CN1229369C - Preparation of escoparone contrast product - Google Patents
Preparation of escoparone contrast product Download PDFInfo
- Publication number
- CN1229369C CN1229369C CN 01113986 CN01113986A CN1229369C CN 1229369 C CN1229369 C CN 1229369C CN 01113986 CN01113986 CN 01113986 CN 01113986 A CN01113986 A CN 01113986A CN 1229369 C CN1229369 C CN 1229369C
- Authority
- CN
- China
- Prior art keywords
- chloroform
- escoparone
- residue
- preparation
- scoparone
- Prior art date
- 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.)
- Expired - Fee Related
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Abstract
The present invention relates to a preparation method of escoparone contrast products, which has the characteristics of short technical process and high yield. Escoparone is arranged into a container; then, chloroform is added; the chloroform is recycled by filtering liquid by ultrasound and filtration; water is added to residue; then, the residue is heated and filtered; chlorophyll is removed; a water solution is evaporated to dryness, and after the residue is heated and recrystallized with methanol for three times, white or yellowish needle crystals are obtained. The present invention provides a path for the production of the escoparone of China.
Description
The present invention relates to medical technical field, exactly it is the preparation method of Scoparone reference substance.
The shore wormwood artemisia is than conventional Chinese medicine, removing damp-heat, and cholagogic protects the liver, and is that Chinese traditional treatment is acute, the key medicine of viral icterohepatitis since ancient times.Existing more than 70 of the shared side of oriental wormwood that China's version " pharmacopeia " in 2000, ministerial standard etc. are recorded does not produce but the reference substance of Scoparone is domestic, always from Japan or U.S.'s import.China abounds with the shore wormwood artemisia, and known domestic extraction process about Scoparone is that its technical process is as follows according to the general extraction separation of natural medicinal ingredients and the principle of preparation:
Getting the shore wormwood artemisia adds the water logging bubble of 80 ℃ or 90 ℃ or decocts, merge the aqueous solution, concentrating under reduced pressure, concentrated solution is with chloroform extraction, chloroform extraction liquid is removed water-soluble impurity with 5% aqueous sodium carbonate and the extraction of 2% aqueous sodium hydroxide solution respectively, be neutral to be washed to chloroform extraction liquid again, reclaim chloroform to doing the residue recrystallizing methanol.
Exist following deficiency in the prior art:
1, Scoparone is soluble in chloroform, is dissolved in ether, acetone, hot methanol etc., is insoluble in water.With water is solvent, and extraction efficiency is low, influences the yield of Scoparone.
2, after the aqueous solution concentrates, be extraction solvent with the chloroform, easily produce emulsification during extraction, layering is slower, need take heating to wait measure to solve, and wastes time and energy, and consumes a large amount of organic solvents.
3, with 5%Na
2CO
3In polar component process in the 2%NaOH aqueous solution extraction chloroformic solution, alkaline aqueous solution easily causes the Scoparone open loop, influences yield.Through inquiry, do not find the technology patent of from shore wormwood artemisia extracting shore wormwood artemisia lactones close as yet with the present invention.
The object of the present invention is to provide a kind of preparation method of Scoparone reference substance, fill up the domestic blank that does not have this reference substance to produce, and technology is fairly simple, can carry to such an extent that content is Scoparone more than 98.5% from the wormwood artemisia of shore, as the reference substance of qualitative, quantitative in shore wormwood artemisia medicinal material and the one-tenth side.
The objective of the invention is to be achieved by the following scheme, the shore wormwood artemisia is placed container, add chloroform, ultrasonic, filter, filtrate is reclaimed chloroform, and residue adds water heating, filtered while hot, remove chlorophyll, with aqueous solution evaporate to dryness, residue heats recrystallization three times with methyl alcohol, promptly gets white or faint yellow needle crystal.
Advantage of the present invention is: be the solvent that extracts Scoparone with the chloroform, the emulsification that has produced when having avoided the chloroform extraction aqueous solution does not need the basic solution removal of impurity, has avoided Scoparone open loop in basic solution, the water-soluble chlorophyll that removes.Whole process flow is short, and the yield height is saved solvent.
Embodiment:
Get the colored fringe 50g of shore wormwood artemisia, put in the container, add the 600ml chloroform, ultrasonic 30min filters, and filtrate is reclaimed chloroform, residue adds water 300ml, heat in the water-bath, filtered while hot is removed chlorophyll, with aqueous solution evaporate to dryness, residue is put cold analysis and is gone out white or faint yellow needle crystal 260mg, yield 0.5% with the methyl alcohol heating for dissolving.
Physicochemical constant and structure are identified:
Mp:145～147 ℃ (fusing point instrument assay method); UV λ
Max(MeOH) nm:228.8,293.4,342.8; IR
Max(KBr) cm
-1: 1716.8 (C=O); 1619.8,1560.8,1517.0 (phenyl ring); 1380 (CH
3);
1HNMR:(300MH
Z, CDCl
3) δ: 3.93 (3H, s, OCH
3), 3.96 (3Hs, OCH
3), 6.30 (1H, d, J=9.5H
Z, 3-H), 6.85 (1H, s, 8-H), 6.86 (1H, s, 5-H), 7.63 (1H, d, J=9.5H
Z, 4H); EIMSm/z:206 (M)
+, 191 (M-CH
3)
+, 178 (M-CH
3-CO)
+, 163 (M-2 CH
3-CO)
+, the spectrogram of the EIMS of sample is consistent with the standard spectrogram of Scoparone among the NIST107.
Purity: select the HPLC method for use.Instrument and chromatographic condition: day island proper Tianjin LC-10A liquid chromatograph, configuration CLASS-LC10 workstation, SPD-M10A diode-array detector, CTO-10A post thermostat container.The ODS post, moving phase: acetonitrile-water (30-70), detect wavelength 230nm.The purity that adopts normalization method to measure the Scoparone of carrying reaches 99.0%.
Claims (1)
1, the preparation method of Scoparone reference substance, it is characterized in that: the shore wormwood artemisia is placed container, add chloroform, ultrasonic, filter, filtrate is reclaimed chloroform, and residue adds water heating, filtered while hot, remove chlorophyll, with aqueous solution evaporate to dryness, residue heats recrystallization three times with methyl alcohol, promptly gets white or faint yellow needle crystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113986 CN1229369C (en) | 2001-05-23 | 2001-05-23 | Preparation of escoparone contrast product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113986 CN1229369C (en) | 2001-05-23 | 2001-05-23 | Preparation of escoparone contrast product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1322722A CN1322722A (en) | 2001-11-21 |
| CN1229369C true CN1229369C (en) | 2005-11-30 |
Family
ID=4660679
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01113986 Expired - Fee Related CN1229369C (en) | 2001-05-23 | 2001-05-23 | Preparation of escoparone contrast product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1229369C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101669979B (en) * | 2009-10-09 | 2012-07-11 | 新疆维吾尔自治区药物研究所 | Artemisia scoparia extractive and production method and applications thereof |
| EP2804351A4 (en) | 2012-01-11 | 2015-07-22 | Nec Corp | Computer system, controller, switch, communication method, and recording medium in which network management program has been stored |
| CN102928380A (en) * | 2012-09-11 | 2013-02-13 | 康普药业股份有限公司 | Amlodipine besylate extraction method |
-
2001
- 2001-05-23 CN CN 01113986 patent/CN1229369C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1322722A (en) | 2001-11-21 |
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