CN101037461A - Preparation method of breviscapine raw material medicine by using big-hole resin - Google Patents
Preparation method of breviscapine raw material medicine by using big-hole resin Download PDFInfo
- Publication number
- CN101037461A CN101037461A CN 200710065713 CN200710065713A CN101037461A CN 101037461 A CN101037461 A CN 101037461A CN 200710065713 CN200710065713 CN 200710065713 CN 200710065713 A CN200710065713 A CN 200710065713A CN 101037461 A CN101037461 A CN 101037461A
- Authority
- CN
- China
- Prior art keywords
- macroporous resin
- breviscarpine
- water
- solution
- preparation
- 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.)
- Granted
Links
Images
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for refining the breviscapinun original material medicine with a large-hole resin, especially an original material medicine of scutellar content of 90-95%. The inventive method is composed of following steps: firstly adopting a large-hole resin of a type D101 or AB-8, with a weight ratio of large-hole resin dosage and original material medicine 10-15:1, having the water as solvent to fill column; secondly, the preparation of the breviscapinun filling solution: choosing the breviscapinun as material with a scutellar content of 75-85%, preparing into a solution with a weight percent concentration of 10-20% with boiling water; adjusting the pH to 7.0-7.5 with lye, filtering, getting the column filling solution; thirdly, adding the column filling solution of the step 2 to the large-hole resin of the step 1, eluting the eluant by water, collecting the eluant until the eluant is substantial transparent; fourthly, adjusting the collected eluant pH value in the third step to 1-2, precipitating yellow deposit, stewing more than 5 hours, filtering, washing the deposit to the neutral, testing no Cl-; fifthly, drying the deposit.
Description
Technical field
The content that the present invention relates to a kind of method, especially scutellarin with the refining Breviscarpine bulk drug of macroporous resin is the preparation method of the bulk drug of 90-95%.
Background technology
The Herba Erigerontis prime system is isolated flavones ingredient from Herba Erigerontis Erigeron breviscapus (Vant) Hand-Mazz herb, " drug standard " promulgated by the ministries or commissions of the Central Government record be defined as that lamp-dish flower acetic content is more than 90% in the Breviscapini injection.Because the method for at present refining Breviscarpine bulk drug is the process for purification of imitated yellow Siberian cocklebur glucoside, quality product does not reach the regulation of cloth standard promulgated by the ministries or commissions of the Central Government.Breviscarpine bulk drug process for purification is failed fine solution always, therefore is necessary to study new process for purification, makes it to meet the regulation of " drug standard " promulgated by the ministries or commissions of the Central Government.
Chinese patent application number 00113019.6 discloses a kind of " active component of fleabane flower and preparation technology and preparation ", it is characterized in that dilute methanol or Diluted Alcohol or rare acetone extraction that Herba Erigerontis raw material (herb) meal is directly passed through, the extracting solution concentrate under reduced pressure at low temperature, place precipitation, remove impurity such as chlorophyll, polystyrene resin column chromatography on the concentrated solution, elder generation's water wash-out is collected water lotion and rare alcohol thereof or allydione wash-out partly, and water liquid transfers to pH1-2 with concentrated hydrochloric acid, this acidic aqueous solution is gone up the polystyrene resin post again, use rare pure wash-out at last, this elutriant decompression, concentrate the spraying drying, get yellow powder, be this efficient part.The raw material that this method adopted is the Herba Erigerontis herb, and its efficient part is flavonoid compound, coffic acid and caffeoyl quinic acid compounds and an acid of burnt alkynes health and a derivative thereof.Its sensing is not the Breviscarpine bulk drug---content is the Breviscarpine bulk drug of scutellarin more than 90%.
6 of the applicant in first to file " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200410062573.3), " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200410040182.1), " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200410040352.6), " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200410079583.8), " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200410079642.1), " preparation technology of high-purity medicine with lamp-dish flower acetic as raw material " (application number 200510010723.1) is to adopt commercially available Breviscarpine bulk drug, through behind certain processing step, make scutellarin content and be the highly purified bulk drug more than 99%.
The Breviscarpine bulk drug should be for more than 90% according to the content of stipulating its scutellarin of " drug standard " promulgated by the ministries or commissions of the Central Government record, but the content of scutellarin does not reach afore mentioned rules at present a large amount of Breviscarpine bulk drugs, the content of its scutellarin only is 75-85%, and how adopting comparatively easy method to make the content of scutellarin reach required standard is problem demanding prompt solution.
Summary of the invention
Purpose of the present invention is intended to overcome the defective of prior art, and a kind of content with scutellarin in the macroporous resin purified method raising Breviscarpine bulk drug is provided, and makes it reach required standard.
Preparation method with the refining Breviscarpine bulk drug of macroporous resin of the present invention is made up of following steps:
One, adopting model is the macroporous resin of D101 or AB-8, and the weight ratio of macroporous resin consumption and bulk drug consumption is 10-15: 1, and be solvent-loaded column with water;
Two, the preparation of Breviscarpine upper prop solution: getting scutellarin content is the Breviscarpine raw material of 75-85%, and being mixed with weight percent concentration with boiling water is 10-20%, again with lye pH adjustment to 7.0-7.5, dissolving filters, and obtains upper prop solution;
Three, the upper prop solution with step 2 adds on the macroporous resin column of step 1, and water is collected elutriant as the eluent wash-out, and is colourless substantially until elutriant;
Four, the elutriant of step 3 collection is 1-2 with acid solution accent pH, separates out yellow mercury oxide, leaves standstill more than 5 hours, filters, and throw out washes with water to neutrality, checks no Cl
-
Five, throw out oven dry, promptly.
The described macroporous resin type of step 1 is to handle qualified resin according to the working method of routine, and the working method of described routine is: with ethanol or acetone repetitive scrubbing, meet water until washings muddiness does not take place.The described alkali lye of step 2 is the alkaline solution of accent pH commonly used, as: 10% NaHCO
3Solution, sodium hydroxide solution of 5% etc.; Described solution can carry out centrifugation earlier before filtering, to improve filtration efficiency.The described acid solution of step 4 is the acid solution of accent pH commonly used, as: 20% hydrochloric acid soln, 15% sulphuric acid soln etc.
As the above-mentioned treating process of process, the content of scutellarin does not reach 90%, and repetitive operation is 1-2 time again, the second cellulose content can be brought up to more than 90%.
The macroporous resin that is adopted among the present invention is a kind of sorbent material commonly used, and the thick step that generally is used for plant constituent separates, and seldom is used for refining chemical ingredients.But it is the macroporous resin of D101 or AB-8 that unique distinction of the present invention just has been to adopt model, make refining Breviscarpine bulk drug, improve wherein that this technical barrier of content of scutellarin has obtained solution.
Processing step of the present invention is simple, is easy to suitability for industrialized production, has solved the refining difficult problem of Breviscarpine bulk drug for many years.Because macroporous resin absorption has been removed many impurity, make the Breviscarpine bulk drug of preparing reach the regulation of " drug standard " promulgated by the ministries or commissions of the Central Government record.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of refining preceding Breviscarpine raw material among the embodiment 1.
Fig. 2 is the high-efficient liquid phase chromatogram of refining back Breviscarpine raw material among the embodiment 1.
Fig. 3 is the high-efficient liquid phase chromatogram of refining preceding Breviscarpine raw material among the embodiment 2.
Fig. 4 is the high-efficient liquid phase chromatogram of refining back Breviscarpine raw material among the embodiment 2.
Among the figure: use the instrument type: liquid chromatography gradient mode: constant current detector: ultraviolet
Instrument model: LC-10A wavelength (nm): 335 column temperatures (℃): 32
Post model: Phenomenx model Prodigy (250*4.6mm) 5u ODS3 100R
Integrative approach: area normalization method
Embodiment
In embodiment of the present invention, the macroporous resin of employing must be handled to the use that is up to the standards.
Embodiment 1:
Take by weighing scutellarin content and be 84.69% Breviscarpine raw material 500g, it is 20% that adding boiling water is mixed with weight percent concentration, with 20% sodium bicarbonate adjust pH to 7.5, make dissolving, filtrate earlier through 16000rpm manage continuously the examination whizzer centrifugal after, filter again, filtrate joins on the D101 macroporous resin column, water is an elutriant, till the collection elutriant is extremely colourless substantially.Elutriant is with 20% hydrochloric acid adjust pH to 1, staticly settled 10 hours, filter, precipitation washes with water to neutral (checking no Cl-with AgNO3), 105 ℃ of oven dry, censorship is through the high performance liquid chromatography analysis, the Breviscarpine bulk drug is 84.69% to bring up to 91.65% from original second cellulose content, meets " drug standard " promulgated by the ministries or commissions of the Central Government Breviscapini injections (1998) regulation.
Analysis chart is seen Fig. 1 Fig. 2.
Detection method: (with octadecyl silane is weighting agent: methyl alcohol-0.1% phosphoric acid solution (40: 60) is a moving phase for chromatographic condition and system suitability test; The detection wavelength is 335nm.Number of theoretical plate calculates by the scutellarin peak should not be lower than 5000).Get this product, add water 1ml dissolving, add methyl alcohol and make the solution that every 1ml contains scutellarin 0.4mg approximately, as need testing solution according to every 10mg scutellarin; Precision is measured need testing solution 1.0ml, puts in the 100ml measuring bottle, adds methyl alcohol to scale, mixing, solution in contrast.Get contrast solution 5ul and inject liquid chromatograph, regulate detection sensitivity, the peak height that makes the principal constituent chromatographic peak is 10% of a full range.Get need testing solution 5ul again and inject liquid chromatograph, the record color atlas is to 2.5 of principal constituent peak retention time.Measure each impurity peak area on the need testing solution color atlas and with the peak area ratio of contrast solution principal constituent, calculate lamp-dish flower acetic purity.
Analytical results table (before refining)
| Peak number | Retention time | Peak height | Peak area | Content |
| 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 | 3.138 3.804 4.052 4.430 6.816 7.367 8.052 8.592 10.396 11.449 12.005 13.053 18.857 21.595 22.568 27.431 35.671 | 9.19755e-1 7.97254 3.47414 3.32300 14.53389 1.27681 1.19722 12.76064 6.40299 141.49791 25.28779 1536.81128 2.29861 58.21960 2.11445 1.34691 14.76332 | 14.56590 128.41640 37.76905 49.33636 201.09874 21.03535 16.85241 204.11977 121.10210 2707.08740 493.17511 3.82260e4 75.80067 2062.33887 61.46141 53.13762 659.36902 | 0.0323 0.2845 0.0837 0.1093 0.4456 0.0466 0.0373 0.4523 0.2683 5.9981 1.0927 84.6970 0.1680 4.5695 0.1362 0.1177 1.4610 |
| Amount to | 1834.20086 | 4.51327e4 | 100.000 |
Analytical results table (refining back)
| Peak number | Retention time | Peak height | Peak area | Content |
| 1 2 3 4 5 6 7 8 9 10 | 3.753 3.991 4.347 5.586 6.680 8.385 10.113 11.159 12.818 20.799 | 2.33789 1.16772 1.22659 5.250402e-1 2.39410 4.45277 1.22218 21.85762 546.31567 14.11109 | 36.11115 12.77846 23.86122 10.96413 35.11035 70.88377 23.06172 427.01724 1.20605e4 458.36243 | 0.2744 0.0971 0.1813 0.0833 0.2668 0.5387 0.1753 3.2452 91.6545 3.4834 |
| Amount to | 595.63604 | 1.31586e4 | 100.000 |
Embodiment 2:
Take by weighing scutellarin content and be 78.99% Breviscarpine raw material 500g, it is 10% that adding boiling water is mixed with weight percent concentration, sodium hydroxide solution adjust pH to 7.5 with 5%, make dissolving, filtrate earlier through 16000rpm manage continuously the examination whizzer centrifugal after, filter again, filtrate joins on the AB-8 macroporous resin column, water is an elutriant, till the collection elutriant is extremely colourless substantially.Elutriant staticly settled 10 hours with 15% sulphuric acid soln adjust pH to 1, filtered, and precipitation washes with water to neutral (checking no Cl-with AgNO3).All repetitive operation is 1 time.80 ℃ of oven dry, censorship, through the high performance liquid chromatography analysis, the Breviscarpine bulk drug is 78.99% to bring up to 91.99% from original second cellulose content, meets " drug standard " promulgated by the ministries or commissions of the Central Government Breviscapini injections (1998) regulation.
Analysis chart is seen Fig. 3 Fig. 4.
Detection method is with embodiment 1.
Analytical results table (before refining)
| Peak number | Retention time | Peak height | Peak area | Content |
| 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 | 10.298 15.798 18.098 19.398 22.998 26.398 28.398 33.998 38.598 39.998 43.198 50.398 56.798 74.398 86.398 90.398 | 71.311 586.425 557.545 1568.917 68610.406 386.152 150.648 3115.636 72.876 70.124 83.117 1880.102 92.088 1023.051 15.025 14.017 | 2298.407 46092.688 41602.719 104840.320 3182385.500 24352.822 17411.982 208551.484 6384.179 5868.765 9576.227 170042.828 17637.947 177617.406 7221.320 6574.357 | 0.0571 1.1442 1.0327 2.6025 78.9976 0.6045 0.4322 5.1770 0.1585 0.1457 0.2377 4.221 0.4378 4.4091 0.1793 0.1632 |
| Amount to | 78297.440 | 4028458.951 | 100.0000 |
Analytical results table (refining back)
| Peak number | Retention time | Peak height | Peak area | Content |
| 1 2 3 4 5 6 7 8 | 3.998 6.898 8.498 11.282 11.765 12.848 20.615 34.098 | 53.485 287.200 832.950 3531.918 2331.835 153268.203 4185.910 628.000 | 443.500 4307.500 14916.800 72116.242 49927.184 3665525.750 147976.406 29397.199 | 0.0111 0.1081 0.3744 1.8099 1.2530 91.9921 3.7137 0.7378 |
| Amount to | 165119.501 | 3984610.581 | 100.0000 |
Claims (3)
1, a kind of preparation method with the refining Breviscarpine bulk drug of macroporous resin is characterized in that being made up of following steps:
One, adopting model is the macroporous resin of D101 or AB-8, and the weight ratio of macroporous resin consumption and bulk drug consumption is 10-15: 1, and be solvent-loaded column with water;
Two, the preparation of Breviscarpine upper prop solution: getting scutellarin content is the Breviscarpine raw material of 75-85%, and being mixed with weight percent concentration with boiling water is 10-20%, again with lye pH adjustment to 7.0-7.5, dissolving filters, and obtains upper prop solution;
Three, the upper prop solution with step 2 adds on the macroporous resin column of step 1, and water is collected elutriant as the eluent wash-out, and is colourless substantially until elutriant;
Four, the elutriant of step 3 collection is 1-2 with acid solution accent pH, separates out yellow mercury oxide, leaves standstill more than 5 hours, filters, and throw out washes with water to neutrality, checks no Cl
-
Five, throw out oven dry, promptly.
2, preparation method as claimed in claim with the refining Breviscarpine bulk drug of macroporous resin, it is characterized in that the described macroporous resin type of step 1 is the qualified resin of working method processing according to routine, the working method of described routine is with ethanol or acetone repetitive scrubbing, meets water until washings muddiness does not take place.
3, the preparation method with the refining Breviscarpine bulk drug of macroporous resin as claimed in claim is characterized in that the described solution of step 2 carried out centrifugation earlier before filtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100657136A CN100457768C (en) | 2007-03-14 | 2007-03-14 | Preparation method of breviscapine raw material medicine by using big-hole resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100657136A CN100457768C (en) | 2007-03-14 | 2007-03-14 | Preparation method of breviscapine raw material medicine by using big-hole resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101037461A true CN101037461A (en) | 2007-09-19 |
| CN100457768C CN100457768C (en) | 2009-02-04 |
Family
ID=38888660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100657136A Active CN100457768C (en) | 2007-03-14 | 2007-03-14 | Preparation method of breviscapine raw material medicine by using big-hole resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100457768C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188440A (en) * | 2010-03-16 | 2011-09-21 | 万生联合制药有限公司 | Preparation method of high-purity breviscapinun material used by breviscapinun injection |
| CN102552359A (en) * | 2008-06-27 | 2012-07-11 | 四川大学 | Preparation method of Erigeron multiradiatus extractive |
| CN102659875A (en) * | 2012-04-27 | 2012-09-12 | 段志雄 | Extracting method of breviscapine |
| CN104914206A (en) * | 2015-06-24 | 2015-09-16 | 昆药集团股份有限公司 | Method for detecting raw material and preparation of scutellarin |
| CN105646620A (en) * | 2015-12-29 | 2016-06-08 | 云南生物谷药业股份有限公司 | Preparation method of apigenin-7-O-glucronide |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053609A (en) * | 1990-01-25 | 1991-08-07 | 云南省生物制药厂 | The extraction process of Herba Erigerontis tablet bulk drug |
| CN1634255A (en) * | 2004-10-15 | 2005-07-06 | 贵阳云岩西创药物科技开发有限公司 | Compound formulation of breviscapine for treating cardiovascular and cerebrovascular diseases and its preparing process |
-
2007
- 2007-03-14 CN CNB2007100657136A patent/CN100457768C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102552359A (en) * | 2008-06-27 | 2012-07-11 | 四川大学 | Preparation method of Erigeron multiradiatus extractive |
| CN102188440A (en) * | 2010-03-16 | 2011-09-21 | 万生联合制药有限公司 | Preparation method of high-purity breviscapinun material used by breviscapinun injection |
| CN102188440B (en) * | 2010-03-16 | 2012-09-26 | 吉林四长制药有限公司 | Preparation method of high-purity breviscapinun material used by breviscapinun injection |
| CN102659875A (en) * | 2012-04-27 | 2012-09-12 | 段志雄 | Extracting method of breviscapine |
| CN102659875B (en) * | 2012-04-27 | 2014-12-10 | 段志雄 | Extracting method of breviscapine |
| CN104914206A (en) * | 2015-06-24 | 2015-09-16 | 昆药集团股份有限公司 | Method for detecting raw material and preparation of scutellarin |
| CN105646620A (en) * | 2015-12-29 | 2016-06-08 | 云南生物谷药业股份有限公司 | Preparation method of apigenin-7-O-glucronide |
| CN105646620B (en) * | 2015-12-29 | 2018-06-26 | 云南生物谷药业股份有限公司 | The preparation method of fleabane flower A prime |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100457768C (en) | 2009-02-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101723996B (en) | Method for separating high-purity anthocyanin monomers from black rice | |
| CN108802255B (en) | Method for determining content of ganoderma lucidum triterpene component in compound preparation | |
| CN103145677B (en) | Method for separating active ingredients from aquilaria sinensis lamina by utilizing high-speed countercurrent chromatography | |
| CN100457768C (en) | Preparation method of breviscapine raw material medicine by using big-hole resin | |
| CN102352402B (en) | Method for preparing red ginseng saponins Rg3 group and Rh2 group mixed saponins | |
| CN1990496B (en) | Process for preparing high purity rhodiola root glycosides | |
| CN101376668B (en) | Preparation technique of high-purity scutellarin raw medicine | |
| CN103340983B (en) | Lycium ruthenicum fruit extract as well as preparation method and application thereof | |
| CN101357147B (en) | Extract of dogbane leaf with finger print and preparation and analytical method thereof | |
| CN101270103B (en) | Method for extracting salvianolic acid B | |
| CN101045741A (en) | Method for separating preparing anthocyan monomer from mulberry | |
| CN1850193A (en) | Method for preparing capsule of Exocarpium citri Tangerinae seu Grandis and loquat, and its quality control technology | |
| CN101935359A (en) | Liriope muscari baily polysaccharide and preparation method thereof | |
| CN103376300B (en) | The detection method of tannin class material in Danshen injection Polyphenol Acids | |
| CN103006721A (en) | Method for extracting phenylethanoid glycoside and flavonoid C-glycoside from corallodiscus flabellata | |
| CN111595972A (en) | Preparation method and quality detection method of lithocarpus polystachyus rehd total flavone extract | |
| CN105434539A (en) | Composition of lotus flavones | |
| CN113440547B (en) | Method for separating and purifying Japanese thistle herb total glycosides by adopting macroporous resin series dynamic axial compression column | |
| CN112763609B (en) | Research method for screening and extracting process of anti-asthma active ingredients of chamomile | |
| CN112851621B (en) | Total iridoid extract of caulis et folium fici Tikouae, extraction and purification method and application thereof | |
| CN111812221B (en) | Method for separating saponin component from Chinese medicinal materials of Panax | |
| CN1840537A (en) | Process for preparing high purity scutellarin raw materials | |
| CN1775234A (en) | Method for preparing compound Folium pyrrosial particles and its quality control technology | |
| CN113655166A (en) | High performance liquid detection method for 14 components in golden flower refreshing granules | |
| CN1778807A (en) | Production of Rhizoma Picrorhizae glucoside II monomer and its drug form for treating hepatitis B |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: KUNMING LONGJIN PHARMACEUTICAL CO., LTD. Free format text: FORMER OWNER: FAN XIANE Effective date: 20100512 |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 650228 KUNMING LONGJIN PHARMACEUTICAL CO., LTD., WUJIADUI, XINWEN ROAD (LOWER SECTION), KUNMING CITY, YUNNAN PROVINCE TO: 650106 NO.2188, KEGAO ROAD, HIGH-TECH. ZONE, KUNMING CITY, YUNNAN PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20100512 Address after: 650106 No. 2188 Gao Lu, hi tech Zone, Yunnan, Kunming Patentee after: Kunming Longjin Pharmaceutical Co., Ltd. Address before: 650228, Yunnan City, Kunming province road under the five pile of Kunming Long Jin Pharmaceutical Co., Ltd. Patentee before: Fan Xiane |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 650500 No. 789, Lanmao Road, majinpu sub district office, Kunming high tech Zone, Kunming, Yunnan Patentee after: KUNMING LONGJIN PHARMACEUTICAL Co.,Ltd. Address before: 650106 No. 2188 Kegao Road, high tech Zone, Kunming, Yunnan Patentee before: KUNMING LONGJIN PHARMACEUTICAL Co.,Ltd. |