CN101168540A - Method for extracting cortex fraxini coumarin - Google Patents
Method for extracting cortex fraxini coumarin Download PDFInfo
- Publication number
- CN101168540A CN101168540A CNA2006101377034A CN200610137703A CN101168540A CN 101168540 A CN101168540 A CN 101168540A CN A2006101377034 A CNA2006101377034 A CN A2006101377034A CN 200610137703 A CN200610137703 A CN 200610137703A CN 101168540 A CN101168540 A CN 101168540A
- Authority
- CN
- China
- Prior art keywords
- cortex fraxini
- bark
- ash
- extracting
- coumarin
- 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
Abstract
The invention discloses a cortex fraxini coumarin extraction method. The method comprises the steps that cortex fraxini is filtered after water extraction and alcohol precipitation, ethyl alcohol is recycled from filter liquor and concentrated, concentrated solution is adsorbed on macroporous resin, and through elution, the collection of eluent, concentration, and drying, the cortex fraxini coumarin is obtained. The cortex fraxini coumarin extraction method related by the invention is the shortcut method with simple operation. The selected macroporous resin has the characteristics that the adsorptive capacity is large and the desorption rate is large. The method of the invention takes the ethyl alcohol as solvent, and the ethyl alcohol is inexpensive and non-toxic. The content of the cortex fraxini coumarin extracted with the method of the invention can reach above 55 percent, the reproducibility is good, and the resin can be repeatedly used.
Description
Technical field
The present invention is the method for traditional Chinese medicine extraction, relates generally to the method that the Chinese medicine active principle extracts, and relates in particular to the extracting method of cortex fraxini coumarin.
Background technology
The bark of ash: this product is dry branch skin or the dry hide of Oleaceae plant fraxinus rhynchophylla Hance Fraxinus rhynchophylla Hance, Chinese ash Fraxinus chinensis Roxb, sharp leaf Chinese ash Fraxinus szaboana Lingelsh. or place post Chinese ash Fraxinus stylosa Lingelsh..Spring, Qiu Erji strip. dry.Point leaf Chinese ash Fraxinus szaboana Lingelsh. or place post Chinese ash FraxinusstylosaLingelsh. skin main product in the weinan, Hua County, Huayin, Changwu; Fraxinus rhynchophylla Hance Fraxinusrhynchophylla Hance skin main product in the Fushun, Benxi, Dandong, the Jilin Huijiang.
Bark of ash bitter, cold in nature, have heat-clearing and damp-drying drug, inducing astrigency, the function that makes eye bright is applicable to hot dysentery, diarrhea, leucorrhea with red and white discharge, conjunctival congestion with pain and swelling of the eye, order is given birth to diseases such as screen film.The contained main component aesculin of the bark of ash, fraxin have multiple biological activity, and antisepsis and anti-inflammation mainly one of acts on for it.Pharmacodynamic experiment prompting bark of ash total coumarins induces rat paw edema that restraining effect is arranged to micro-crystal type uric acid sodium, and certain dose-effect trend is arranged.In vitro tests shows that the bark of ash has significant inhibitory effect to streptococcus aureus, shigella flexneri, sonne bacillus, and Corynebacterium diphtheriae, paratyphosum Bacterium are also had to a certain degree susceptibility, but invalid to intestinal bacteria.In vivo test shows that the bark of ash can reduce the mortality ratio of the chmice acute abdominal cavity infection that is caused by Corynebacterium diphtheriae.Bark of ash LD
50Be 14.60gkg
-1, show that its toxicity is lower.
Be prepared from ophthalmic preparation by the extraction of Chinese medicinal materialss such as the bark of ash, in clinical application for many years, viral and bacillary eye disease had curative effect preferably, especially best to the superficial punctate keratitis effect.The mid-80 begins design and has prepared eye drop and be applied to clinical.
Mainly contain compounds such as coumarins in the bark of ash.In addition, also contain a small amount of phenolic constituent, saponin(e and tannin etc.
Existing method for extracting cortex fraxini coumarin generally adopts water extraction, concentrates, and drying, that is, the tonka bean camphor content that this method is extracted is low, can overcome this shortcoming with the present invention.
Summary of the invention
The purpose of this invention is to provide a kind of cortex fraxini coumarin macroporous resin purification method, is with the water heating and refluxing extraction bark of ash, uses the ethanol alcohol precipitation, filter, filtrate concentrates, with concentrated solution be adsorbed on the macroporous resin, wash-out, collection elutriant, concentrate, dry, obtain cortex fraxini coumarin.Cortex fraxini coumarin macroporous resin purification method provided by the invention with water refluxing extraction 1～4 time, most preferably is the bark of ash: 3 times.Cortex fraxini coumarin macroporous resin purification method provided by the invention, the volume ratio of at every turn extracting bark of ash quality and ethanolic soln is 1～14 times, preferably extracts volume to be: 4～12 times, most preferably extract volume and be: 8 times.Cortex fraxini coumarin macroporous resin purification method provided by the invention, each time of extracting is 0.5～2h, most preferably the time is: 1h.Cortex fraxini coumarin macroporous resin purification method provided by the invention, the concentration of ethanol alcohol precipitation is 20%～90%, and is preferred: 60%～90%, most preferably be: 70%.Cortex fraxini coumarin macroporous resin purification method provided by the invention, macroporous resin is selected the HP20 of MIT, SP825, SP850, SP700, SP70 for use, preferred macroporous resin SP825, SP700, SP70, most preferably SP70.Cortex fraxini coumarin macroporous resin purification method provided by the invention, and the applied sample amount of bark of ash extracting solution (bark of ash quality: the resin volume) be 0.5: 1～8: 1, preferred 1: 1～4: 1, most preferably 1.5: 1.Cortex fraxini coumarin macroporous resin purification method provided by the invention, elution flow rate are that eluent flow rate is 1BV/h～5BV/h, most preferably are 2BV/h.Cortex fraxini coumarin macroporous resin purification method provided by the invention, eluent is organic alcohol, preference is an ethanol.Cortex fraxini coumarin macroporous resin purification method provided by the invention, the wash-out concentration of eluent are that most preferable concentrations is 10%～40%.Cortex fraxini coumarin macroporous resin purification method provided by the invention, the elution volume of macroporous resin eluent are 1～10 times of column volume, and best elution volume is 5 times of column volumes.Cortex fraxini coumarin macroporous resin purification method provided by the invention, the cortex fraxini coumarin content that obtains purifying is greater than 55%.
The present invention has the following advantages:
The method of the cortex fraxini coumarin resin purification that 1, the present invention relates to is a kind of easy and simple to handle, method efficiently.
2, to have adsorptive capacity big for selected macroporous resin, the characteristics that desorption efficiency is big.
3, the inventive method with ethanol is solvent, and is not only inexpensive but also nontoxic.
4, with the inventive method purifying Cortex Fraxini extract, tonka bean camphor content can reach more than 55%, and favorable reproducibility, and resin is reusable.
Description of drawings:
Fig. 1. bark of ash Static Adsorption and desorption efficiency curve
Fig. 2. bark of ash dynamic adsorption leakage plot
Fig. 3. bark of ash dynamic desorption curve
Fig. 4 bark of ash is than upper column quantity curve
Fig. 5. bark of ash wash-out terminal point curve
Embodiment
The present invention will be described further in conjunction with specific embodiments, and these examples only are used for illustration purpose, and are not used in the restriction scope of the invention.
Illustrate:
The cortex fraxini coumarin content assaying method
1. instrument and reagent
Instrument: the general TU-1901 of the universal apparatus company limited type UV, visible light spectrophotometer of analysing in Beijing, association digital processing center.Day island proper Tianjin LIBROR AEL-200 ten thousand/electronic analytical balance, the inferior flourish 2000A type Rotary Evaporators in Shanghai, the SP70 of MIT, SP700, SP825, SP850, HP20 type macroporous resin.
Reagent: aesculin reference substance (, providing lot number 110740-200405 by Nat'l Pharmaceutical ﹠ Biological Products Control Institute) for assay usefulness, used in the preposition Vanadium Pentoxide in FLAKES vacuum drying apparatus dry 24 hours, make it constant weight.Water is double distilled water, and other reagent is analytical pure.
2. detect wavelength: 334nm blank: methyl alcohol.
3. the preparation of reference substance solution
Precision takes by weighing aesculin reference substance 9.1mg, puts in the 25ml measuring bottle, and dissolve with methanol also is diluted to scale, shakes up, and promptly gets reference substance solution.
4. working curve is made:
Accurately absorption 0.1,0.5,1.0,1.5,2.0ml put in the 10ml measuring bottle, add methyl alcohol and are diluted to scale, shake up.Measure absorbancy in 334nm wavelength place.With the absorbancy is ordinate zou, and aesculin reference substance concentration is X-coordinate, the drawing standard curve, and the calculating regression equation is: Y=37.998X-0.0196, R
2=0.9996.
Aesculin is the good linear relation in 3.64 μ g/ml～72.80 μ g/ml scopes.
5. the preparation of need testing solution
It is an amount of to get Cortex Fraxini extract, and accurate the title decides, and puts in the 25ml volumetric flask, adds methyl alcohol and is diluted to scale, shakes up, and precision pipettes in 1.0ml to the 25ml measuring bottle again, adds methyl alcohol and is diluted to scale, shakes up, promptly.
6. assay
Extracting sample solution is put the 334nm place and is measured absorbancy, the record absorbance, and the substitution working curve calculates tonka bean camphor content.
Embodiment 1 a kind of purification process of the present invention
(1) bark of ash extracts: the bark of ash is with 8 times of volume water heating and refluxing extraction three times, and each 1h merges three times filtrate, and being evaporated to proportion is 1.133-1.137 (50-60 ℃), adds 95% ethanol and makes determining alcohol to 80%, standing over night.Precipitation solution is evaporated to not to be had alcohol flavor back thin up and makes liquor capacity reach 2 times of crude drug weight, filters, standby.
(2) upper prop: with bark of ash extracting solution upper prop, it is 0.5BV/h that controlling flow goes out flow velocity, and applied sample amount is a medicinal material weight: the resin volume is 1.5: 1, all enters resin bed to extracting solution.
(3) wash-out: with 10% alcohol flushing resin bed of 5BV volume, it is 2BV/h that controlling flow goes out flow velocity, to remove impurity.With 40% ethanol of 5BV volume, the control flow velocity is 2BV/h then, collects elutriant, is evaporated to certain volume, carries out spraying drying, promptly gets purified product.
Adopt method provided by the invention, select for use different condition to carry out cortex fraxini coumarin and extract experiment.
Table 1 level of factor table
Table 2 bark of ash extracts orthogonal design table
Annotate: with the D factor is error term
Take by weighing bark of ash medicinal material 50g, totally 9 parts, press the level of factor of table 1, the extraction conditions of table 2 carries out orthogonal test respectively, the extraction rear filtrate merges, and is evaporated to driedly, and precision takes by weighing proper amount of dry cream, be dissolved in the 10ml measuring bottle with methyl alcohol, and be diluted to scale, and shake up, pipette again in 1.0ml to the 10ml measuring bottle, add methyl alcohol and be diluted to scale, shake up.Measure the content of total coumarins as stated above.And the result carried out variance analysis, the results are shown in Table 2,3.
Table 3 orthogonal test analysis of variance table
**：F
0.01(2，2)＝99.0 *：F
0.05(2，2)＝19.0
The result: The results of analysis of variance shows that to extract the total coumarins amount be index, and factor A, B, C have significant difference, and influencing size order is C＞A＞B, and yield the best is A
3B
3C
3Combination, from time-saving energy-saving, the angle that reduces cost is considered A
1B
2C
3, be preferred plan.So determine 8 times of water gagings of extraction conditions of the bark of ash, extract each 1 hour 3 times.
Conclusion: add 8 times of water gagings, extract each 1 hour 3 times.
Verify preferred extraction process by water: take by weighing bark of ash medicinal material 50g, add 8 times of decoctings and boil 3 times, each 1 hour (A
1B
2C
3), filtering, filtrate merges, and is evaporated to driedly, and it is an amount of that precision takes by weighing dried cream, is dissolved in the 10ml measuring bottle with methyl alcohol, and is diluted to scale, shakes up, and pipettes in 1.0ml to the 10ml measuring bottle again, and be diluted to scale, shakes up, and repeats 3 times.Other gets bark of ash medicinal material 50g, adds 12 times of decoctings and boils 3 times, each 1.5 hours (A
3B
3C
3), extract rear filtrate and merge, be evaporated to driedly, precision takes by weighing proper amount of dry cream, is dissolved in the 25ml measuring bottle with methyl alcohol, and is diluted to scale, shakes up, and pipettes in 1.0ml to the 10ml measuring bottle again, and is diluted to scale, shakes up, and repeats 3 times.Measure the content of total coumarins as stated above, the results are shown in Table 4.
The preferred bark of ash extraction process by water result of table 4 checking
The result: as can be seen from Table 4, A
3B
3C
3Compare A
1B
2C
3Process recovery ratio is only high about 4.6%, A
1B
2C
3Has good circulation ratio.
Conclusion: preferred extraction process by water has good circulation ratio.
Bark of ash alcohol precipitation orthogonal test:, need with bark of ash the water extracted immersing paste alcohol precipitation in order further to improve the content and the purity of total coumarins.Get 270g bark of ash medicinal material, extract as stated above, extracting solution is merged, be divided into 9 parts, wherein 3 parts of concentrating under reduced pressure are 1.133-1.137 (50-60 ℃) to proportion, wherein 3 parts to be concentrated into proportion be 1.203-1.209 (50-60 ℃), wherein 3 parts to be concentrated into proportion be 1.102-1.108 (50-60 ℃).Level of factor by table 5 is tested, and being concentrated into respectively behind the alcohol precipitation does not have the alcohol flavor, is evaporated to driedly, and it is an amount of that precision takes by weighing dried cream, is dissolved in the 10ml measuring bottle with methyl alcohol, and is diluted to scale, shakes up, and pipettes in 1.0ml to the 10ml measuring bottle again, and be diluted to scale, shakes up.Measure wherein total coumarins content as stated above.The results are shown in Table 6,7.
Table 5 bark of ash alcohol precipitation level of factor table
Table 6 bark of ash alcohol precipitation size of experiment is measured table
Table 7 bark of ash alcohol precipitation experimental variance analytical table
The result: as shown in Table 30, the concentrated solution liquor ratio is heavily remarkable to the influence of alcohol precipitation, and alcohol concn is comparatively remarkable to the influence of alcohol precipitation, and best of breed is A
1B
2, promptly being concentrated into proportion is 1.13-1.17 (50-60 ℃), alcohol precipitation concentration is 70%.
Conclusion: the alcohol precipitation condition is 1.13-1.17 (50-60 a ℃) for being concentrated into proportion, and alcohol precipitation concentration is 70%.
Verify preferred alcohol precipitation process: take by weighing bark of ash medicinal material 100g, add 8 times of decoctings and boil 3 times, each 1 hour, filter, merging filtrate, being evaporated to proportion is 1.135 (55 ℃), adds 70ml 95% ethanol, stir evenly, standing over night filters, be evaporated to driedly, it is an amount of that precision takes by weighing dried cream, is dissolved in the 10ml measuring bottle with methyl alcohol, and be diluted to scale, and shake up, pipette again in 1.0ml to the 10ml measuring bottle, and be diluted to scale, and shake up, repeat 3 times.Measure wherein total coumarins content as stated above.The results are shown in Table 8.
The preferred bark of ash alcohol precipitation process results of table 8 checking
Conclusion: as can be seen from Table 8, preferred alcohol extraction process has good circulation ratio.
Choose resin kind, liquor strength, adsorption rate, applied sample amount, ethanol elution concentration, elution rate, wash-out terminal point 6 factors and carry out single factor experiment respectively, determine the optimum value of each factor.
1. upper prop liquid preparation takes by weighing bark of ash medicinal material 500g, extract by above-mentioned preferred extraction process, 8 times of water gagings boil three times each 1 hour, merging filtrate is evaporated to about 125ml, and proportion is 1.138 (55 ℃), add 95% ethanol, making determining alcohol is 80%, standing over night, filter, decompression recycling ethanol is diluted to 500ml to there not being the alcohol flavor with deionized water, filters, supernatant is standby, and recording total coumarins content is 18.7mgml
-1
2. Static Adsorption is got 5 kinds of each 10g of the macroporous resin of handling well, and (active principle concentration is 6.24mgml to add bark of ash aqueous solution 30ml respectively
-1), every 5min jolting is once got solution 0.4ml after each resin absorption respectively in the 10ml measuring bottle behind the 2h, and methyl alcohol is diluted to scale, shakes up.Measure absorbancy in the 334nm place, calculate the adsorption rate of each resin bark of ash total coumarins.See Table 9, Fig. 1.
3. the resin filter of Static Adsorption is drained in static desorb, adds 30ml 40% alcohol desorption, and every 5min jolting is once got solution 0.1ml after each resin absorption respectively in the 10ml measuring bottle behind the 2h, and methyl alcohol is diluted to scale.Measure total coumarins concentration as stated above, calculate the desorption efficiency of each resin bark of ash total coumarins.See Table 9, Fig. 1.
Table 95 kind of macroporous resin is to the attached rate of the adsorption and desorption of bark of ash total coumarins
The result: as can be seen from Figure 1, the adsorption rate of 5 kinds of resins is big (greater than 90%) all, and the desorption efficiency of HP20 and SP850 is all less.
Conclusion: choose SP70, SP700, the SP825 resin is done dynamic adsorption test.
Table 103 kind of macroporous resin dynamic adsorption result
4. dynamic adsorption is got preferred 3 kinds of each 20ml of resin of the Static Adsorption of handling well (1cm * 13cm), (total coumarins concentration is 6.24mgml to add the bark of ash aqueous solution in post
-1) in capital, carry out dynamic adsorption with the flow velocity of 0.5BV/h, collect effluent liquid, press the resin bed volume and collect, in 334nm place mensuration absorbancy, calculate the content of each total coumarins, the leakage plot of drawing each resin the results are shown in Table 10, Fig. 2.
The result: as can be seen from Figure 2, SP70 and SP825 reach absorption when saturated, and the amount of adsorbed total coumarins is bigger, and SP70 is big than SP825.
Conclusion: choose SP70 and SP825 and do the dynamic desorption test.
5. dynamic resolution is drawn the SP70 handle well and each 20ml of SP825 resin (1cm * 13cm) is 6.24mgml with total coumarins concentration in post
-1Bark of ash aqueous solution 30ml be added on capital, after adsorbing with the flow velocity of 0.5BV/h, carry out wash-out with the flow velocity of 2BV/h with 40% ethanol, press the resin bed volume and collect elutriant, measure absorbancy in the 334nm place, calculate the content of ethanol eluate total coumarins, the results are shown in Table 11, Fig. 3.
Table 11 bark of ash dynamic desorption result
The result: as can be seen from Figure 3, SP70 is good than the desorption effect of SP825, therefore selects SP70 as optimum resin.
Conclusion: select the SP70 resin.
6. liquor strength is investigated and to be got the bark of ash aqueous solution (total coumarins concentration is 18.7mgml
-1) 10ml, be diluted to liquor capacity (ml) respectively: crude drug heavy (g) be 1: 1,1.5: 1,2: 1,4: 1,, 10: 1, add 20ml (on the SP70 resin of 1cm * 13cm), after adsorbing with the flow velocity of 0.5BV/h, with 40% ethanol elution, collect elutriant to 100ml, measure absorbancy in the 334nm place, calculate the content of total coumarins.The results are shown in Table 12.
Table 12 bark of ash liquor strength is investigated the result
The result: from table 35 as can be seen, when soup diluted 4 times, resolution factor was the highest, dilute 1.5 times with 2 times of dilutions quite, and more about 2% than not diluting height, take all factors into consideration production timeliness factor, select 1.5 times of dilutions, ie in solution volume (ml): crude drug heavy (g)=1.5: 1.
Conclusion: go up column liquid concentration and be liquor capacity and reach heavy 1.5 times of crude drug.
7. adsorption rate is investigated and to be got the bark of ash aqueous solution (total coumarins concentration is 18.7mgml
-1) 10ml, be added on 20ml (1cm * 13cm), respectively with 0.5BV/h, 1BV/h, 2BV/h, 3BV/h, 4BV/h, flow velocity adsorb after, carry out wash-out with 5BV 40% with the flow velocity of 2BV/h, measure absorbancy in the 334nm place, calculate the content of ethanol eluate total coumarins.The results are shown in Table 13.
Table 13 bark of ash adsorption rate is investigated the result
Result: can find out from table 13, when adsorption rate is 0.5BVh
-1The time, adsorption effect is best.
Conclusion: adsorption rate is 0.5BVh
-1
8. applied sample amount is investigated and to be got the bark of ash aqueous solution (total coumarins concentration is 18.7mgml
-1) be added on 20ml and (on the SP70 resin of 1cm * 13cm), adsorb with the flow velocity of 0.5BV/h, press the resin bed volume and collect effluent liquid, measure absorbancy in 334nm place, the content of calculating total coumarins.The results are shown in Table 14, Fig. 4.
Table 14 bark of ash applied sample amount is investigated the result
Result: as can be seen from Figure 4, applied sample amount begins when being 4 times of resin bed volumes (BV) to leak, it is saturated to reach absorption during 7 times of times of resin bed volumes (BV), so selects 1.5 times of resin bed volumes (BV) applied sample amount in the actual process, i.e. crude drug heavy (g): resin volume (ml)=1.5: 1.
Conclusion: applied sample amount is crude drug heavy (g): resin volume (ml)=1.5: 1.
9. alcohol concn is investigated and to be got the bark of ash aqueous solution (total coumarins concentration is 18.7mgml
-1) 150ml, add deionized water and be diluted to 225ml (total coumarins concentration is 12.47mgml
-1), be added on 100ml (on the SP70 resin of 2.5cm * 23cm), flow velocity with 0.5BV/h adsorbs, carry out wash-out with 5BV water, 5%, 10%, 20%, 30%, 40%, 60%, 80% ethanol with the 2BV/h flow velocity respectively, collect elutriant to 500ml, measure absorbancy in the 334nm place, calculate the content of total coumarins.The results are shown in Table 15.
Table 15 bark of ash ethanol elution concentration is investigated the result
The result: as can be seen from Table 15, when alcohol concn was 10%-40%, the content of total coumarins the highest (greater than 50%) therefore selected elder generation with 10% ethanol elution, again with 40% ethanol elution, collects 40% ethanol eluate.
Conclusion: select elder generation with 10% and 40% ethanol elution, collect 40% ethanol eluate.
10. elution rate is investigated and to be got the bark of ash aqueous solution (total coumarins concentration is 18.7mgml
-1) 10ml, be added on 20ml (on the SP70 resin of 1cm * 13cm), after adsorbing with the flow velocity of 0.5BV/h, with 40% ethanol elution, flow velocity is respectively 1BV/h, 2BV/h, 3BV/h, 4BV/h, 5BV/h, collection elutriant to 100ml, measure absorbancy in the 334nm place, calculate the content of total coumarins.The results are shown in Table 16.
Table 16 bark of ash takes off speed and investigates the result
The result: as seen from Table 16, desorption efficiency was the highest when flow velocity was the 1BV/h wash-out, but was more or less the same with the 2BV/h wash-out, for raising the efficiency with 2BV/h flow velocity wash-out.
Conclusion: elution rate is 2BV/h.
Result: as can be seen from Figure 5, when elutriant is 5 times of resin bed volumes, substantially total coumarins is cleaned.
Table 17 bark of ash wash-out endpoint determination result
Conclusion: select with 5 times of resin bed volume of ethanol wash-outs.
Verify preferred bark of ash macroporous resin extraction technology: (total coumarins concentration is 18.7mgml to get the bark of ash aqueous solution
-1) 150ml, add deionized water and be diluted to 225ml (total coumarins concentration is 12.47mgml
-1), be added on 100ml (on the SP70 resin of 2.5cm * 23cm), flow velocity with 0.5BV/h adsorbs the back earlier with 500ml 10% ethanol elution, again with 500ml 40% ethanol elution, collects 40% ethanol eluate to 500ml, measure the content of active principle, be evaporated to driedly, dried cream yield is measured in 75 ℃ of vacuum-drying 8 hours, calculate the content of total coumarins, repeat 3 times.The results are shown in Table 41.
Table 18 total coumarins yield and assay result
The result: from table 41 as can be seen, through the bark of ash aqueous solution that the SP70 macroporous resin treatment was handled, total coumarins content can reach about 60%, and yield is about 1.7%, and has good circulation ratio.
Conclusion: selection process has good circulation ratio.
Embodiment 4SP70 macroporous resin stability in use is repeatedly investigated
Take by weighing bark of ash medicinal material 1kg, extract by above-mentioned preferred poach and alcohol precipitation process, extracting solution is settled to 1000ml.Get bark of ash aqueous solution 150ml, thin up is to 225ml, be added on 100ml (on the SP70 resin of 2.5cm * 23cm), flow velocity with 0.5BV/h adsorbs the back earlier with 500ml 10% ethanol 2BV speed wash-out, again with 500ml 40% ethanol 2BV/h speed wash-out, collect 40% ethanol eluate to 500ml, wash post with 500ml 75% ethanol again, 40% ethanol eluate is evaporated to dried, 75 ℃ of vacuum-dryings are to constant weight, measure the content of total coumarins, calculate yield, on same resin column, repeat 5 times by above-mentioned steps.The results are shown in Table 19.
Table 19SP70 macroporous resin uses 5 stability of period to investigate repeatedly
The result: more stable from the above-mentioned as can be seen resin technology of table 42 product yield and total coumarins content in 5 cycles, the SP70 resin can use repeatedly.
Conclusion: use SP70 rosin products yield and total coumarins content more stable in 5 cycles.
The reference that the present invention relates to:
1. Liu Li plum, Chen Lin, Wang Ruihai, etc. the chemical constitution study of the bark of ash. herbal medicine, 2001,32 (12): 1073.
2. Liu Li plum, Chen Lin, Wang Ruihai, etc. the chemical constitution study of the bark of ash. herbal medicine, 2003,34 (10): 889
3. the Lu Yan flower is towards the pharmaceutically active ingredient extraction and separation technology. Beijing: Chemical Industry Press, 2005.228-229.
4. Guo Xi sage, Zhang Yuzhong. the high performance liquid chromatography of effective constituent separates and measures in the bark of ash. Acta Pharmaceutica Sinica, 1983,18 (7): 525.
5. Wang Shu, Xu Xiaoping, Li Tao. the extraction process of aesculin during arthritis with fixed pain caused by dampness is clear. West China pharmaceutical journal, 2002,17 (1): 30-31.
6. the new medical college in Jiangsu. Chinese medicine voluminous dictionary (volume two). Shanghai: Science and Technology of Shanghai press, 1977:2008
7. Pharmacopoeia of People's Republic of China version (an one) in 2005. Beijing: Chemical Industry Press, 2005.218,191.
Claims (12)
1. method for extracting cortex fraxini coumarin, concrete grammar is: the bark of ash through water extraction, through the ethanol alcohol precipitation, is filtered, and filtrate concentrates, concentrated solution is adsorbed onto on the macroporous resin, wash-out, collection elutriant, concentrate, dry, obtain cortex fraxini coumarin.
2. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the bark of ash with water refluxing extraction 1～4 time, most preferably is: 3 times
3. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the volume ratio of at every turn extracting bark of ash quality and water is 1～14 times, preferably extracts volume and is: 6～12 times, most preferably extract volume and be: 8 times.
4. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: each time of extracting is 0.5～2 hour, and most preferably the time is: 1 hour.
5. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the concentration of ethanol alcohol precipitation is 20%～90%, and is preferred: 60%～90%, most preferably be: 70%.
6. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: macroporous resin is selected the HP20 of MIT, SP825, SP850, SP700, SP70 for use, preferred macroporous resin SP825, SP700, SP70, most preferably SP70.
7. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: and the applied sample amount of bark of ash extracting solution macroporous resin (bark of ash quality: the resin volume) be 0.5: 1～8: 1, preferred 1: 1～4: 1, most preferably 1.5: 1.
8. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the macroporous resin eluent is organic alcohol, and preference is an ethanol.
9. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the macroporous resin eluent flow rate is 1 times of column volume/hour (BV/h)～5BV/h, most preferably is 2BV/h.
10. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the wash-out concentration of macroporous resin eluent ethanolic soln is: 5% to 95%, and best wash-out concentration is 10% to 40%.
11. the method for extracting cortex fraxini coumarin as claim 1 is stated is characterized in that: the elution volume of macroporous resin eluent is 1～10 times of column volume.Best elution volume is 5 times of column volumes.
12. method for extracting cortex fraxini coumarin as claimed in claim 1 is characterized in that: the cortex fraxini coumarin content that obtains purifying is greater than 55%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101377034A CN101168540B (en) | 2006-10-27 | 2006-10-27 | Method for extracting cortex fraxini coumarin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006101377034A CN101168540B (en) | 2006-10-27 | 2006-10-27 | Method for extracting cortex fraxini coumarin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101168540A true CN101168540A (en) | 2008-04-30 |
| CN101168540B CN101168540B (en) | 2010-09-29 |
Family
ID=39389330
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006101377034A Active CN101168540B (en) | 2006-10-27 | 2006-10-27 | Method for extracting cortex fraxini coumarin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101168540B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633867B (en) * | 2009-08-05 | 2011-12-28 | 成都大帝汉克生物科技有限公司 | Artificially prepared coumarin |
| CN103664855A (en) * | 2012-09-20 | 2014-03-26 | 浙江大学苏州工业技术研究院 | Preparation method of high-purity oligomer lotus seedpod procyanidin |
| CN104147140A (en) * | 2014-07-31 | 2014-11-19 | 安徽济人药业有限公司 | Preparation method and quality control method of cortex fraxini formula granules |
| CN106596426A (en) * | 2016-12-09 | 2017-04-26 | 广州白云山和记黄埔中药有限公司 | Detection method applied in gynostemma total saponin extraction and separation process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186336C (en) * | 2002-08-29 | 2005-01-26 | 成都迪康药物研究所 | Prepn and application in preparing medicine of fraxinus general coumarin |
-
2006
- 2006-10-27 CN CN2006101377034A patent/CN101168540B/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633867B (en) * | 2009-08-05 | 2011-12-28 | 成都大帝汉克生物科技有限公司 | Artificially prepared coumarin |
| CN103664855A (en) * | 2012-09-20 | 2014-03-26 | 浙江大学苏州工业技术研究院 | Preparation method of high-purity oligomer lotus seedpod procyanidin |
| CN103664855B (en) * | 2012-09-20 | 2015-09-09 | 浙江大学苏州工业技术研究院 | A kind of high purity oligomer LSPC preparation method |
| CN104147140A (en) * | 2014-07-31 | 2014-11-19 | 安徽济人药业有限公司 | Preparation method and quality control method of cortex fraxini formula granules |
| CN106596426A (en) * | 2016-12-09 | 2017-04-26 | 广州白云山和记黄埔中药有限公司 | Detection method applied in gynostemma total saponin extraction and separation process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101168540B (en) | 2010-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101167775B (en) | Method for extracting chrysanthemum total flavone | |
| CN101703599B (en) | Method for detecting cape jasmine fruit extract | |
| CN101085224B (en) | Detection method of 'Mailuoning' injection preparation | |
| CN102631414B (en) | SepHaniadelavayi Diels total alkaloid extraction and purification technology | |
| CN101168540B (en) | Method for extracting cortex fraxini coumarin | |
| CN106420849A (en) | Shuxuening parental injection prepared from ginkgo bioba composition, and preparation method of Shuxuening parenteral injection | |
| CN108864217A (en) | A kind of purification process of granatum punicalagins | |
| CN101812098B (en) | Method for extracting monotropein monomers from medicinal indianmulberry root | |
| CN102659802B (en) | Application in terms of the preparation method of coumarin Neolignans and anti-marime fouling thereof | |
| US20130231469A1 (en) | Method for preparing albiflorin and paeoniflorin | |
| CN101168552B (en) | Method for extracting gentiana macrophylla secoiridoid Glucoside | |
| CN100388940C (en) | Quality control method of Chinese medicinal preparation for treating child hyperpyrexia | |
| CN101195646A (en) | Production method of stilbene glycoside extract | |
| CN104027403B (en) | A kind of preparation method of Radix Polygalae sugar ester effective site | |
| CN112763609B (en) | Research method for screening and extracting process of anti-asthma active ingredients of chamomile | |
| CN109045087A (en) | A kind of enriching and purifying technique of Chinese sumac active component | |
| CN102464586A (en) | Preparation method of danshinolic acid A | |
| CN109010409A (en) | The extraction and purification process and detection method of content of flavonoid compound in a kind of people face fruit leaf | |
| CN110487942B (en) | Fingerprint detection method of antidepressant | |
| CN104111295A (en) | Method for controlling quality of Chinese herbal preparation | |
| CN114617913A (en) | Method for extracting, separating and purifying total saponins of astragalus stems and leaves | |
| CN102093210A (en) | Purified preparation method of six ginkgoic acid monomers | |
| CN101255165A (en) | Extraction method of dahurian angelica root coumarin | |
| CN1935199A (en) | Quality control method for Chinese medicine compound preparation | |
| CN108853274A (en) | A kind of extraction of the total phenols of radix tetrastigme and purification process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| DD01 | Delivery of document by public notice |
Addressee: Guo Song Document name: Notification to Go Through Formalities of Registration |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| DD01 | Delivery of document by public notice | ||
| DD01 | Delivery of document by public notice |
Addressee: Guo Song Document name: Notification to Pay the Fees |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230427 Address after: 1036, Floor 9, No. 6, Chaowai Street, Chaoyang District, Beijing, 100020 Patentee after: Beijing Quanfang Biotechnology Co.,Ltd. Address before: 100083 Beijing city Haidian District Forestry University Road No. 11 Bai Ruyuan District 3E701 Patentee before: Guo Song |