CN102603730A - Method for extracting lycopodine from lycopodium clavatum - Google Patents
Method for extracting lycopodine from lycopodium clavatum Download PDFInfo
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- CN102603730A CN102603730A CN2011100262072A CN201110026207A CN102603730A CN 102603730 A CN102603730 A CN 102603730A CN 2011100262072 A CN2011100262072 A CN 2011100262072A CN 201110026207 A CN201110026207 A CN 201110026207A CN 102603730 A CN102603730 A CN 102603730A
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- chloroform
- extracting
- piliganine
- methanol
- solution
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Abstract
The invention relates to a method for extracting lycopodine from lycopodium clavatum. The method comprises the following steps of: smashing the lycopodium clavatum to 80-100 meshes; adding 90-99% methanol the amount of which is 3-5 times that of the lycopodium clavatum, and carrying out reflux extraction for two-three times; recovering methanol from an extract solution; adding an acetic acid water solution in extract for dissolution; filtering, and then adding calcium oxide for drying; successively carrying out ultrasonic extraction with petroleum ether and chloroform; recovering chloroform from a chloroform extraction solution; adding silica gel for drying, and packing; and eluting a chloroform methanol mixed solution; carrying out a thin film test, collecting high-concentration flow fraction and recovering reagents; and carrying out dissolution and recrystallization for 2-3 times with absolute ethyl alcohol, and drying a crystal substance so as to obtain the pure lycopodine product. According to the invention, the method is adopted to produce the lycopodine, so as to reduce environmental pollution; and the method has the advantages of good stability and high specificity.
Description
Technical field:
The invention belongs to the crude drug field, particularly relate to a kind of method of from Herba Lycopodii, extracting piliganine.
Background technology:
Piliganine be quinoline in western class D vegeto-alkali, molecular formula C
16H
25NO, molecular weight 247.38, column crystallization, 116 ℃ of fusing points.Specific rotation-24.5 (c=1.1, ethanol).Be dissolved in benzene and chloroform etc.
Piliganine is a kind of vegeto-alkali that from lycopsid, extracts, and has step-down, analgesic, antibacterial and excitation.
Herba Lycopodii is dry whole herb with root rhizome and the root of Lycopodiaceae Lycopodium plant lycopod Lycopodium japonicum Thunb..Its expelling wind and cold. dehumidifying detumescence, the effect of stimulating the circulation of the blood and cause the muscles and joints to relax.
The existing method of from Herba Lycopodii, extracting piliganine is less, because mostly vegeto-alkali and composition is complicated in the Herba Lycopodii is the biology total alkali of extraction.
Summary of the invention:
The technical problem that present method will solve provides a kind of method of from Herba Lycopodii, extracting piliganine, and this method industrialization degree is high, can prepare the high-content piliganine.
In order to realize above-mentioned purpose of the present invention, the invention provides following technical scheme:
A kind of method of from Herba Lycopodii, extracting piliganine is characterized in that may further comprise the steps: get Herba Lycopodii and pulverize the 80-100 order, add 3-5 and doubly measure 90-99% methanol eddy extraction 2-3 time, extracting solution reclaims methyl alcohol; Medicinal extract adds aqueous acetic acid dissolving, filters, add the quicklime drying after; Use sherwood oil, chloroform supersound extraction more successively, chloroform extracted solution reclaims chloroform, adds the silica gel oven dry; The dress post, chloroform methanol mixing solutions wash-out, thin layer monitoring; Collect the high density flow point and reclaim reagent, with anhydrous alcohol solution recrystallization 2 times, crystallisate is drying to obtain the pure article of piliganine.
Described aqueous acetic acid concentration is 2-4%, and consumption is 3-5 a times of medicinal extract amount.
The 1-3 that said quicklime consumption is a solution amount doubly.
Described chloroform methanol miscible fluid ratio is 33-27: 9.
The present invention adopts anhydrous methanol to extract, and solvent load is littler than sour water percolation ration, and solvent can recycle and reuse, and is beneficial to environmental protection.
The present invention adopts in the quicklime and absorption, has removed unnecessary acid, has adsorbed other impurity, lacks than extraction solvent amount in the buck, and is simple to operate.
The present invention adopts chloroform methanol mixing wash-out, and does not adopt gradient elution, is because this method is simple to operate, is prone to reappear and amplify and produce, and reagent is prone to reclaim and recycling.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment:
Embodiment 1
Get Herba Lycopodii pulverizing medicinal materials 80-100 order, take by weighing 1kg, add the 5L90% methanol eddy and extract hour, filter extracting solution; Add the 3L90% methanol eddy again and extracted 1 hour, leach extracting solution and add 3L refluxing extraction hour again, united extraction liquid reclaims methyl alcohol to medicinal extract, adds the dissolving of 120ml2% aqueous acetic acid; Filter, add 240g quicklime drying after, add 500ml sherwood oil supersound extraction 1 hour, leach sherwood oil; Add 600ml chloroform supersound extraction 1 hour again, chloroform extracted solution reclaims chloroform, adds oven dry of silica gel 20g (120-200) order and 200g silica gel dress post; Chloroform methanol mixing solutions (33: 9) wash-out, thin layer detects, and collects the high density flow point and reclaims reagent; Use the anhydrous alcohol solution recrystallization again 3 times, the dry pure article 805mg of piliganine, the content 98.5% of getting.
Embodiment 2
Get Herba Lycopodii pulverizing medicinal materials 80-100 order, take by weighing 1kg, add the 5L99% methanol eddy and extract hour, filter extracting solution; Add the 5L99% methanol eddy again and extracted 1 hour, united extraction liquid reclaims methyl alcohol to medicinal extract, adds the dissolving of 100ml4% aqueous acetic acid, filters; After adding 200g quicklime drying, add 400ml sherwood oil supersound extraction 1 hour, leach sherwood oil, add 500ml chloroform supersound extraction 1 hour again; Chloroform extracted solution reclaims chloroform, adds oven dry of silica gel 30g (120-200) order and 150g silica gel dress post; Chloroform methanol mixing solutions (27: 9) wash-out, thin layer detects, and collects the high density flow point and reclaims reagent; Use the anhydrous alcohol solution recrystallization again 2 times, the dry pure article 826mg of piliganine, the content 95.5% of getting.
Embodiment 3:
Get Herba Lycopodii pulverizing medicinal materials 80-100 order, take by weighing 10kg, add the 50L90% methanol eddy and extract hour, filter extracting solution; Add the 30L90% methanol eddy again and extracted 1 hour, united extraction liquid reclaims methyl alcohol to medicinal extract, adds the dissolving of 1L2% aqueous acetic acid, filters; After adding 2.5kg quicklime drying, add 4L sherwood oil supersound extraction 1 hour, leach sherwood oil, add 6L chloroform supersound extraction 1 hour again; Chloroform extracted solution reclaims chloroform, adds oven dry of silica gel 200g (120-200) order and 1000g silica gel dress post; Chloroform methanol mixing solutions (31: 9) wash-out, thin layer detects, and collects the high density flow point and reclaims reagent; Use the anhydrous alcohol solution recrystallization again 3 times, the dry pure article 8.15g of piliganine, the content 97.1% of getting.
Claims (4)
1. a method of from Herba Lycopodii, extracting piliganine is characterized in that may further comprise the steps: get Herba Lycopodii and pulverize the 80-100 order, add 3-5 and doubly measure 90-99% methanol eddy extraction 2-3 time, extracting solution recovery methyl alcohol; Medicinal extract adds aqueous acetic acid dissolving, filters, add the quicklime drying after; Use sherwood oil, chloroform supersound extraction more successively, chloroform extracted solution reclaims chloroform, adds the silica gel oven dry; The dress post, chloroform methanol mixing solutions wash-out, thin layer monitoring; Collect the high density flow point and reclaim reagent, with anhydrous alcohol solution recrystallization 2-3 time, crystallisate is drying to obtain the pure article of piliganine.
2. according to the said method of from Herba Lycopodii, extracting piliganine of claim 1, it is characterized in that the described aqueous acetic acid concentration of step is 2-4%, consumption is 3-5 a times of medicinal extract amount.
3. according to the said method of from Herba Lycopodii, extracting piliganine of claim 1, it is characterized in that 1-3 that the said quicklime consumption of step is a solution amount doubly.
4. according to the said method of from Herba Lycopodii, extracting piliganine of claim 1, it is characterized in that the described chloroform methanol miscible fluid of step ratio is 33-27: 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100262072A CN102603730A (en) | 2011-01-25 | 2011-01-25 | Method for extracting lycopodine from lycopodium clavatum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100262072A CN102603730A (en) | 2011-01-25 | 2011-01-25 | Method for extracting lycopodine from lycopodium clavatum |
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| CN102603730A true CN102603730A (en) | 2012-07-25 |
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| CN2011100262072A Pending CN102603730A (en) | 2011-01-25 | 2011-01-25 | Method for extracting lycopodine from lycopodium clavatum |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644208A (en) * | 2004-11-26 | 2005-07-27 | 谢德隆 | China fir extracts with lycopodine A and B composition and their preparing method |
| WO2007110637A1 (en) * | 2006-03-28 | 2007-10-04 | Bioniqs Limited | Method for extracting target alkaloid using an ionic liquid as extracting solvent |
-
2011
- 2011-01-25 CN CN2011100262072A patent/CN102603730A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644208A (en) * | 2004-11-26 | 2005-07-27 | 谢德隆 | China fir extracts with lycopodine A and B composition and their preparing method |
| WO2007110637A1 (en) * | 2006-03-28 | 2007-10-04 | Bioniqs Limited | Method for extracting target alkaloid using an ionic liquid as extracting solvent |
Non-Patent Citations (4)
| Title |
|---|
| R. H. MANSKE 等: "The alkaloids of Lycopodium Species III. Lycopodium Annotinum L.", 《CANADIAN JOURNAL OF RESEARCH》, vol. 21, no. 5, 31 December 1943 (1943-12-31), pages 92 - 96 * |
| R.H.BURNELL 等: "Lycopodium Alkaloids-VII Lycofoline and Related Bases", 《TETRAHEDRON》, vol. 18, no. 12, 31 December 1962 (1962-12-31), pages 1467 - 1469 * |
| WA AYER 等: "The structure and stereochemistry of lycodoline (lycopodium alkaloid L.8)", 《TETRAHEDRON LETTERS》, vol. 3, no. 3, 31 December 1962 (1962-12-31), pages 87 - 92 * |
| 王龙 等: "石松碱的合成方法综述", 《有机化学》, vol. 28, no. 4, 30 April 2008 (2008-04-30), pages 755 - 760 * |
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Application publication date: 20120725 |