CN105949191A - Technology for extracting borreria stricta alkali - Google Patents
Technology for extracting borreria stricta alkali Download PDFInfo
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- CN105949191A CN105949191A CN201610563926.0A CN201610563926A CN105949191A CN 105949191 A CN105949191 A CN 105949191A CN 201610563926 A CN201610563926 A CN 201610563926A CN 105949191 A CN105949191 A CN 105949191A
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- borreria stricta
- alkali
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- mey
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains two hetero rings
- C07D471/04—Ortho-condensed systems
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a technology for extracting borreria stricta alkali. The technology includes the steps that borreria stricta is pretreated, mixing and grinding are carried out with the mechanochemical technology, ethanol extraction, active carbon decoloration, petroleum ether extraction, sample resin chromatographic column feeding and eluent drying are carried out in a single-grade continuous adverse-current ultrasonic extractor, and borreria stricta alkali is obtained. Compared with the prior art, the technology has the advantages that extraction of borreria stricta alkali is assisted with the mechanochemical technology, the solubility of borreria stricta alkali in an ethanol solution can be effectively improved in the ultramicro-pulverized powder state, and the separating-out rate of borreria stricta alkali is further increased; in the ethanol extraction process of borreria stricta alkali, under the effect of ultrasonic waves, the permeating, dissolving and dispersing speeds in the borreria stricta alkali extraction process can be increased in cooperation with the continuous adverse-flow extraction technology, extraction time is shortened, the use quantity of solvents can be decreased, and the technology for extracting borreria stricta alkali is high in efficiency and low in consumption.
Description
Technical field
The invention belongs to effective ingredients in plant extractive technique field, be specifically related to the extraction process of a kind of Borrerine.
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 the extraction process of a kind of Borrerine.
Concrete, the extraction process of employing Borrerine of the present invention, with Borreria stricta (L. f.) G. Mey. as raw material, wherein, including following
Step:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 30～60 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. 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 70～90% 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) add concentrated filtrate weight 2～5% activated carbon adsorption pigment until supernatant is without color, be subsequently added into concentrated filtrate
The petroleum ether of weight 2～5 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract is added to resin chromatography post loading, successively use distilled water and 5～10% ethanol aqueous wash removing go
Impurity, then with 30～50% ethanol water eluting obtain eluent, flow speed control is 20～50mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
Further illustrating as the present invention, resin used by described resin chromatography post is D901 type macroporous adsorbent resin.
Borrerine, molecular formula is C16H20ON2, molecular weight is 240.35, is to extract to divide from the verticillate Borreria stricta (L. f.) G. Mey. of Rubiaceae
From a kind of carboline alkaloid compounds.Experimental study shows, rich colored alkali has antimicrobial acivity, to Staphylococcus aureus
Bacterium and some enterobacteria are active, and have cytotoxic activity, have high cell cytotoxic activity when 3-6 μ g/ml.
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 Borreria stricta (L. f.) G. Mey. powder and reach micronizing state, thus improve its cell-wall breaking ratio, promote effective ingredient Borrerine further
Exposing and release, change its micro-property, surface can increase, and surface area increases, and adsorptivity and polarity increase, for chemical assistant carbon
Occur adsorption to provide condition in advance between acid sodium and effective ingredient Borrerine, improve effective ingredient Borrerine molten at ethanol
Dissolubility in liquid, improves the eduction rate of Borrerine 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, present invention process uses micro-cutting interaction technology assisted extraction Borrerine, at ultra micro powdery
Borrerine dissolubility in ethanol solution can be effectively improved under state, improve the eduction rate of Borrerine further；At rich flower
During potash ethanol extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate Borrerine 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 Borrerine extraction process 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
The extraction process of a kind of Borrerine, with Borreria stricta (L. f.) G. Mey. as raw material, specifically includes following steps:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 40 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. powder and sodium carbonate 95:5 by weight are put in planetary mills or vibromill and be ground 20min, obtain mixing
Micropowder；
(3) admixed finepowder and 70% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:15ml,
Frequency is 50KHz, power is 350w, temperature is ultrasonic countercurrent extraction 20min under the ul-trasonic irradiation of 40 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) the activated carbon adsorption pigment of addition concentrated filtrate weight 4% is until supernatant is without color, is subsequently added into concentrated filtrate weight
The petroleum ether measuring 3 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 10% ethanol water-soluble successively
Liquid eluting removes impurity, then obtains eluent with 40% ethanol water eluting, and flow speed control is 35mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
Embodiment 2
The extraction process of a kind of Borrerine, with Borreria stricta (L. f.) G. Mey. as raw material, specifically includes following steps:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 50 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. powder and sodium carbonate 96:4 by weight are put in planetary mills or vibromill and be ground 25min, obtain mixing
Micropowder；
(3) admixed finepowder and 80% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:10ml,
Frequency is 20KHz, power is 500w, temperature is ultrasonic countercurrent extraction 15min under the ul-trasonic irradiation of 40 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) the activated carbon adsorption pigment of addition concentrated filtrate weight 2% is until supernatant is without color, is subsequently added into concentrated filtrate weight
The petroleum ether measuring 5 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 5% ethanol water successively
Eluting removes impurity, then obtains eluent with 30% ethanol water eluting, and flow speed control is 35mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
Embodiment 3
The extraction process of a kind of Borrerine, with Borreria stricta (L. f.) G. Mey. as raw material, specifically includes following steps:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 50 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. powder and sodium carbonate 97:3 by weight are put in planetary mills or vibromill and be ground 30min, obtain mixing
Micropowder；
(3) admixed finepowder and 90% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:12ml,
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 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) the activated carbon adsorption pigment of addition concentrated filtrate weight 5% is until supernatant is without color, is subsequently added into concentrated filtrate weight
The petroleum ether measuring 2 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract 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 50% ethanol water eluting, and flow speed control is 50mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
Embodiment 4
The extraction process of a kind of Borrerine, with Borreria stricta (L. f.) G. Mey. as raw material, specifically includes following steps:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 60 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. powder and sodium carbonate 99:1 by weight are put in planetary mills or vibromill and be ground 10min, obtain mixing
Micropowder；
(3) admixed finepowder and 80% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8ml, at frequency
Rate is 30KHz, power is 350w, temperature is ultrasonic countercurrent extraction 25min under the ul-trasonic irradiation of 35 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) the activated carbon adsorption pigment of addition concentrated filtrate weight 3% is until supernatant is without color, is subsequently added into concentrated filtrate weight
The petroleum ether measuring 3 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract is added to D901 type macroporous adsorption resin chromatography post loading, uses distilled water and 8% ethanol water successively
Eluting removes impurity, then obtains eluent with 10% ethanol water eluting, and flow speed control is 30mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
Claims (2)
1. an extraction process for Borrerine, with Borreria stricta (L. f.) G. Mey. as raw material, it is characterised in that comprise the following steps:
(1) take Borreria stricta (L. f.) G. Mey. to remove root, clean, be dried the most under vacuum, control dried Borreria stricta (L. f.) G. Mey. water content below 5%,
Then dried Borreria stricta (L. f.) G. Mey. is pulverized, cross 30～60 mesh sieves, obtain Borreria stricta (L. f.) G. Mey. powder；
(2) Borreria stricta (L. f.) G. Mey. 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 70～90% 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) add concentrated filtrate weight 2～5% activated carbon adsorption pigment until supernatant is without color, be subsequently added into concentrated filtrate
The petroleum ether of weight 2～5 times extracts, and then carries out sucking filtration, isolated extract；
(6) extract is added to resin chromatography post loading, successively use distilled water and 5～10% ethanol aqueous wash removing go
Impurity, then with 30～50% ethanol water eluting obtain eluent, flow speed control is 20～50mL/min；
(7) eluent is carried out concentrating under reduced pressure, be dried under vacuum, obtain Borrerine.
The extraction process of Borrerine the most according to claim 1, it is characterised in that resin used by described resin chromatography post is
D901 type macroporous adsorbent resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610563926.0A CN105949191A (en) | 2016-07-18 | 2016-07-18 | Technology for extracting borreria stricta alkali |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610563926.0A CN105949191A (en) | 2016-07-18 | 2016-07-18 | Technology for extracting borreria stricta alkali |
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| CN201610563926.0A Pending CN105949191A (en) | 2016-07-18 | 2016-07-18 | Technology for extracting borreria stricta alkali |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649791A (en) * | 2012-04-25 | 2012-08-29 | 南京泽朗医药科技有限公司 | Method for extracting borrerine |
| CN104490894A (en) * | 2014-12-01 | 2015-04-08 | 中国科学院华南植物园 | Preparation method of spermacoce latifolia triterpenoids and application of spermacoce latifolia triterpenoid in preparation of glycosidase inhibitor medicine |
-
2016
- 2016-07-18 CN CN201610563926.0A patent/CN105949191A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649791A (en) * | 2012-04-25 | 2012-08-29 | 南京泽朗医药科技有限公司 | Method for extracting borrerine |
| CN104490894A (en) * | 2014-12-01 | 2015-04-08 | 中国科学院华南植物园 | Preparation method of spermacoce latifolia triterpenoids and application of spermacoce latifolia triterpenoid in preparation of glycosidase inhibitor medicine |
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