CN102060885B - Preparation method for forsythoside A - Google Patents
Preparation method for forsythoside A Download PDFInfo
- Publication number
- CN102060885B CN102060885B CN200910228550.8A CN200910228550A CN102060885B CN 102060885 B CN102060885 B CN 102060885B CN 200910228550 A CN200910228550 A CN 200910228550A CN 102060885 B CN102060885 B CN 102060885B
- Authority
- CN
- China
- Prior art keywords
- drip washing
- forsythiaside
- preparation
- resin
- alcohol
- 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
Links
- DTOUWTJYUCZJQD-UJERWXFOSA-N Forsythiaside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](OC(=O)\C=C\C=2C=C(O)C(O)=CC=2)[C@H](O)[C@@H](O)[C@H](OCCC=2C=C(O)C(O)=CC=2)O1 DTOUWTJYUCZJQD-UJERWXFOSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- DTOUWTJYUCZJQD-QJDQKFITSA-N Forsythiaside Natural products C[C@@H]1O[C@H](OC[C@H]2O[C@@H](OCCc3ccc(O)c(O)c3)[C@H](O)[C@@H](O)[C@@H]2OC(=O)C=Cc4ccc(O)c(O)c4)[C@H](O)[C@H](O)[C@H]1O DTOUWTJYUCZJQD-QJDQKFITSA-N 0.000 title abstract 5
- 239000011347 resin Substances 0.000 claims abstract description 53
- 229920005989 resin Polymers 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000003814 drug Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 138
- 238000005406 washing Methods 0.000 claims description 64
- 238000011068 loading method Methods 0.000 claims description 23
- 150000001408 amides Chemical class 0.000 claims description 15
- 238000002955 isolation Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000499 gel Substances 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000004744 fabric Substances 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims 1
- 229940079593 drug Drugs 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 14
- 238000000926 separation method Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000012467 final product Substances 0.000 abstract description 4
- 239000004952 Polyamide Substances 0.000 abstract 1
- 229920005654 Sephadex Polymers 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229920002647 polyamide Polymers 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 description 12
- 229960001866 silicon dioxide Drugs 0.000 description 10
- 241000576429 Forsythia suspensa Species 0.000 description 9
- 239000002775 capsule Substances 0.000 description 9
- 230000007613 environmental effect Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000003809 water extraction Methods 0.000 description 3
- 241000233866 Fungi Species 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000555712 Forsythia Species 0.000 description 1
- 102000004861 Phosphoric Diester Hydrolases Human genes 0.000 description 1
- 108090001050 Phosphoric Diester Hydrolases Proteins 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- RMZZTJOADJVCIO-UHFFFAOYSA-N acetic acid;acetonitrile;hydrate Chemical compound O.CC#N.CC(O)=O RMZZTJOADJVCIO-UHFFFAOYSA-N 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 238000005220 pharmaceutical analysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Landscapes
- Saccharide Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method for forsythoside A. The preparation method for the forsythoside A comprises the following steps of: (1) immersing raw material medicament in acid, and extracting; (2) separating by using resin; (3) separating by using polyamide; (4) separating by using resin; (5) purifying by using reverse phase silica gel; and (6) purifying by using dextrangel. According to the method, an alcohol-water system is used for extraction and separation, and resin materials used in the process are recycled, so the production cost is reduced. By the extraction method of the preparation method for the forsythoside A, the content of the final product forsythoside A is up to 90 to 95 percent; therefore, the process is simple and efficient, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of Traditional Chinese medicine extraction method, specifically, is a kind of preparation method of forsythiaside A, belongs to field of medicaments.
Background technology
Forsythia Oleaceae capsule of weeping forsythia machaka, its fruit can be used as medicine, and has the effect of clearing heat and detoxicating, mass dissipating and swelling eliminating, antibacterium and fungi.Forsythiaside A is the main component in the capsule of weeping forsythia, not only inhibited to various pathogens such as streptococcus aureuses, but also can suppress phosphodiesterase, fungi and active oxygen, therefore at natural antiseptic agent and natural antioxidants field, there is application prospect very widely.
The extraction and separation method of forsythiaside A all has report in various documents and materials at present.After the direct water extraction of method that prior art adopts or water extraction, use again organic solvent extraction, and then by silicagel column separation or column chromatography for separation, obtain final product.As beam decorative embellishments of writing etc. (pharmaceutical analysis magazine, 1986,6 (5), 263-266) from the capsule of weeping forsythia, extracting forsythiaside A product is applied chemistry separation method, then with preparation of lamina plate, carries out purifying, obtains sterling.The defect of aforesaid method is too much that production efficiency is low, organic solvent is used, and material used can not be reused, and is unfavorable for suitability for industrialized production.Sansel (Chem.Pharm.Bull, 1982,32 (12), the method for 4548-4553) using is first water extraction, then goes up silica gel column chromatography separated.Its defect is complex process, needs to rinse with a large amount of organic solvents in sepn process.Chinese patent 200610027024.1,200610027036.4,200610027037.9 is all also in a large number with an organic solvent, and material price used is expensive, and production cost is high.
The extraction of forsythiaside A and isolation technique, present forward is simple, the modern future development of environmental protection, but document also rests on the organic reagent extraction stage separated with silicagel column with the technique majority in patent now, such technique had not both met the requirement of environmental protection, and, in production operation process, also extremely inconvenient.
Therefore, need to find the simple environmental protection of a kind of technique, forsythiaside A extracting method with low cost, to meet the market requirement of continuous expansion.
Summary of the invention
The object of this invention is to provide that a kind of technique is simple, solvent safety is nontoxic, the forsythiaside A extracting method of with low cost, environmental protection.
For achieving the above object, the present invention adopts following technical proposal:
A preparation method for forsythiaside A, is characterized in that comprising several steps below:
1, acid extraction: get dry capsule of weeping forsythia medicinal material, 10～20 times of amounts of the sour water that is 1～3 by pH value are soaked 5～10 times, each 24h, with 200～300 order filter-cloth filterings, filtrate merges.
2, resin isolation: sour water drip washing resin 1～4BV (column volume) that above-mentioned filtrate is first 1～2 by pH value, upper AB-8 resin carries out separation, after loading, use again water wash 1～2BV, it is faint yellow to leacheate, clarifying, then uses 30～50% ethanol drip washing 3～10BV, collects alcohol leacheate, 60 ℃ of drying under reduced pressure are to without alcohol, and adjust pH is 1～3.
3, polymeric amide is separated: by 100～300 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 1～4BV that is first 1～2 by pH value, then use 0.06% NaHCO
3solution rinses 3～8BV, collect alkali lye, and adjust pH is 1～3.
4, resin isolation: the sour water drip washing resin 1～4BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 2～8BV, then uses 95% ethanol drip washing 2～6BV, collects alcohol leacheate, 60 ℃ are evaporated to dry.
5, reverse phase silica gel purifying: get 5～10 times of amount 30～50% dissolve with ethanol loadings for dry thing separated in above-mentioned (4), with 10% ethanol drip washing 2～10BV, then use the drip washing of 30-50% ethanol, collect 30-50% ethanol leacheate, 60 ℃ are evaporated to dry.
6, dextrane gel purifying: get 5～10 times of amount 30～50% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 30～50% ethanol drip washing 3～10BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Extraction process of the present invention has following beneficial effect: this technique is to use alcohol water system to extract and separated technique completely, through processing parameter, improves, and has formed rational, modern and operational path environmental protection.
In addition, the resin material used of this operational path all can reuse, and has reduced production cost.Polymeric amide and AB-8 are very cheap resins, although and reverse phase silica gel and dextrane gel price are slightly high, while using, be that the purity of forsythiaside A is in nearly 80% left and right, so, the impurity seeing in seldom, through simple 95% alcohol flushing, just can reuse.Use extracting method of the present invention, the content of final product forsythiaside A can reach 90%～95%.Therefore, technique is simple, efficient, is applicable to suitability for industrialized production.
Embodiment
By the following example, will contribute to understand the present invention, but not limit content of the present invention.
Embodiment 1
(1) acid extraction: get dry capsule of weeping forsythia medicinal material 1000g, 10 times of amounts of the sour water that is 1 by pH value are soaked 5 times, each 24h, with 200 order filter-cloth filterings, filtrate merges.
(2) resin isolation: the sour water drip washing resin 1BV that above-mentioned filtrate is first 1 by pH value, upper AB-8 resin carries out separation, after loading, use water wash 1BV, it is faint yellow to leacheate, clarifying, then uses 30% ethanol drip washing 3BV again, collect alcohol leacheate, 60 ℃ of drying under reduced pressure are extremely without alcohol, and adjust pH is 1.
(3) polymeric amide is separated: by 100-200 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 1BV that is first 1 by pH value, then use 0.06% NaHCO
3solution rinses 3BV, collect alkali lye, and adjust pH is 1.
(4) resin isolation: the sour water drip washing resin 1BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 2BV, then uses 95% ethanol drip washing 2BV, collects alcohol leacheate, 60 ℃ of concentrating under reduced pressure as for.
(5) reverse phase silica gel purifying: get dry thing separated in above-mentioned (4) and purify with reverse phase silica gel: get dry thing, by 5 times of amount 30% dissolve with ethanol loadings, with 10% ethanol drip washing 2BV, then use 30% ethanol drip washing, collect 30% ethanol leacheate, 60 ℃ are evaporated to dry.
(6) dextrane gel purifying: get 5 times of amount 30% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 30% ethanol drip washing 3BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Embodiment 2
(1) acid extraction: get dry capsule of weeping forsythia medicinal material 5000g, 20 times of amounts of the sour water that is 3 by pH value are soaked 10 times, each 24h, with 300 order filter-cloth filterings, filtrate merges.
(2) resin isolation: the sour water drip washing resin 4BV that above-mentioned filtrate is first 2 by pH value, upper AB-8 resin carries out separation, after loading, use water wash 2BV, it is faint yellow to leacheate, clarifying, then uses 50% ethanol drip washing 10BV again, collect alcohol leacheate, 60 ℃ of drying under reduced pressure are extremely without alcohol, and adjust pH is 3.
(3) polymeric amide is separated: by 200-300 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 4BV that is first 2 by pH value, then use 0.06% NaHCO
3solution rinses 8BV, collect alkali lye, and adjust pH is 3.
(4) resin isolation: the sour water drip washing resin 4BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 8BV, then uses 95% ethanol drip washing 6BV, collects alcohol leacheate, 60 ℃ of concentrating under reduced pressure as for.
(5) reverse phase silica gel purifying: get dry thing separated in above-mentioned (4), by 10 times of amount 50% dissolve with ethanol loadings, with 10% ethanol drip washing 10BV, then use 50% ethanol drip washing, collect 50% ethanol leacheate, 60 ℃ are evaporated to dry.
(6) dextrane gel purifying: get 10 times of amount 50% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 50% ethanol drip washing 10BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Embodiment 3
(1) acid extraction: get dry capsule of weeping forsythia medicinal material 800g, 15 times of amounts of the sour water that is 1.5 by pH value are soaked 8 times, each 24h, with 200 order filter-cloth filterings, filtrate merges.
(2) resin isolation: the sour water drip washing resin 3BV that above-mentioned filtrate is first 1.5 by pH value, upper AB-8 resin carries out separation, after loading, use water wash 1BV, it is faint yellow to leacheate, clarifying, then uses 40% ethanol drip washing 4BV again, collect alcohol leacheate, 60 ℃ of drying under reduced pressure are extremely without alcohol, and adjust pH is 2.
(3) polymeric amide is separated: by 100-200 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 3BV that is first 1.5 by pH value, then use 0.06% NaHCO
3solution rinses 6BV, collect alkali lye, and adjust pH is 2.
(4) resin isolation: the sour water drip washing resin 3BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 5BV, then uses 95% ethanol drip washing 4BV, collects alcohol leacheate, 60 ℃ are evaporated to dry.
(5) reverse phase silica gel purifying: get dry thing separated in above-mentioned (4), by 8 times of amount 40% dissolve with ethanol loadings, with 10% ethanol drip washing 6BV, then use 40% ethanol drip washing, collect 40% ethanol leacheate, 60 ℃ are evaporated to dry.
(6) dextrane gel purifying: get 8 times of amount 40% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 40% ethanol drip washing 4BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Embodiment 4
(1) acid extraction: get dry capsule of weeping forsythia medicinal material 30g, 13 times of amounts of the sour water that is 2 by pH value are soaked 6 times, each 24h, with 200 order filter-cloth filterings, filtrate merges.
(2) resin isolation: the sour water drip washing resin 2BV that above-mentioned filtrate is first 1.3 by pH value, upper AB-8 resin carries out separation, after loading, use again water wash 1BV, it is faint yellow to leacheate, clarifying, then uses 35% ethanol drip washing 8BV, collects alcohol leacheate, 60 ℃ of drying under reduced pressure are extremely without alcohol, and adjust pH is 2.5.
(3) polymeric amide is separated: by 200-300 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 2BV that is first 1.3 by pH value, then use 0.06% NaHCO
3solution rinses 5BV, collect alkali lye, and adjust pH is 1.5.
(4) resin isolation: the sour water drip washing resin 2BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 4BV, then uses 95% ethanol drip washing 3BV, collects alcohol leacheate, 60 ℃ are evaporated to dry.
(5) reverse phase silica gel purifying: get dry thing separated in above-mentioned (4), by 6 times of amount 25% dissolve with ethanol loadings, with 10% ethanol drip washing 5BV, then use 35% ethanol drip washing, collect 35% ethanol leacheate, 60 ℃ are evaporated to dry.
(6) dextrane gel purifying: get 7 times of amount 25% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 25% ethanol drip washing 8BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Embodiment 5
(1) acid extraction: get dry capsule of weeping forsythia medicinal material 200g, 18 times of amounts of the sour water that is 2.5 by pH value are soaked 9 times, each 24h, with 300 order filter-cloth filterings, filtrate merges.
(2) resin isolation: the sour water drip washing resin 4BV that above-mentioned filtrate is first 1.8 by pH value, upper AB-8 resin carries out separation, after loading, use again water wash 2BV, it is faint yellow to leacheate, clarifying, then uses 45% ethanol drip washing 7BV, collects alcohol leacheate, 60 ℃ of drying under reduced pressure are extremely without alcohol, and adjust pH is 1.5.
(3) polymeric amide is separated: by 100-300 object polymeric amide on the parting liquid in above-mentioned (2), and the sour water drip washing resin 4BV that is first 1.8 by pH value, then use 0.06% NaHCO
3solution rinses 7BV, collect alkali lye, and adjust pH is 2.5.
(4) resin isolation: the sour water drip washing resin 4BV that is first 1～2 by pH value by the parting liquid in above-mentioned (3), upper AB-8 resin, applied sample amount is 7BV, then uses 95% ethanol drip washing 5BV, collects alcohol leacheate, 60 ℃ are evaporated to dry.
(5) reverse phase silica gel purifying: get dry thing separated in above-mentioned (4), by 9 times of amount 45% dissolve with ethanol loadings, with 10% ethanol drip washing 8BV, then use 45% ethanol drip washing, collect 45% ethanol leacheate, 60 ℃ are evaporated to dry.
(6) dextrane gel purifying: get 9 times of amount 45% dissolve with ethanol loadings for dry thing of purifying in above-mentioned (5), with 45% ethanol drip washing 5BV, collect flaxen colour band, 60 ℃ are evaporated to dry.
Test example
The present invention carries out qualitative detection by thin layer detection system to extract.
First measure the weight (in Table 1) of extract in every group of embodiment, and then according to following detection method, the forsythiaside A content of 5 embodiment samples of the present invention is carried out to detection by quantitative, detected result is in Table 2.
Content assaying method: measure according to high performance liquid chromatography (< < Pharmacopoeia of People's Republic of China > > appendix VI D in 2005).
1, chromatographic condition chromatographic column: Dikma C
18(250mm * 4.6mm, 5 μ m); Moving phase: acetonitrile-water-acetic acid (15: 85: 0.2); Flow velocity: 1.0mLmin
-1; Detect wavelength: 332nm; Column temperature: room temperature; Forsythiaside A theoretical plate number is not less than 3000 with this understanding.
2, it is appropriate that forsythiaside A reference substance is got in the preparation of reference substance solution, accurately weighed, adds 50% ethanol to make every 1ml containing the solution of 0.4mg, obtains.
The preparation precision of need testing solution takes sample powder 10mg, puts in 25ml volumetric flask.Add 50% ethanolic soln 20ml, jolting is all dissolved it, then adds 50% ethanolic soln to scale, shakes up, and with 0.45 μ m filtering with microporous membrane, obtains.
Table 1
| Sample | Example weight (g) | Extract weight (g) |
| Embodiment 1 | 1000 | 6.98 |
| Embodiment 2 | 5000 | 35.31 |
| Embodiment 3 | 800 | 5.58 |
| Embodiment 4 | 30 | 0.22 |
| Embodiment 5 | 200 | 1.41 |
Table 2
| Sample | Extract weight (mg) | Forsythiaside A weight (mg) |
| Embodiment 1 | 9.98 | 9.18 |
| Embodiment 2 | 10.01 | 9.26 |
| Embodiment 3 | 9.97 | 9.46 |
| Embodiment 4 | 10.03 | 9.35 |
| Embodiment 5 | 9.99 | 9.21 |
Discuss: adopt extracting method of the present invention, the stable content of final extract, extraction yield is about 7 ‰, and the content of final product forsythiaside A reaches more than 90%, illustrates that technique is simple and efficient, is applicable to suitability for industrialized production.
Claims (10)
1. a preparation method for forsythiaside A, is characterized in that, comprises the following steps:
(1) acid soak of bulk drug is extracted, and described sour pH value is 1～3;
(2) resin isolation: first use sour drip washing, after loading, then use water wash, it is faint yellow clarifying to leacheate, then uses alcohol drip washing, collects alcohol leacheate, drying under reduced pressure, adjust pH is 1～3;
(3) polymeric amide is separated: by 100～300 object polymeric amide on the parting liquid in (2), and sour drip washing, then use alkaline flushing, and collect alkali lye, adjust pH is 1～3;
(4) resin isolation: first use sour drip washing resin, then by solution loading in step 3, then use alcohol drip washing, and collect alcohol leacheate, be evaporated to dry;
(5) reverse phase silica gel purifying: get the dry thing of step (4) gained, dissolve loading, alcohol drip washing, collects alcohol leacheate, is evaporated to dry;
(6) dextrane gel purifying: get dry thing in step (5) and dissolve loading, alcohol drip washing, collects flaxen colour band, is evaporated to dry.
2. method for preparing forsythiaside A according to claim 1, is characterized in that, the acid soak described in step (1) is extracted as: with the acid of 10～20 times of medicinal material volumes, soak 5～10 times, each 24h, with 200～300 order filter-cloth filterings.
3. the preparation method of forsythiaside A according to claim 1, is characterized in that, step 3 alkaline flushing is: the NaHCO with 0.06%
3solution rinses 3～8BV.
4. the preparation method of forsythiaside A according to claim 1, is characterized in that, described resin is AB-8 resin.
5. the preparation method of forsythiaside A according to claim 1, is characterized in that, described sour drip washing is: the sour drip washing resin 1～4BV that is 1～2 by pH value.
6. the preparation method of forsythiaside A according to claim 1, is characterized in that, the alcohol drip washing described in step 4 is with 95% ethanol drip washing 2～6BV.
7. the preparation method of forsythiaside A according to claim 1, is characterized in that, the alcohol drip washing of described step 5 is with 10% ethanol drip washing 2～10BV, then uses the drip washing of 30-50% ethanol.
8. the preparation method of forsythiaside A according to claim 1, is characterized in that, the dissolving loading solution used described in step 5 and 6 is 5～10 times of amount 30～50% ethanol.
9. the preparation method of forsythiaside A according to claim 1, is characterized in that, the alcohol drip washing described in step 6 is with 30～50% ethanol drip washing 3～10BV.
10. the preparation method of forsythiaside A according to claim 1, is characterized in that, described decompression temperature is 60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910228550.8A CN102060885B (en) | 2009-11-13 | 2009-11-13 | Preparation method for forsythoside A |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910228550.8A CN102060885B (en) | 2009-11-13 | 2009-11-13 | Preparation method for forsythoside A |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102060885A CN102060885A (en) | 2011-05-18 |
| CN102060885B true CN102060885B (en) | 2014-09-17 |
Family
ID=43996405
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910228550.8A Expired - Fee Related CN102060885B (en) | 2009-11-13 | 2009-11-13 | Preparation method for forsythoside A |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102060885B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193836B (en) * | 2013-04-19 | 2015-09-09 | 山东农业大学 | The separation purification method of monomeric compound in a kind of Flos Forsythiae |
| CN104130858B (en) * | 2014-07-02 | 2016-05-18 | 河南科技大学 | Forsythiaside A is in the application and the preparation method that prepare in oil quality retention agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398868A (en) * | 2001-07-24 | 2003-02-26 | 山西大学 | Forsythigenol extracting process |
| CN101215302A (en) * | 2008-01-08 | 2008-07-09 | 山西大学 | Method for preparing forsythiaside A |
-
2009
- 2009-11-13 CN CN200910228550.8A patent/CN102060885B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1398868A (en) * | 2001-07-24 | 2003-02-26 | 山西大学 | Forsythigenol extracting process |
| CN101215302A (en) * | 2008-01-08 | 2008-07-09 | 山西大学 | Method for preparing forsythiaside A |
Non-Patent Citations (10)
| Title |
|---|
| Sansei Nishibe, et al..The structure of Forsythiaside isolated from Forsythia suspensa.《chem. pharm. bull.》.1982,第30卷(第3期),第1048-1050页. |
| The structure of Forsythiaside isolated from Forsythia suspensa;Sansei Nishibe, et al.;《chem. pharm. bull.》;19821231;第30卷(第3期);第1048-1050页 * |
| 任延久等.连翘的提取工艺及有效成份的研究.《黑龙江医药》.1995,第8卷(第6期),第308-310页. |
| 张立伟等.连翘酯甙分离提取及抑制弹性蛋白酶活性研究.《化学研究与应用》.2002,第14卷(第2期),第219-221页. |
| 正交法优选连翘酯苷最佳提取工艺;王进东等;《山西中医》;20080831;第24卷(第8期);第48-49页 * |
| 王进东等.正交法优选连翘酯苷最佳提取工艺.《山西中医》.2008,第24卷(第8期),第48-49页. |
| 王霖娇等.青翘和黄翘中连翘酯甙含量的比较及其提取工艺研究.《种子》.2006,第25卷(第10期),第29-31页. |
| 连翘的提取工艺及有效成份的研究;任延久等;《黑龙江医药》;19951231;第8卷(第6期);第308-310页 * |
| 连翘酯甙分离提取及抑制弹性蛋白酶活性研究;张立伟等;《化学研究与应用》;20020430;第14卷(第2期);第219-221页 * |
| 青翘和黄翘中连翘酯甙含量的比较及其提取工艺研究;王霖娇等;《种子》;20061031;第25卷(第10期);第29-31页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102060885A (en) | 2011-05-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107337586A (en) | A kind of method of extraction purification cannabidiol in fiber crops from the Chinese | |
| CN101215302B (en) | Method for preparing forsythiaside A | |
| CN103773820A (en) | Method for extracting, separating and purifying isoflavone active components biochanin A and genistein from dalbergia odorifera T.Chen leaves | |
| CN103012415A (en) | Method for preparing copper chlorophyll and sodium salt thereof from silkworm excrement | |
| CN100482655C (en) | Epigallocatechin gallate monomer purification method | |
| CN103961381A (en) | Method for negative-pressure boiling extraction and preparation of low-acid ginkgo extract | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN102060885B (en) | Preparation method for forsythoside A | |
| CN1935798B (en) | Method for preparing and rographalide | |
| CN101973983A (en) | Method for extracting orientins from Chinese globeflower flowers | |
| CN102060884B (en) | Preparation method of forsythoside A | |
| CN103172601B (en) | Method for separating and extracting salvianolic acid B | |
| CN102617674B (en) | Preparation method of scopolin monomer in anisodus tanguticus root | |
| CN111595972A (en) | Preparation method and quality detection method of lithocarpus polystachyus rehd total flavone extract | |
| CN105884722B (en) | A kind of method that andrographolide and Dehydro and drographolide are isolated and purified from Herba Andrographitis | |
| CN102040500A (en) | Method for extracting and separating xanthohumol and flavone compounds | |
| CN103183658A (en) | Method for extracting effective component of coleus forskohlii | |
| CN103012346B (en) | Preparation method of pectolinarigenin monomer | |
| CN102267877A (en) | Method for extracting and separating magnolol and honokiol from leaf of magnolia officinalis | |
| CN104844550A (en) | Method for separating and purifying cnidium lactone and imperatorin from fructus cnidii | |
| CN103235067A (en) | Method for enriching gallotannin with antioxidation activity from mangos | |
| CN103044253A (en) | Extraction separation method of rosmarinic acid in salvia castabea diels f. tomentosa stib | |
| CN102373248A (en) | Method for purifying biochanin A | |
| CN102302523B (en) | Preparation method of low-phenolic-acid ginkgo biloba extract | |
| CN101297878A (en) | Preparation technique of high-content white peony root effective composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Applicant after: Tasly Pharmaceutical Group Co., Ltd. Address before: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Applicant before: Tianjin Tianshili Pharmaceutical Co., Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: TIANJIN TASLY PHARMACEUTICAL CO., LTD. TO: TASLY PHARMACEUTICAL GROUP CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee after: Tasly Pharmaceutical Group Limited by Share Ltd Address before: 300410 Tianjin City Hedong District of Beichen Puji Road No. 2 city of the modern Chinese Medicine Patentee before: Tasly Pharmaceutical Group Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140917 Termination date: 20201113 |