CN104961739A - Method for extracting eulexine from aboveground parts of thermopsis lanceolate - Google Patents
Method for extracting eulexine from aboveground parts of thermopsis lanceolate Download PDFInfo
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- CN104961739A CN104961739A CN201510435047.5A CN201510435047A CN104961739A CN 104961739 A CN104961739 A CN 104961739A CN 201510435047 A CN201510435047 A CN 201510435047A CN 104961739 A CN104961739 A CN 104961739A
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- thermopsis
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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 a method for extracting eulexine from aboveground parts of thermopsis lanceolate. A specific cationic resin is adopted as a major separation carrier to extract the eulexine extract. The raw materials adopted in the method refer to the aboveground parts of the thermopsis lanceolate at the flowering phase, and the fluid extract of the aboveground parts of the thermopsis lanceolate can be obtained by virtue of conventional methanol thermal reflux extraction and concentration. The extract is dissolved in an inorganic acid and then filtered; the pH value of the filtrate is approximately regulated to the range of 8-12 by use of ammonia water and the like; after partial impurities are removed by virtue of chromatographic separation by using the cationic resin, the filtrate is eluted by use of ammoniacal ethanol, and then the eluate containing the eulexine is concentrated and dried to obtain the eulexine extract, wherein the content of the eulexine can be above 43%. The method is used for overcoming the problem that the existing method for extracting the eulexine is not available for taking the aboveground parts of the thermopsis lanceolate as the raw materials, and the method has the characteristics of simple and convenient operation, low dosage of organic solvents, relatively low cost, easy industrial production and the like.
Description
Technical field
The invention belongs to effective ingredients in plant separation and extraction technology field, be specifically related to the method extracting Tocosamine from experiment of general alkaloid of Thermopsis over-ground part.
Background technology
Tocosamine is a kind of to α
4β
2nAChR has the partial agonist of high-affinity, is also the relatively low and smoking cessation composition of successful of a kind of price.
Although experiment of general alkaloid of Thermopsis seed position is the traditional raw material of extraction and isolation Tocosamine, but because this kind of plant is wild species, the output climate of seed and the impact of own growth physiological condition larger, be not suitable for as a large amount of industrial raw material, and this kind of plant is perennial herb, at the pasture dominant species that Northern grassland is main, aboundresources, also be simultaneously harm livestock industry mainly contain poisonous plant, the alkaloid comprising Tocosamine etc. at the florescence is higher, as the raw material extracting Tocosamine, both there is higher economic benefit, also there is obvious social benefit.
At present, the seed of the industrial extraction method of Tocosamine mainly experiment of general alkaloid of Thermopsis experiment of general alkaloid of Thermopsis (T.lanceolata R.Br.) is raw material, be main carrier of separating with organic solvent, as (Inner Mongol Normal University's journal natural science (Chinese) version such as Wu Yong " Study on Extraction Method of high purity Tocosamine ", 2004,33:186-187) and Chinese patent ZL200910023485.5 etc.Detect according to the present inventor; this aboveground vegetation part be in seed Tocosamine be about 1/2 of content; and impurity alkaloid (pharmaceutical analysis magazine as larger in proportions such as N-formyl radical Tocosamine, N-Methylcytisines; 2014; 34:1737-1740), further abstraction and purification Tocosamine is difficult to.In addition, existing technique needs to use a large amount of low boiling point organic solvent, and as methylene dichloride or trichloromethane or ethyl acetate etc., cost is high, and therefore existing Tocosamine scale production process has larger limitation.
Other adopt experiment of general alkaloid of Thermopsis over-ground part or herb as the method being separated Tocosamine, generally using silica gel etc. as main carrier of separating, with mixed organic solvents wash-outs such as chloroform-methanols, Tocosamine loss is serious, auxiliary material is difficult to recycle, complex process, causes cost high, is difficult to realize industrial applications.
Summary of the invention
The object of this invention is to provide a kind of method extracting Tocosamine from experiment of general alkaloid of Thermopsis over-ground part, the problem that it is raw material that the method that instant invention overcomes existing extraction Tocosamine is not suitable for experiment of general alkaloid of Thermopsis over-ground part, have easy and simple to handle, consumption of organic solvent is few, cost is lower, is easy to the features such as suitability for industrialized production.
The inventive method with the experiment of general alkaloid of Thermopsis over-ground part of steady sources for raw material, be main carrier of separating with the better resin cation (R.C.) of economy, hydrogen form cation resin is passed through after regulating the pH value of experiment of general alkaloid of Thermopsis over-ground part extracting solution, after deionized water wash-out impurity, again with ammonia ethanol elution Tocosamine, obtain Tocosamine finally by concentrated, dry, easy and simple to handle, extraction yield is high.
Extract a method for Tocosamine from experiment of general alkaloid of Thermopsis over-ground part, concrete operation step is as follows:
1, extract: after the over-ground part crushed after being dried at experiment of general alkaloid of Thermopsis florescence, with ethanol or methyl alcohol circumfluence distillation 2-3 time, concentration and recovery organic solvent after extracting liquid filtering, obtains the experiment of general alkaloid of Thermopsis extracting solution that proportion is 1.05-1.10;
2, organic solvent removal of impurities: by said extracted liquid with about inorganic acid for adjusting pH to 2, with equivalent extraction into ethyl acetate 2 times, stripped acidic aqueous solution is for subsequent use after reclaiming organic solvent;
3, the preparation of sample solution: above-mentioned acidic aqueous solution alkaline reagents is regulated about pH to 8-12, controls the content of Tocosamine in the aqueous solution not higher than 30mg/mL simultaneously, both obtained sample solution;
4, cation separation: by sample solution by Hydrogen 001 × 7 type Zeo-karb, with the abundant washing resin of deionized water to reacting (Dragendorff reagent) without obvious alkaloid, again with ammonia alcohol mixed solution as eluting solvent wash-out resin to reacting (Dragendorff reagent) without obvious alkaloid, merge elutriant, concentrated, dry, both obtained Tocosamine extract.
Wherein strong acidic ion resin refers to vinylbenzene and divinylbenzene polymer for skeleton, with strong acid group sulfonic group (-SO
3h) be the resin of cation exchange groups.
Wherein adsorbed the resin cation (R.C.) ammonia ethanol elution after experiment of general alkaloid of Thermopsis extracting solution, preferred 1.0N NH
4oH/90%EtOH solution.
In the preparation method of Tocosamine extract provided by the invention, preferred mineral acid is hydrochloric acid, and alkaline reagents is ammoniacal liquor.
In the preparation method of Tocosamine extract provided by the invention, preferred sample solution pH is 12.
In the present invention, the flow velocity of experiment of general alkaloid of Thermopsis extracting solution loading is 1BV/h, and ammonia ethanol elution flow velocity is 2BV/h.
Instant invention overcomes the deficiency of existing technique, adopt resin cation (R.C.) to carry out abstraction and purification to target, effectively can improve Tocosamine extractive content, reduce low boiling point organic solvent as the consumption of chloroform etc., reduce production cost.
Advantage of the present invention:
1, preparation method of the present invention is easy and simple to handle, extraction yield is high, cost is low, be easy to suitability for industrialized production.
2, to adopt Hydrogen 001 × 7 type Zeo-karb to have Tocosamine exchange capacity high in the present invention, the feature that feed throughput is large.
3, the present invention selects sample solution pH to be about 12 according to the physico-chemical property of Tocosamine, effectively can remove the impurity components such as N-formyl radical Tocosamine, improves the purity of the finished product.
Accompanying drawing explanation
Fig. 1 is the HPLC collection of illustrative plates of Tocosamine and N-formyl radical Tocosamine.
Fig. 2 is the HPLC collection of illustrative plates of Tocosamine extract.
Embodiment
Below by drawings and Examples, the inventive method is described in further detail.
Embodiment 1-3: different sample solution volume is to the comparison of Tocosamine extraction effect
Get dry experiment of general alkaloid of Thermopsis over-ground part material 100 kilograms, with 80% methyl alcohol circumfluence distillation 3 times, united extraction liquid, filter, concentrating under reduced pressure, with about salt acid for adjusting pH to 2, with equivalent extraction into ethyl acetate 2 times, stripped acidic aqueous solution concentrating under reduced pressure removing ethyl acetate, obtains experiment of general alkaloid of Thermopsis extracting solution.The said extracted liquid NaOH aqueous solution regulates pH to 12, wherein Tocosamine content is 23.05mg/mL, obtain experiment of general alkaloid of Thermopsis sample solution, this sample solution is further divided into 1/10 of original volume, 3/10 and 3/5, respectively with 1.0, 1.5 and different Hydrogen 001 × 7 type cation exchange resin column of flow velocity by handling well of 2.0BV/h, after loading, till being washed till lifeless matter alkali reaction with deionized water (Dragendorff reagent), with 1N ammoniacal liquor/90% ethanol elution, to not aobvious alkaloid reaction (Dragendorff reagent) of elutriant, elutriant concentrating under reduced pressure reclaims organic solvent, dry, both Tocosamine extract was obtained.The results are shown in following table.
Embodiment 4: the HPLC of Tocosamine extract purity analyzes
Chromatographic condition:
Chromatographic column: UltisilTM Wel-C8 (5 μm, 4.6mm × 250mm); Moving phase: methyl alcohol-0.05mol/L potassium dihydrogen phosphate aqueous solution (15:85); Volumetric flow rate: 1.0ml/min; Determined wavelength: 314nm, column temperature: 25 DEG C.
The preparation of reference substance solution:
Respectively accurate take 60 DEG C of Tocosamines being dried to constant weight and N-formyl radical Tocosamine appropriate; put in 50mL measuring bottle; be dissolved to scale by moving phase, make every 1mL is respectively 0.36mg and 0.22mg reference substance solution containing Tocosamine and N-formyl radical Tocosamine.
Linear relationship is examined or check
Accurate draw 0.10,0.25,0.5,1.25, the above-mentioned reference substance solution solution of 2.5mL is placed in 10mL measuring bottle respectively, be diluted to scale by moving phase, be mixed, the accurate each 10 μ L of above-mentioned solution that draw inject high performance liquid chromatographs, the relevant chromatographic peak area of record.Take sample size as X-coordinate, peak area is ordinate zou, carries out linear regression, obtains Tocosamine typical curve equation Y=2.941 × 106X+18946, r=0.9995, linearity range 0.036 ~ 3.6 μ g; N-formyl radical Tocosamine typical curve equation Y=2.608 × 106X+10342, linearity range 0.022 ~ 2.2 μ g.After measured, in Tocosamine extracting solution, the content of Tocosamine is 23.0mg/mL, N-formyl radical Tocosamine is 4.5mg/mL.
Tocosamine reference substance and Tocosamine extractive HPLC figure are shown in accompanying drawing 1 and accompanying drawing 2 respectively.
Claims (5)
1. one kind is extracted the method for Tocosamine from experiment of general alkaloid of Thermopsis over-ground part, it is characterized in that the raw materials used experiment of general alkaloid of Thermopsis over-ground part for being in the florescence, after conventional methanol circumfluence distillation, be evaporated to the experiment of general alkaloid of Thermopsis extracting solution containing Tocosamine that proportion is 1.05-1.10; Extracting solution, with after inorganic acid for adjusting pH to 2, filters, is extracted with ethyl acetate removal of impurities, and stripped acidic aqueous solution alkaline reagents regulates pH to 8-12, controls the content of Tocosamine in the aqueous solution not higher than 30mg/mL simultaneously, both obtains sample solution; Sample solution adsorbs Tocosamine by strong acidic ion resin, with the abundant washing resin of deionized water to reacting without obvious alkaloid, use ammonia ethanol elution again, collect containing alkaloidal elutriant, again through concentrate drying, both obtain Tocosamine extract, wherein can reach more than 43% containing Tocosamine.
2. extract the method for Tocosamine from experiment of general alkaloid of Thermopsis over-ground part according to claim 1, it is characterized in that strong acidic ion resin refers to vinylbenzene and divinylbenzene polymer for skeleton, with strong acid group sulfonic group (-SO
3h) be the resin of cation exchange groups.
3. extract the method for Tocosamine according to claim 1 from experiment of general alkaloid of Thermopsis over-ground part, it is characterized in that the resin cation (R.C.) ammonia ethanol elution after adsorbing experiment of general alkaloid of Thermopsis extracting solution, preferred 1.0N NH
4oH/90%EtOH solution.
4. extract the method for Tocosamine according to claim 1 from experiment of general alkaloid of Thermopsis over-ground part, it is characterized in that sample solution pH is 12.
5. extract the method for Tocosamine according to claim 1 from experiment of general alkaloid of Thermopsis over-ground part, it is characterized in that the flow velocity of experiment of general alkaloid of Thermopsis extracting solution loading is 1BV/h, ammonia ethanol elution flow velocity is 2BV/h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510435047.5A CN104961739A (en) | 2015-07-22 | 2015-07-22 | Method for extracting eulexine from aboveground parts of thermopsis lanceolate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891740A (en) * | 2010-07-30 | 2010-11-24 | 王小银 | Method for extracting laburnine from upper part of thermopsis lanceolate |
| CN102349940A (en) * | 2011-08-08 | 2012-02-15 | 南京泽朗医药科技有限公司 | Process for preparing thermopsis lanceolate total alkaloids and several high-purity medicinal substances |
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2015
- 2015-07-22 CN CN201510435047.5A patent/CN104961739A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891740A (en) * | 2010-07-30 | 2010-11-24 | 王小银 | Method for extracting laburnine from upper part of thermopsis lanceolate |
| CN102349940A (en) * | 2011-08-08 | 2012-02-15 | 南京泽朗医药科技有限公司 | Process for preparing thermopsis lanceolate total alkaloids and several high-purity medicinal substances |
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Application publication date: 20151007 |