CN103342677A - Method of enriching arecoline by using H103 type macroporous adsorption resin - Google Patents
Method of enriching arecoline by using H103 type macroporous adsorption resin Download PDFInfo
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- CN103342677A CN103342677A CN2013102850114A CN201310285011A CN103342677A CN 103342677 A CN103342677 A CN 103342677A CN 2013102850114 A CN2013102850114 A CN 2013102850114A CN 201310285011 A CN201310285011 A CN 201310285011A CN 103342677 A CN103342677 A CN 103342677A
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Abstract
The invention discloses a method for enriching arecoline by using H103 type macroporous adsorption resin. The method comprises the following steps: step one, drying and crushing areca-nut into areca-nut dry powder, soaking in distilled water, and ultrasonically extracting to obtain extracting solution; step two, adding the extracting solution in H103 type macroporous adsorption resin column dynamically adsorb the arecoline; step three, after dynamically adsorbing the arecoline, adding deionized water in H103 type macroporous adsorption resin column, washing, adding ethanol in the H103 type macroporous adsorption resin column to elute the adsorbed arecoline, collecting the eluting solution; step four, reducing pressing and concentrating the eluting solution by using rotary evaporator to obtain the arecoline. The method disclosed by the invention has the beneficial effect that the arecoline is extracted by using environment-friendly water extraction; the eluting solution is ethanol which is convenient to recycle, and the finally obtained arecoline is high in refining degree. The method is easy to operate and can be applied to large-scale production.
Description
Technical field
The present invention relates to the Separation of Natural Products technical field, particularly a kind of method of using H103 type macroporous adsorbent resin enrichment methylarecaidin.
Background technology
Macroporous adsorbent resin claims full porous resin again, polymer absorbant, it be a class to be adsorbed as characteristics, organism is had high molecular polymer concentrated, centrifugation.Macroporous resin is to be prepared from through polyreaction by additives such as polymerization single polymerization monomer and linking agent, pore-creating agent, dispersion agents.Behind the polymer formation, pore-creating agent is removed, and has stayed hole big and small, different, that interpenetrate in resin.Therefore macroporous resin its inside under drying regime has higher porosity, and the aperture is bigger, between 100-1000nm, so be called macroporous adsorbent resin.
Betel nut (Areca catechu L.) is Palmae (Palmae) Areca L. (Areca) plant, the perennial evergreen arbor, and betel nut is extensively cultivated in countries in Southeast Asia such as India, Indonesia.In China, betel nut mainly is distributed in provinces such as Taiwan, Hainan, south of Yunnan, Guangdong, Fujian, and betel nut cultivated area and output are only second to India, and China has become one of main place of production of world's betel nut.Betel nut fruit and pericarp all can be used as medicine, be listed in first of the five Da Nan medicines, main active ingredient wherein be methylarecaidin (Arecoline, AC).
Methylarecaidin chemistry IV-methyl isophthalic acid by name, 2,5,6. guvacoline is the light yellow oily liquid of a kind of no color or smell under the normal temperature, 209 ℃ of boiling points, molecular weight: 155.20, miscible with water, ethanol and ether, be dissolved in chloroform.Methylarecaidin has the effect of the choline of plan, has desinsection, the enhancing of excited unstriated muscle gastrointestinal peristalsis, calm nervus centralis, the antidepressant effect of refreshing oneself.
The extracting method of existing methylarecaidin has water extraction and organic solvent method.Organic solvent method extracts will consume a large amount of organic reagents, toxicity is big, energy consumption is high.And behind the water extraction extraction methylarecaidin, containing a large amount of water-soluble impurities in the extracting solution, extracting liquid volume is big, wants further separation and purification usually.
The separation and purification methylarecaidin generally adopts the method for chloroform extraction in the prior art, and chloroform has hypotoxicity, narcoticness and carcinogenic possibility.The macroporous adsorbent resin technology is widely used in the separation and purification alkaloid in recent years, as be applied in Berberine in radix aconiti agrestis alkaloid, the coptis, Sophora alopecuroides alkali, ephedrine, the lotus leaf A Piao Alkaloid etc., but also do not have about the macroporous adsorbent resin of the concrete kind separation and refining method to methylarecaidin.
In view of foregoing description, demand a kind of environmental protection urgently and effectively remove the method for extracting the refining methylarecaidin of impurity in the methylarecaidin solution occurring.
Summary of the invention
The technical problem to be solved in the present invention is a kind of method of the H103 of use type macroporous adsorbent resin enrichment methylarecaidin.The present invention realizes by the following technical solutions:
A kind of method of using H103 type macroporous adsorbent resin enrichment methylarecaidin of the present invention is characterized in that, may further comprise the steps:
Step 1 will betel nut be ground into betel nut dry powder after the oven dry, add the distilled water immersion 1～2h of 4～7 times of weight in the described betel nut dry powder, supersound extraction 15～30min then, filter extracting solution, adjust extracting liquid pH value with hydrochloric acid soln and be 6.2～6.7, standby;
Step 2, above sample flow velocity are that 1～3BV/h will carry out the dynamic adsorption methylarecaidin in the described extracting solution adding H103 type macroporous adsorptive resins;
Step 3, after described dynamic adsorption methylarecaidin finishes, adding in the described H103 type macroporous adsorptive resins after deionized water wash removes impurity, is the methylarecaidin that 1～3BV/h adds ethanol elution absorption again in the described H103 type macroporous adsorptive resins with elution flow rate, collects elutriant;
Step 4 adopts Rotary Evaporators that described elutriant is carried out concentrating under reduced pressure and obtains methylarecaidin.
Preferably, the described extracting liquid pH value of described step 1 is 6.56.
Preferably, resin content and described extracting liquid volume ratio are 1: 5～1: 7 in the described H103 type of the described step 2 macroporous resin column.
Preferably, described upward sample flow velocity is 2BV/h.
Preferably, the described alcohol concn of described step 3 is 10%～15% and 50%～70%.
Preferably, the described alcohol concn of described step 3 is 70%.
Preferably, the described ethanol pH of described step 3 value is 3.5～3.0.
Preferably, the described ethanol pH of described step 3 value is 3.0.
Preferably, the described extracting solution of described step 3 and described ethanol usage quantity volume ratio are 1: 2～1: 3.
Preferably, the described extracting solution of described step 3 and described deionized water usage quantity volume ratio are 1: 1～1: 2.
The present patent application people is through a large amount of tests, analyzed different sorts polarity and nonpolar macroporous adsorption resin and carried out analysis-by-synthesis under various conditions, these conditions comprise the extracting solution of the betel nut dry powder that uses different pH values and the ethanol eluate under use different concns and the different pH condition.And the content of the methylarecaidin by reverse high effective liquid chromatography for measuring extracting solution and elutriant, by mathematic calculation and calculation of correlation formula, it is best to obtain under the various preferred parameters of the inventive method H103 type macroporous adsorbent resin enrichment methylarecaidin effect.
The correlation parameter of H103 type macroporous adsorbent resin: polarity: nonpolar; Mean pore size AVE:85-95; Pore volume: 1.08-1.12ml/g; Particle size range: 0.315-1.25mm 〉=90% (60-16 order); Water content: 45～50%; Apparent density: 0.53-0.57g/ml; Skeleton is crosslinked polyethylene, skeletal density: 1.20～1.24g/ml; Wet true density: 1.05-1.07g/ml; Wet volume density: 0.70-0.75g/ml; Specific surface area: 1000-1100m
2/ g.
Described reverse high performance liquid chromatography is a chromatographic important branch, be moving phase with liquid, adopt the high pressure transfusion system, the moving phase such as mixed solvent, damping fluid that will have the single solvent of opposed polarity or different ratios pumps into the chromatographic column that stationary phase is housed, in post each composition separated after, enter detector and detect, thereby realization is to the analysis of sample.The chromatographic condition of reverse high performance liquid chromatography of the present invention is Hypersil BDS chromatographic column: C
18, 250 * 4.6mm, 5 μ m; Moving phase: the mass ratio of water-methanol-phosphoric acid-sodium laurylsulfonate is 55: 35.64: 0.17: 1; Flow velocity: 1.0mL/min; Column temperature: 60 ℃; Detect wavelength: 215nm; Sample size: 10 μ l.
The invention has the beneficial effects as follows that the present invention uses water extraction and supersonic method to cooperate and extracts methylarecaidin, the replace organic solvent extracting method had both reduced use cost, had protected environment again; To be 1～3BV/h with described extracting solution add above sample flow velocity carries out the dynamic adsorption methylarecaidin in the H103 type macroporous adsorptive resins and with the methylarecaidin of elution flow rate to be 1～3BV/h add in described H103 type macroporous adsorptive resins ethanol elution absorption in step 2 and the step 3, the described sample flow velocity of going up of these two processes suits, namely save the time, reached adsorption rate and the resolution factor of reasonable methylarecaidin again; After described dynamic adsorption methylarecaidin finishes, add deionized water wash in the described H103 type macroporous adsorptive resins and can remove impurity, make elutriant after carrying out concentrating under reduced pressure, obtain the refining Du Genggao of methylarecaidin; Elutriant is selected ethanol for use, and it is convenient to reclaim, asepsis environment-protecting.In a word, the inventive method is simple to operation, and relatively environmental protection, and the refining degree of the methylarecaidin that finally obtains is higher, can be applicable to scale operation.
Embodiment
Embodiment 1
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 1h that 1kg adds 4kg, supersound extraction 15min then, filter extracting solution 4kg, be 6.2 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 0.6kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 1BV/h joins the gained extracting solution dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 4L deionized water wash, with 50% ethanol 4L wash-out methylarecaidin, the desorb flow velocity is 1BV/h then, collects elutriant.
Embodiment 2
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 1h that 1kg adds 4kg, supersound extraction 22min then, filter extracting solution 4kg, be 6.2 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 0.7kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 2BV/h joins the dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins with embodiment 1 gained extracting solution.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 6L deionized water wash, with 60% ethanol 8L wash-out methylarecaidin, the desorb flow velocity is 2BV/h then, collects elutriant.
Embodiment 3
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 1h that 1kg adds 4kg, supersound extraction 30min then, filter extracting solution 4kg, be 6.2 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 0.8kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 3BV/h joins the dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins with embodiment 1 gained extracting solution.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 8L deionized water wash, with 70% ethanol 12L wash-out methylarecaidin, the desorb flow velocity is 3BV/h then, collects elutriant.
Embodiment 4
Be ground into betel nut dry powder with after the betel nut oven dry, take by weighing 1kg betel nut dry powder, add the distilled water immersion 1h of 5kg, supersound extraction 15min then, filter extracting solution 5kg, be 6.56 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 1BV/h joins the gained extracting solution dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 5L deionized water wash, with 50% ethanol 5L wash-out methylarecaidin, the desorb flow velocity is 1BV/h then, collects elutriant.
Embodiment 5
Be ground into betel nut dry powder with after the betel nut oven dry, take by weighing 1kg betel nut dry powder, add the distilled water immersion 1.5h of 4kg, supersound extraction 22min then, filter extracting solution 5kg, be 6.56 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1.2kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 3BV/h joins the gained extracting solution dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 8L deionized water wash, with 60% ethanol 10L wash-out methylarecaidin, the desorb flow velocity is 3BV/h then, collects elutriant.
Embodiment 6
Be ground into betel nut dry powder with after the betel nut oven dry, take by weighing 1kg betel nut dry powder, add the distilled water immersion 2h of 5kg, supersound extraction 30min then, filter extracting solution 5kg, be 6.7 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1.5kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 2BV/h joins the gained extracting solution dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 10L deionized water wash, with 70% ethanol 15L wash-out methylarecaidin, the desorb flow velocity is 2BV/h then, collects elutriant.
Embodiment 7
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 2h that 1kg adds 7kg, supersound extraction 15min then, filter extracting solution, be 6.7 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 1BV/h joins the dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins with embodiment 3 gained extracting solutions.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 7L deionized water wash, with 50% ethanol 7L wash-out methylarecaidin, the desorb flow velocity is 1BV/h then, collects elutriant.
Embodiment 8
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 2h that 1kg adds 7kg, supersound extraction 22min then, filter extracting solution, be 6.7 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1.3kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 2BV/h joins the dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins with embodiment 3 gained extracting solutions.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 10L deionized water wash, with 60% ethanol 14L wash-out methylarecaidin, the desorb flow velocity is 2BV/h then, collects elutriant.
Embodiment 9
Will betel nut be ground into betel nut dry powder after the oven dry, take by weighing the distilled water immersion 2h that 1kg adds 7kg, supersound extraction 30min then, filter extracting solution, be 6.7 with the hydrochloric acid soln adjustment extracting liquid pH value of 0.1mol/mL, standby.Taking by weighing H103 type macroporous resin 1.5kg (weight in wet base), to put into adsorption column standby, and above sample flow velocity is that 3BV/h joins the dynamic adsorption that carries out methylarecaidin in the H103 type macroporous adsorptive resins with embodiment 3 gained extracting solutions.Extracting solution is all flowed through behind the H103 type macroporous resin adsorption post, and with the 14L deionized water wash, with 70% ethanol 21L wash-out methylarecaidin, the desorb flow velocity is 3BV/h then, collects elutriant.
The various embodiments described above result is as follows:
It is 6.56 that above-described embodiment relatively draws at extracting liquid pH value, and last sample flow velocity is 2BV/h, and alcohol concn is 70%, and ethanol pH value is 3.0, and extracting solution and described ethanol usage quantity volume ratio are 1: 3 o'clock, and eluting rate and refining degree are the highest.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification sheets and the embodiment, it can be applied to various suitable the field of the invention fully, for those skilled in the art, can easily realize other modification, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment that describes.
Claims (10)
1. a method of using the enrichment of H103 type macroporous adsorbent resin to get rid of bulky alkali is characterized in that, may further comprise the steps:
Step 1 will be got rid of to be ground into after the bulky oven dry and get rid of bulky dry powder, to the described distilled water immersion 1～2h that adds 4～7 times of weight in the bulky dry powder that gets rid of, supersound extraction 15～3Omin then, filter extracting solution, adjust extracting liquid pH value with hydrochloric acid soln and be 6.2～6.7, standby;
Step 2, above sample flow velocity are that 1～3BV/h gets rid of bulky alkali with carrying out dynamic adsorption in the described extracting solution adding H103 type macroporous adsorptive resins;
Step 3, after described dynamic adsorption is got rid of bulky alkali end, adding in the described H103 type macroporous adsorptive resins after deionized water wash removes impurity, is the bulky alkali of getting rid of that 1～3BV/h adds ethanol elution absorption again in the described H103 type macroporous adsorptive resins with elution flow rate, collects elutriant;
Step 4 adopts Rotary Evaporators that described elutriant is carried out concentrating under reduced pressure and obtains getting rid of bulky alkali.
2. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described extracting liquid pH value of described step 1 is 6.56.
3. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that resin content and described extracting liquid volume are than being 1:5～1:7 in the described H103 type of the described step 2 macroporous resin column.
4. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that described upward sample flow velocity is 2BV/h.
5. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described alcohol concn of described step 3 is 50%～70%.
6. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described alcohol concn of described step 3 is 70%.
7. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described ethanol pH of described step 3 value is 3.5～3.0.
8. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described ethanol pH of described step 3 value is 3.0.
9. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described extracting solution of described step 3 and described ethanol usage quantity volume ratio are 1:2～1:3.
10. the method for bulky alkali is got rid of in use H103 type macroporous adsorbent resin as claimed in claim 1 enrichment, it is characterized in that the described extracting solution of described step 3 and described deionized water usage quantity volume ratio are 1:1～1:2.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106387737A (en) * | 2016-08-27 | 2017-02-15 | 湖南皇爷食品有限公司 | Areca catechu processing method capable of improving chewiness of areca catechu |
| CN108420918A (en) * | 2018-04-27 | 2018-08-21 | 湖南口味王集团有限责任公司 | A kind of betel nut of the suitable middle-aged and the old |
| CN114702435A (en) * | 2022-04-12 | 2022-07-05 | 长沙绿叶生物科技有限公司 | Preparation method of arecoline |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912496A (en) * | 2010-07-29 | 2010-12-15 | 江苏大学 | Method for preparing betelnut total alkaloids |
| CN101967119A (en) * | 2010-10-26 | 2011-02-09 | 南京泽朗农业发展有限公司 | Method for purifying arecoline |
-
2013
- 2013-07-08 CN CN2013102850114A patent/CN103342677A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101912496A (en) * | 2010-07-29 | 2010-12-15 | 江苏大学 | Method for preparing betelnut total alkaloids |
| CN101967119A (en) * | 2010-10-26 | 2011-02-09 | 南京泽朗农业发展有限公司 | Method for purifying arecoline |
Non-Patent Citations (1)
| Title |
|---|
| 刘文杰: "槟榔中生物碱的提取纯化及其抑菌性能研究", 《北京林业大学学位论文》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106387737A (en) * | 2016-08-27 | 2017-02-15 | 湖南皇爷食品有限公司 | Areca catechu processing method capable of improving chewiness of areca catechu |
| CN108420918A (en) * | 2018-04-27 | 2018-08-21 | 湖南口味王集团有限责任公司 | A kind of betel nut of the suitable middle-aged and the old |
| CN114702435A (en) * | 2022-04-12 | 2022-07-05 | 长沙绿叶生物科技有限公司 | Preparation method of arecoline |
| CN114702435B (en) * | 2022-04-12 | 2024-03-19 | 长沙绿叶生物科技有限公司 | Preparation method of arecoline |
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Application publication date: 20131009 |