:1 by weight are put in planetary mills or vibromill and be ground 30min, must mix micro-
Powder；
(3) admixed finepowder and 65% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:10ml,
Frequency is 80KHz, power is 300w, temperature is ultrasonic countercurrent extraction 30min 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 40% ethanol water eluting, and flow speed control is 25mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain safflower yellow.
Embodiment 4
A kind of process extracting safflower yellow from Flos Carthami, specifically includes following steps:
Concrete, the process extracting safflower yellow from Flos Carthami of the present invention, comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 60 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami powder and sodium carbonate 95:5 by weight are put in planetary mills or vibromill and be ground 25min, must mix micro-
Powder；
(3) admixed finepowder and 65% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8ml, at frequency
Rate is 50KHz, power is 300w, temperature is ultrasonic countercurrent extraction 20min under the ul-trasonic irradiation of 50 DEG C, filters extracting solution, receives
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 8% ethanol water-soluble successively
Liquid eluting removes impurity, then obtains eluent with 40% ethanol water eluting, and flow speed control is 35mL/min；
(6) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain safflower yellow.
Claims (2)
1. the process extracting safflower yellow from Flos Carthami, it is characterised in that comprise the following steps:
(1) take Flos Carthami to clean, be dried the most under vacuum, control dried Flos Carthami water content below 5%, then will be dry
Flos Carthami after dry is pulverized, and crosses 30～60 mesh sieves, obtains Flos Carthami powder；
(2) Flos Carthami 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 30～45% 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 safflower yellow.
The process of safflower yellow is extracted the most according to claim 1, it is characterised in that described resin chromatography from Flos Carthami
Resin used by post is D901 type macroporous adsorbent resin.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111334116A (en) * | 2020-03-31 | 2020-06-26 | 吴永淇 | Environment-friendly printing ink |
| CN111944329A (en) * | 2020-09-09 | 2020-11-17 | 江西丹霞生物科技股份有限公司 | Preparation process for preparing carthamus red pigment and product thereof |
| CN112679451A (en) * | 2020-12-31 | 2021-04-20 | 福建师范大学 | Method for extracting fucoxanthin from gulfweed |
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| CN112679451A (en) * | 2020-12-31 | 2021-04-20 | 福建师范大学 | Method for extracting fucoxanthin from gulfweed |
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Application publication date: 20161207 |