CN105949194A - Extraction process for matrine - Google Patents
Extraction process for matrine Download PDFInfo
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- CN105949194A CN105949194A CN201610563924.1A CN201610563924A CN105949194A CN 105949194 A CN105949194 A CN 105949194A CN 201610563924 A CN201610563924 A CN 201610563924A CN 105949194 A CN105949194 A CN 105949194A
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- matrine
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- radix sophorae
- sophorae flavescentis
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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
- C07D471/22—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 systems contains four or more hetero rings
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Abstract
The invention discloses an extraction process for matrine and belongs to the technical field of plant effective ingredient extraction. The method includes the steps that firstly, radix sophorae flavescentis is smashed, and radix sophorae flavescentis powder is prepared; the radix sophorae flavescentis powder and sodium carbonate are mixed and ground, and mixed micro-powder is prepared; then the mixed micro-powder is put in a single-stage type continuous countercurrent ultrasonic extraction machine for ethanol extraction; finally, extracted filtrate is subjected to reduced pressure distillation and drying, and matrine is obtained. Compared with the prior art, by means of the process, the micro-cutting interaction technology is adopted for assisting in matrine extraction, the solubility of matrine in the ethanol solution can be effectively improved in a super micro-powder state, and the precipitation rate of matrine is further increased. In the matrine ethanol extraction process, under the ultrasonic effect, the continuous countercurrent extraction technology is used for assistance, the permeation, dissolution and dispersion speed in the matrine extraction process can be increased, the extraction time is shortened, the use quantity of a solvent can be reduced, and the extraction process for matrine 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 matrine.
Background technology
Natural plants is because its aboundresources, toxic and side effects are little, without Drug resistance, be increasingly subject to the favor of people without advantages such as hazard residues.Composition contained by natural plants is extremely complex, it is divided into effective ingredient, invalid components and toxic component, wherein, cellulose, chlorophyll, natural gum and inorganic salt etc. are considered as invalid components, and 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 its 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 goes mouldy, corrupt, and some are thermo-labile or volatile ingredient is more easily damaged, volatilizees and loses during decocting.Infusion process 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 the operating 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-maceration, it is with volatile organic solvent extraction medicinal ingredients such as ethanol, leachate is added thermal distillation, it is condensed again after wherein volatile solvent distillates, repeat 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 is constantly groped and is optimized by many Chinese scholars, 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 the most progressive than conventional art, but the problem that effective ingredient poorly water-soluble, availability are low the most fundamentally has been resolved, and some technology is special due to equipment, also it is only limitted to laboratory research, and may not apply to Industrialized Production Practice.Visible, the imperfection of extractive technique always governs plant effective active composition deeper into research and the key issue of development and application.Therefore, improve the extraction efficiency of effective ingredient, reduce cost, the Maturity that develops skill thus reach target and the direction that the exploitation always people of the new technique of industrialization production requirements pursue.
Summary of the invention
The purpose of the present invention aims to provide the extraction process of a kind of matrine.
Concrete, the extraction process of matrine of the present invention, with Radix Sophorae Flavescentis as raw material, wherein, comprise the following steps:
(1) take sophora flavescens ait to pulverize, cross 30～60 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate by weight 95～99:1～5 are put into and be ground 10～30min in planetary mills or vibromill, obtain admixed finepowder；
(3) by admixed finepowder and 60～80% ethanol put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8～15ml, frequency be 20～80KHz, power be 300～500w, temperature be 20～50 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 10～30min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2～3 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Radix Sophorae Flavescentis, Chinese medicine name.For the dry root of leguminous plant Radix Sophorae Flavescentis, excavate in spring, season in autumn two, remove root head and little supporting root, cleaning, drying, or take advantage of fresh slices, be dried.It is bitter, cold.There are heat clearing and damp drying, parasite killing, the merit of diuresis.For hematodiarrhoea, have blood in stool, jaundice urine retention, leucorrhea with red and white discharge, swelling of the vulva pudendal pruritus, eczema, eczema, skin pruritus, scabies leprosy, external treatment trichomonal vaginitis.Matrine is made by the dry root of leguminous plant Radix Sophorae Flavescentis, plant, fruit are extracted, main component has the multiple alkaloids such as matrine, sophocarpine, N-oxysophocarpine, sophoridine, it is the class alkaloid with the multiple pharmacological effect such as antitumor, antibacterial and antiviral and effect, there is great Development volue.
The employing micro-cutting interaction technology of the present invention, it is to utilize mechanochemical effect produced by the grinding of high intensity, Radix Sophorae Flavescentis powder can be made to reach micronizing state, thus improve its cell-wall breaking ratio, promote exposure and the release of effective ingredient matrine further, change its micro-property, surface can increase, surface area increases, adsorptivity and polarity increase, for occurring adsorption to provide condition in advance between chemical assistant sodium carbonate and effective ingredient matrine, improve effective ingredient matrine dissolubility in ethanol solution, improve the eduction rate of matrine 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, use Continuous Countercurrent Extraction technology, in extraction tube, keep the most uninterrupted reverse flow state, each section realizes maximum trial gradient, uses minimum solvent to obtain the dissolubility of maximum, reduces solvent load, and whole process uses pipeline closed to produce, and reduces 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 is prone to concentrate energy by focusing on, and therefore the effect between it and ature of coal can be divided into calorifics mechanism, Mechanics of Machinery mechanism and cavitation mechanism 3 kinds.Its action principle is the cavitation effect and mechanical effect utilizing ultrasound wave to produce, and increases solvent and enters the permeability of plant cell, strengthens extract mass transfer rate between plant cell and Extraction medium；And the cavitation bubble that ultrasonic activation produces defines shearing force, form local assault ripple during the collapse of this bubble and high-speed jet can make plant cell rupture, accelerate the release of cellular content.
Compared with prior art, present invention process uses micro-cutting interaction technology assisted extraction matrine, can be effectively improved matrine dissolubility in ethanol solution under superfine powder state, improves the eduction rate of matrine further；During matrine ethanol extraction, under ul-trasonic irradiation, it is aided with employing Continuous Countercurrent Extraction technology, both can accelerate matrine 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 matrine extraction process.
Detailed description of the invention
Being described in further detail the present invention below in conjunction with embodiment, the present embodiment is only that the present invention makees clearer explanation 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 the inventive concept of the premise, 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 matrine, with Radix Sophorae Flavescentis as raw material, specifically includes following steps:
(1) take sophora flavescens ait to pulverize, cross 30 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate 95:5 by weight are put in planetary mills or vibromill and be ground 30min, obtain admixed finepowder；
(3) admixed finepowder and 60% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:15ml, frequency be 20KHz, power be 500w, temperature be 50 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 30min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Embodiment 2
The extraction process of a kind of matrine, with Radix Sophorae Flavescentis as raw material, specifically includes following steps:
(1) take sophora flavescens ait to pulverize, cross 40 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate 96:4 by weight are put in planetary mills or vibromill and be ground 25min, obtain admixed finepowder；
(3) admixed finepowder and 70% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:12ml, frequency be 50KHz, power be 350w, temperature be 40 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 25min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Embodiment 3
The extraction process of a kind of matrine, with Radix Sophorae Flavescentis as raw material, specifically includes following steps:
(1) take sophora flavescens ait to pulverize, cross 50 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate 97:3 by weight are put in planetary mills or vibromill and be ground 20min, obtain admixed finepowder；
(3) admixed finepowder and 70% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:10ml, frequency be 60KHz, power be 350w, temperature be 35 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 15min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Embodiment 4
The extraction process of a kind of matrine, with Radix Sophorae Flavescentis as raw material, specifically includes following steps:
(1) take sophora flavescens ait to pulverize, cross 60 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate 99:1 by weight are put in planetary mills or vibromill and be ground 10min, obtain admixed finepowder；
(3) admixed finepowder and 80% ethanol are put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8ml, frequency be 80KHz, power be 300w, temperature be 35 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 12min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 3 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Claims (1)
1. an extraction process for matrine, with Radix Sophorae Flavescentis as raw material, it is characterised in that comprise the following steps:
(1) take sophora flavescens ait to pulverize, cross 30～60 mesh sieves, obtain Radix Sophorae Flavescentis powder；
(2) Radix Sophorae Flavescentis powder and sodium carbonate by weight 95～99:1～5 are put into and be ground 10～30min in planetary mills or vibromill, obtain admixed finepowder；
(3) by admixed finepowder and 60～80% ethanol put in single stage type continuous flow upstream ultrasonic extractor by solid-liquid ratio 1g:8～15ml, frequency be 20～80KHz, power be 300～500w, temperature be 20～50 DEG C ul-trasonic irradiation under ultrasonic countercurrent extraction 10～30min, filter extracting solution, collect and obtain filtrate and filtering residue；Filtering residue is repeated ultrasonic countercurrent extraction 2～3 times, repeats to filter, finally merge all filtrate, obtain total filtrate；
(4) total filtrate is carried out decompression distillation by rotary distillation instrument, reclaim ethanol, obtain concentrated filtrate；
(5) concentrated filtrate is dried under vacuum, obtains water content matrine below 5%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610563924.1A CN105949194A (en) | 2016-07-18 | 2016-07-18 | Extraction process for matrine |
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| CN201610563924.1A CN105949194A (en) | 2016-07-18 | 2016-07-18 | Extraction process for matrine |
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Citations (7)
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| US7384657B2 (en) * | 2004-10-14 | 2008-06-10 | Jeffrey Young | Composition of natural herb extract for treating cardiovascular disease and its method of preparation thereof |
| KR20100122222A (en) * | 2009-05-12 | 2010-11-22 | 인하대학교 산학협력단 | Method for extracting and separating active constituents from sophora flavescens ait. using liquid-liquid extraction and rp-hplc |
| CN102453030A (en) * | 2010-10-20 | 2012-05-16 | 叶乐珍 | Matrine extraction technology |
| CN103373998A (en) * | 2012-04-14 | 2013-10-30 | 庄芳 | Extraction process of sophocarpidine |
| CN104435090A (en) * | 2013-09-25 | 2015-03-25 | 青岛中人智业生物科技有限公司 | Process for extracting matrine |
| CN105418446A (en) * | 2015-11-30 | 2016-03-23 | 广西恒得润生物科技有限公司 | Method for extracting capsaicin crystals from oleoresin capsicum |
| CN105566944A (en) * | 2015-12-28 | 2016-05-11 | 广西恒得润生物科技有限公司 | Method for separating decolorized chilli extract and chili pigments from chilli extract crude product |
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2016
- 2016-07-18 CN CN201610563924.1A patent/CN105949194A/en active Pending
Patent Citations (7)
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| US7384657B2 (en) * | 2004-10-14 | 2008-06-10 | Jeffrey Young | Composition of natural herb extract for treating cardiovascular disease and its method of preparation thereof |
| KR20100122222A (en) * | 2009-05-12 | 2010-11-22 | 인하대학교 산학협력단 | Method for extracting and separating active constituents from sophora flavescens ait. using liquid-liquid extraction and rp-hplc |
| CN102453030A (en) * | 2010-10-20 | 2012-05-16 | 叶乐珍 | Matrine extraction technology |
| CN103373998A (en) * | 2012-04-14 | 2013-10-30 | 庄芳 | Extraction process of sophocarpidine |
| CN104435090A (en) * | 2013-09-25 | 2015-03-25 | 青岛中人智业生物科技有限公司 | Process for extracting matrine |
| CN105418446A (en) * | 2015-11-30 | 2016-03-23 | 广西恒得润生物科技有限公司 | Method for extracting capsaicin crystals from oleoresin capsicum |
| CN105566944A (en) * | 2015-12-28 | 2016-05-11 | 广西恒得润生物科技有限公司 | Method for separating decolorized chilli extract and chili pigments from chilli extract crude product |
Non-Patent Citations (5)
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Application publication date: 20160921 |