CN1034135A - The preparation method of peganum harmala seed extract - Google Patents
The preparation method of peganum harmala seed extract Download PDFInfo
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- CN1034135A CN1034135A CN 87104598 CN87104598A CN1034135A CN 1034135 A CN1034135 A CN 1034135A CN 87104598 CN87104598 CN 87104598 CN 87104598 A CN87104598 A CN 87104598A CN 1034135 A CN1034135 A CN 1034135A
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- CN
- China
- Prior art keywords
- peganum harmala
- seed
- preparation
- seed extract
- ethanol
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 240000005523 Peganum harmala Species 0.000 title claims abstract description 22
- 235000005126 Peganum harmala Nutrition 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims description 15
- 229930013930 alkaloid Natural products 0.000 claims description 13
- BXNJHAXVSOCGBA-UHFFFAOYSA-N Harmine Chemical compound N1=CC=C2C3=CC=C(OC)C=C3NC2=C1C BXNJHAXVSOCGBA-UHFFFAOYSA-N 0.000 claims description 12
- 241000159213 Zygophyllaceae Species 0.000 claims description 4
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 230000000259 anti-tumor effect Effects 0.000 abstract 1
- 230000000767 anti-ulcer Effects 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 11
- RERZNCLIYCABFS-UHFFFAOYSA-N harmaline Chemical compound C1CN=C(C)C2=C1C1=CC=C(OC)C=C1N2 RERZNCLIYCABFS-UHFFFAOYSA-N 0.000 description 5
- RHVPEFQDYMMNSY-UHFFFAOYSA-N harmalol Chemical compound N1C2=CC(O)=CC=C2C2=C1C(C)=NCC2 RHVPEFQDYMMNSY-UHFFFAOYSA-N 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 3
- YIICVSCAKJMMDJ-UHFFFAOYSA-N L-vasicine Natural products C1=CC=C2N=C3C(O)CCN3CC2=C1 YIICVSCAKJMMDJ-UHFFFAOYSA-N 0.000 description 2
- YIICVSCAKJMMDJ-SNVBAGLBSA-N Peganine Chemical compound C1=CC=C2N=C3[C@H](O)CCN3CC2=C1 YIICVSCAKJMMDJ-SNVBAGLBSA-N 0.000 description 2
- YIICVSCAKJMMDJ-JTQLQIEISA-N Peganine Natural products C1=CC=C2N=C3[C@@H](O)CCN3CC2=C1 YIICVSCAKJMMDJ-JTQLQIEISA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 102000011759 adducin Human genes 0.000 description 1
- 108010076723 adducin Proteins 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- ONBIUAZBGHXJDM-UHFFFAOYSA-J bismuth;potassium;tetraiodide Chemical compound [K+].[I-].[I-].[I-].[I-].[Bi+3] ONBIUAZBGHXJDM-UHFFFAOYSA-J 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- VJHLDRVYTQNASM-UHFFFAOYSA-N harmine Natural products CC1=CN=CC=2NC3=CC(=CC=C3C=21)OC VJHLDRVYTQNASM-UHFFFAOYSA-N 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229960003316 potassium mercuric iodide Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- CGFYHILWFSGVJS-UHFFFAOYSA-N silicic acid;trioxotungsten Chemical compound O[Si](O)(O)O.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1.O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 CGFYHILWFSGVJS-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The invention provides a kind of method for preparing peganum harmala seed extract.The present invention adopts the aquiferous ethanol of 40%-95% (W/W) that seed of peganum harmala is extracted.Production technology of the present invention is simple, nontoxic, safety, and cost is low, and the active ingredient extraction ratio is higher, and water-solubility impurity is low, saves man-hour, and after extraction was finished, ethanol can reclaim fully, and can reuse.Peganum harmala seed extract is to make antitumor, the raw material of medicines such as antiulcer.
Description
The invention provides a kind of method for preparing peganum harmala seed extract.
Herba pegani harmalae (Peganum harmala L.Zygophyllaceae) belongs to the zygophyllaceae herbaceos perennial.Main active ingredient is in the seed of peganum harmala: banisterine (Harmaline), yageine (Harmine), Harmalol (Harmalol) and peganine. (Vasicine) etc. are referred to as total alkaloid of harmaline (Total alkaloid harmala).
The present invention once found banisterine in 1841 by lid Bel abroad in the past, found yageine by Fu Liteqi in 1847, but extraction separation method was not quite clear.Nineteen twenty-seven have again Bai Qin and Robinson adopt between-methoxybenzene diazonium chloride and phosphorus phthalimido-acetyl group-penta vinegar ester through the complicated approach synthetic banisterine and yageine (Su Aoliehefu shows; the alkaloid chemistry; Beijing Science Press; 1960; 504～506); but, have not yet to see report both at home and abroad to the preparation method of peganum harmala seed extract.
The invention provides and a kind ofly need not hang down utmost point organic solvent, produce peganum harmala seed extract, with the output that improves active substance and reduce production costs, make full use of abundant seed of peganum harmala resource, be suitable for the preparation method of suitability for industrialized production with ethanol.
The present invention adopts 40%-95%(W/W) aquiferous ethanol seed of peganum harmala is extracted.
The used ethanol of the present invention is the mixture of alcohol and water.Because concentration of ethanol is excessive, organic molecule impurity such as polysaccharide, protein is corresponding is leached, and causes the difficulty of granulating, and concentration of alcohol is low excessively, and the water-solubility impurity effective component contents that extract low more, and cost consumption is big.Alcoholic acid weight can be to account for 40%-95%, is preferably 60%-90%, is preferably 75%-85%.
Active ingredient in the seed of peganum harmala can extract with several different methods, for example infusion process, percolation, ion exchange, but in order to improve the output of active substance, extraction process is preferably the hot reflux extraction.
Hot reflux is extracted 3-5 time, counts 3-5 hour, because alcoholic acid boiling point is 78.3 ℃, the hot reflux temperature adopts the decompression hot reflux also can at 75 ℃-85 ℃ certainly.
In preparation peganum harmala seed extract process, whenever seed of peganum harmala is not placed in more than 100 ℃.
Seed of peganum harmala is the ripe exsiccant seed of zygophyllaceae herbaceos perennial Herba pegani harmalae.
Peganum harmala seed extract contains two kinds of alkaloids, i.e. banisterine and yageine at least.
Production technology of the present invention is simple, nontoxic, safety, and cost is low, and the active ingredient extraction ratio is higher, and water-solubility impurity is low, saves man-hour, and after extraction was finished, ethanol can reclaim fully, and can reuse.
Discrimination method:
Get extractum 1 gram,, get filtrate and do following test with 5% dilute hydrochloric acid or spirit of vinegar 50ml dissolution filter:
1. get 1 of filtrate or 2ml and place on the spot plate or in vitro, add reagent such as potassium mercuric iodide, bismuth potassium iodide, silico-tungstic acid and generate reddish brown precipitation.
2. filtrate presents intensive blue green fluorescence under sunlight or uviol lamp.
3. thin layer chromatography, condition: silica gel G plate, 105 ℃ of activation 1 hour, developing solvent: CHCL
3: EtOH(6.3: 3.7) under uviol lamp, should present 2 above fluorescence speckles.
Embodiment 1
The ripe dry seed of 10kg Herba pegani harmalae (picking up from the Urumchi Western Hills) is broken slightly, it is inserted in the extractor, add 40% ethanol 20kg-30kg, reflux, extract 5 times, each 1 hour, temperature got extracting solution at 75 ℃-85 ℃, reclaim ethanol, get thick body of paste, promptly extractum 1.37kg presses the mensuration mensuration total alkaloid content 15.0% of known heavy.When hot reflux extraction 3 times, and other condition is identical, gets extractum 1.23kg, total alkaloid content 13.6%
Embodiment 2
The ripe dry seed of 10kg Herba pegani harmalae (picking up from the Urumchi Western Hills) is broken slightly, it is inserted in the extractor, add 60% ethanol 20kg-30kg, reflux, extract 5 times, each 1 hour, temperature got extracting solution at 75 ℃-85 ℃, reclaim ethanol, get thick body of paste, promptly extractum 1.26kg presses the mensuration mensuration total alkaloid content 17.2% of known heavy.When hot reflux extraction 3 times, and other condition is identical, gets extractum 1.14kg, total alkaloid content 14.8%
Embodiment 3
The ripe dry seed of 10kg Herba pegani harmalae (picking up from the Urumchi Western Hills) is broken slightly, it is inserted in the extractor, add 80% ethanol 20kg-30kg, reflux, extract 5 times, each 1 hour, temperature got extracting solution at 75 ℃-85 ℃, reclaim ethanol, get thick body of paste, promptly extractum 1.21kg presses the mensuration mensuration total alkaloid content 20.0% of known heavy.When hot reflux extraction 3 times, and other condition is identical, gets extractum 1.08kg, total alkaloid content 16.4%
Embodiment 4
The ripe dry seed of 10kg Herba pegani harmalae (picking up from the Urumchi Western Hills) is broken slightly, it is inserted in the extractor, add 95% ethanol 20kg-30kg, reflux, extract 5 times, each 1 hour, temperature got extracting solution at 75 ℃-85 ℃, reclaim ethanol, get thick body of paste, promptly extractum 1.15kg presses the mensuration mensuration total alkaloid content 25.5% of known heavy.When hot reflux extraction 3 times, and other condition is identical, gets extractum 0.85kg, total alkaloid content 23.1%
Claims (6)
1, a kind of preparation method of peganum harmala seed extract is characterized in that the method adopts the aquiferous ethanol of 40%--95% (W/W) that seed of peganum harmala is extracted.
2, preparation method according to claim 1 is characterized in that extraction process is preferably the hot reflux extraction.
3, preparation method according to claim 2 is characterized in that hot reflux extraction 3-5 time, counts 3-5 hour, and the hot reflux temperature is at 75 ℃-85 ℃.
4, preparation method according to claim 1 is characterized in that whenever seed of peganum harmala is not placed in more than 100 ℃.
5, preparation method according to claim 1 is characterized in that seed of peganum harmala is the ripe exsiccant seed of zygophyllaceae herbaceos perennial Herba pegani harmalae.
6, preparation method according to claim 1 is characterized in that peganum harmala seed extract contains two kinds of alkaloids, i.e. banisterine and yageine at least.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87104598 CN1034135A (en) | 1987-10-27 | 1987-10-27 | The preparation method of peganum harmala seed extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87104598 CN1034135A (en) | 1987-10-27 | 1987-10-27 | The preparation method of peganum harmala seed extract |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1034135A true CN1034135A (en) | 1989-07-26 |
Family
ID=4814941
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87104598 Pending CN1034135A (en) | 1987-10-27 | 1987-10-27 | The preparation method of peganum harmala seed extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1034135A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999024048A1 (en) * | 1997-11-06 | 1999-05-20 | Pharmaceutical Research Center | Cancer treatment drug |
| CN104628731A (en) * | 2015-01-27 | 2015-05-20 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
-
1987
- 1987-10-27 CN CN 87104598 patent/CN1034135A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999024048A1 (en) * | 1997-11-06 | 1999-05-20 | Pharmaceutical Research Center | Cancer treatment drug |
| CN104628731A (en) * | 2015-01-27 | 2015-05-20 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
| CN104628731B (en) * | 2015-01-27 | 2017-02-22 | 中国农业科学院兰州畜牧与兽药研究所 | Method for extracting peganum harmala alkaloid under microwave assistance |
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| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| RJ01 | Rejection of invention patent application after publication |