CN103012424B - Separation and purification method of notopterol monomer - Google Patents
Separation and purification method of notopterol monomer Download PDFInfo
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- CN103012424B CN103012424B CN201210577581.6A CN201210577581A CN103012424B CN 103012424 B CN103012424 B CN 103012424B CN 201210577581 A CN201210577581 A CN 201210577581A CN 103012424 B CN103012424 B CN 103012424B
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Abstract
The invention provides a separation and purification method of a notopterol monomer, and belongs to the technical field of traditional Chinese medicines. The separation and purification method comprises the following steps in sequence: based on root stocks of umbelliferae notopterygium root as raw materials, carrying out ethanol solution extraction, ethyl acetate extraction, methanol dissolution and filtration, high-performance preparative liquid chromatography separation and product recycling to obtain the notopterol monomer. According to the preparation method, the optimal technology and parameter conditions are utilized, thus the content of the notopterol in the notopterol monomer is up to more than 98%; and the method is stable in the whole technological process, simple and convenient for operation, high in separating efficiency and low in cost, can realize high-purity separation and preparation of the notopterol monomer as mass.
Description
Technical field
The present invention relates to a kind of preparation method of plant compound monomer, from notopterygium root, especially extract the separation purification method of Notopterol monomer, belong to technical field of traditional Chinese medicines.
Background technology
The dry rhizome that notopterygium root (Rhizoma et Radix Notopterygii) is samphire notopterygium root Notopterygium incisum Ting ex H. T. Chang or root and rhizome of Forbes Notopterygium Notopterygium forbesii Boiss. and root.Notopterygium root bitter warm in nature, pungent, enter bladder, kidney channel.There is loose exterior cold curing rheumatism, the effect in sharp joint.Control catch cold, have a headache lossless, the strong muscular contracture of arthralgia due to wind-cold-dampness pathogen BI syndrome, item, joint are ached, geomantic omen edema, the swollen sore of pain etc.
Notopterol is Notopterol again, incised Notopterygium, and molecular formula is C
21h
22o
5, molecular weight is 354.40, and structural formula is as follows:
Notopterol derives from umbelliferae Notopterygium plant notopterygium root
notopterygium incisumthe dry rhizome of Ting ex H. T. Chang is the main active ingredient in notopterygium root medicinal material, has the effects such as analgesia, calmness and anti-inflammatory.
According to coordinate indexing, at present for the refining main method adopting conventional column chromatography and silica gel column chromatography and crystallization phases to combine of Notopterol monomer, its production cycle is long, and reagent waste is serious, and product yield is low.
Summary of the invention
A kind of easy sharp separation is the object of the present invention is to provide to prepare the method for high-content high purity Notopterol.The method separation efficiency is high, with short production cycle, and process stabilizing is easy and simple to handle, with low cost, and the high purity (more than 98%) that can realize a large amount of Notopterol monomer is separated preparation.
In order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A kind of separation purification method of Notopterol monomer, it is characterized in that with the rhizome of samphire notopterygium root for raw material, obtain Notopterol monomer by extraction, extraction, dissolution filter, high performance preparative liquid chromatography separation, Product recycling process, specifically comprise following processing step:
1) extract
Notopterygium root rhizome is ground into the meal of 1 ~ 4mm, by volume/quality adds the methanol solution of 6 ~ 10 times, extracts 3 ~ 4 times, each 2 ~ 3 hours, reclaims methyl alcohol, merges filtered liquid, treats that next step processes;
The concentration of volume percent of described methanol solution is 80 ~ 95%.
2) extract
By step 1) filtered liquid of gained, add isopyknic extraction into ethyl acetate 3 ~ 4 times, point get upper solution, be concentrated into dry, gained solids treats that next step processes;
3) dissolution filter
According to solids quality: solvent volume=1g:(5 ~ 8) mL, by step 2) solids of gained adds dissolve with methanol, filter lysate, namely filtered liquid is the raw material preparing Notopterol monomer;
4) HPLC preparation
Chromatographic column filler is: C
18filler;
Moving phase is: acetonitrile-aqueous solution V/V=50:50;
Get the filtered liquid sample introduction of step 3) gained, online ultraviolet monitoring, determined wavelength is 326nm, collects target compound and prepares solution, carry out the preparation of Notopterol monomer;
5) Product recycling
The HPLC of step 4) gained is prepared liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, 45 DEG C are concentrated into and do and obtain Notopterol monomer.
The invention has the advantages that:
1. the present invention makes Notopterol be transferred in ethyl acetate solution from extraction concentrated aqueous solution by extraction, not only increases target concentration, simultaneously because ethyl acetate is easy to concentrated, also reduces energy consumption.
2. the present invention adopts preparative high performance liquid chromatography system to carry out separation and purification to Notopterol monomer, reach good separating effect, and by online ultraviolet monitoring, collect Notopterol monomer targetedly, with clearly defined objective, avoid the wasting of resources that conventional column chromatography etc. causes, and be convenient to control quality product, product purity can reach more than 98%.
3. because high performance liquid chromatography requires higher to the color and luster, purity etc. of sample, the extracting solution obtained by simple process can not direct injection, if therefore before carrying out high performance liquid chromatography separation, not in accordance with the inventive method step, pre-treatment is carried out to sample introduction solution, then not only separating effect is bad, but also may cause instrument and have a strong impact on (as shortened the life-span etc.), and then increase the production cost of product.
4. for the physico-chemical property of the various compositions existed in notopterygium root medicinal material, the inventive method is by abovementioned steps 1), 2), 3) order collocation, and suitable parameters combination, the compositions such as Notopterol are effectively extracted, and eliminate a large amount of impurity, obtain the sample solution that can enter preparative high performance liquid chromatography system thus, very large impact can not be caused on highly effective liquid phase chromatographic system, extend its life cycle as far as possible, save production cost.
5., in high performance liquid chromatography sepn process, selection and the combination thereof of each chromatographic condition are very important, because it directly affects the appearance time, peak shape etc. of material; Chromatographic condition mainly comprises chromatographic column (comprising filler, column length, column temperature etc.), moving phase (comprising composition, flow velocity etc.), detector and determined wavelength etc.The present invention, by a large amount of experimental studies and comparative analysis, determines above-described chromatographic condition, thus makes the appearance time of material, peak shape, separating effect etc. reach optimizing, achieves the high efficiency separation of Notopterol monomer.
Accompanying drawing explanation
Fig. 1 is the HPLC collection of illustrative plates of the embodiment of the present invention 1 gained Notopterol monomer product.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but this should be interpreted as the present invention is only limitted to following embodiment.
In following each embodiment, the purity of finished product Notopterol monomer is rechecked and is all adopted inverse analysis type liquid chromatography (RP-HPLC) method, and chromatographic condition is as follows:
Filler is C
18, moving phase is acetonitrile-aqueous solution (45:55), and column temperature is 30 DEG C, and flow velocity is 1.0mL/min, and determined wavelength is 326 nm.
embodiment 1
A separation purification method for Notopterol monomer, comprises following processing step:
1) extract
Notopterygium root medicinal material 1kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 10L concentration of volume percent is 90%, extract 3 times, each 2 hours, reclaim methyl alcohol, merge filtered liquid, altogether 2.9L;
2) extract
By step 1) filtered liquid of gained, add isopyknic extraction into ethyl acetate 3 times, point get upper solution, be concentrated into dry, obtain solids 80g;
3) dissolution filter
Step 2) gained solids adds 400mL dissolve with methanol, and filter lysate, obtain filtered liquid 400mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 8cm;
Moving phase consists of: acetonitrile-aqueous solution (50:50)
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size is 10g/ pin (the dry product weighing scale with contained by filtered liquid), carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, collection obtains target compound and prepares solution 3000mL, carries out the preparation of Notopterol monomer;
Before carrying out high performance preparative liquid chromatography separation, the peak shape of Notopterol monomer in high performance liquid chromatography is determined by liquid-mass chromatography method (chromatographic condition is the same), get step 3) gained filtered liquid sample introduction, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography.
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C are concentrated into and dryly obtain Notopterol monomer product 4.0 grams.
About 2.5 days whole Production Flow Chart used times.
Calculating product yield is (4.0/1000) × 100%=0.40%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 98.85%.
embodiment 2
A separation purification method for Notopterol monomer, comprises following processing step:
1) extract
Notopterygium root medicinal material 10kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 90L concentration of volume percent is 95%, extract 4 times, each 3 hours, reclaim methyl alcohol, merge filtered liquid, altogether 18L;
2) extract
By step 1) filtered liquid of gained, add isopyknic extraction into ethyl acetate 4 times, point get upper solution, be concentrated into dry, obtain solids 85g;
3) dissolution filter
Step 2) gained solids adds 680mL dissolve with methanol, and filter lysate, obtain filtered liquid 680mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 10cm;
Moving phase consists of: acetonitrile-aqueous solution (50:50)
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size is 15g/ pin (the dry product weighing scale with contained by filtered liquid), carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, collection obtains target compound and prepares solution 4200mL, carries out the preparation of Notopterol monomer;
Before carrying out high performance preparative liquid chromatography separation, the peak shape of Notopterol monomer in high performance liquid chromatography is determined by liquid-mass chromatography method (chromatographic condition is the same), get the filtered liquid sample introduction of step 3) gained, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography.
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C concentrated draws and dryly obtain Notopterol monomer product 42.0 grams.
About 4 days whole Production Flow Chart used times.
Calculating product yield is (42.0/10000) × 100%=0.42%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 98.65%.
embodiment 3
A separation purification method for Notopterol monomer, comprises following processing step:
1) extract
Notopterygium root medicinal material 50kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 300L concentration of volume percent is 80%, extract 3 times, each 2 hours, reclaim methyl alcohol, merge filtered liquid, altogether 125L;
2) extract
By step 1) filtered liquid of gained, add isopyknic extraction into ethyl acetate 3 times, point get upper solution, be concentrated into dry, obtain solids 410g;
3) dissolution filter
Step 2) gained solids adds 2460mL dissolve with methanol, and filter lysate, obtain filtered liquid 2460mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 15cm;
Moving phase consists of: acetonitrile-aqueous solution (50:50)
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size is 20g/ pin (the dry product weighing scale with contained by filtered liquid), carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, collection obtains target compound and prepares solution 15000mL, carries out the preparation of Notopterol monomer;
Before carrying out high performance preparative liquid chromatography separation, the peak shape of Notopterol monomer in high performance liquid chromatography is determined by liquid-mass chromatography method (chromatographic condition is the same), get the filtered liquid sample introduction of step 3) gained, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography.
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C concentrated draws and dryly obtain Notopterol monomer product 200 grams.
About 7 days whole Production Flow Chart used times.
Calculating product yield is (200/50000) × 100%=0.4%.
By changing mobile phase composition, utilize inverse analysis type liquid chromatography (RP-HPLC) to recheck product purity, recording result is 99.5%.
Claims (3)
1. a separation purification method for Notopterol monomer, is characterized in that processing step is as follows:
1) extract
Notopterygium root medicinal material 1Kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 10L concentration of volume percent is 90%, extract 3 times, each 2 hours, reclaim methyl alcohol, merge filtered liquid, altogether 2.9L;
2) extract
By the filtered liquid of step 1) gained, add isopyknic extraction into ethyl acetate 3 times, divide and get upper solution, be concentrated into dry, obtain solids 80g;
3) dissolution filter
Step 2) gained solids adds 400mL dissolve with methanol, and filter lysate, obtain filtered liquid 400mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 8cm;
Moving phase consists of: acetonitrile-aqueous solution V/V=50:50;
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size counts 10g/ pin by the dry product weight contained by filtered liquid, carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, and collection obtains target compound and prepares solution 3000mL;
Before carrying out high performance preparative liquid chromatography separation, by the peak shape of Notopterol monomer in the liquid-mass chromatography method determination high performance liquid chromatography identical with HPLC preparative chromatography condition, get step 3) gained filtered liquid sample introduction, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography;
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C are concentrated into and dryly obtain Notopterol monomer product 4.0 grams;
2.5 days whole Production Flow Chart used times;
Calculating product yield is 4.0/1000 × 100%=0.40%;
By changing mobile phase composition, utilize inverse analysis type liquid chromatography RP-HPLC to recheck product purity, recording result is 98.85%.
2. a separation purification method for Notopterol monomer, is characterized in that processing step is as follows:
1) extract
Notopterygium root medicinal material 10Kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 90L concentration of volume percent is 95%, extract 4 times, each 3 hours, reclaim methyl alcohol, merge filtered liquid, altogether 18L;
2) extract
By the filtered liquid of step 1) gained, add isopyknic extraction into ethyl acetate 4 times, divide and get upper solution, be concentrated into dry, obtain solids 85g;
3) dissolution filter
Step 2) gained solids adds 680mL dissolve with methanol, and filter lysate, obtain filtered liquid 680mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 10cm;
Moving phase consists of: acetonitrile-aqueous solution V/V=50:50;
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size counts 15g/ pin by the dry product weight contained by filtered liquid, carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, and collection obtains target compound and prepares solution 4200mL;
Before carrying out high performance preparative liquid chromatography separation, by the peak shape of Notopterol monomer in the liquid-mass chromatography method determination high performance liquid chromatography identical with HPLC preparative chromatography condition, get step 3) gained filtered liquid sample introduction, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography;
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C concentrated draws and dryly obtain Notopterol monomer product 42.0 grams;
4 days whole Production Flow Chart used times;
Calculating product yield is 42.0/10000 × 100%=0.42%;
By changing mobile phase composition, utilize inverse analysis type liquid chromatography RP-HPLC to recheck product purity, recording result is 98.65%.
3. a separation purification method for Notopterol monomer, is characterized in that processing step is as follows:
1) extract
Notopterygium root medicinal material 50Kg is ground into the meal of 1 ~ 4mm, adds the methanol solution that 300L concentration of volume percent is 80%, extract 3 times, each 2 hours, reclaim methyl alcohol, merge filtered liquid, altogether 125L;
2) extract
By the filtered liquid of step 1) gained, add isopyknic extraction into ethyl acetate 3 times, divide and get upper solution, be concentrated into dry, obtain solids 410g;
3) dissolution filter
Step 2) gained solids adds 2460mL dissolve with methanol, and filter lysate, obtain filtered liquid 2460mL;
4) HPLC preparation
Employing filler is C
18chromatographic column, post specification is 50cm × 15cm;
Moving phase consists of: acetonitrile-aqueous solution V/V=50:50;
Determined wavelength is 326nm, ambient operation;
Get the filtered liquid sample introduction of step 3) gained, sample size counts 20g/ pin by the dry product weight contained by filtered liquid, carries out the preparative separation of Notopterol monomer, online ultraviolet monitoring, and collection obtains target compound and prepares solution 15000mL;
Before carrying out high performance preparative liquid chromatography separation, by the peak shape of Notopterol monomer in the liquid-mass chromatography method determination high performance liquid chromatography identical with HPLC preparative chromatography condition, get step 3) gained filtered liquid sample introduction, carry out the preparative separation of Notopterol monomer, according to mass spectrometric detection result, determine the peak shape that Notopterol monomer is corresponding in liquid chromatography;
5) Product recycling
The HPLC of step 4) gained prepares liquid, reclaims acetonitrile, remaining aqueous solution isopyknic extraction into ethyl acetate 2 times, and 45 DEG C concentrated draws and dryly obtain Notopterol monomer product 200 grams;
7 days whole Production Flow Chart used times;
Calculating product yield is 200/50000 × 100%=0.40%;
By changing mobile phase composition, utilize inverse analysis type liquid chromatography RP-HPLC to recheck product purity, recording result is 99.5%.
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| CN105106259A (en) * | 2015-09-15 | 2015-12-02 | 中国科学院西北高原生物研究所 | Method for preparing colon cancer resistance notopterygium extract powder in scale mode |
| CN106674240B (en) * | 2016-12-30 | 2019-03-29 | 成都普思生物科技股份有限公司 | The isolation and purification method of alicyclic monomer in a kind of different RADIX PEUCEDANI |
| CN109912614A (en) * | 2019-02-25 | 2019-06-21 | 中国人民解放军北部战区总医院 | Rhizoma Et Radix Notopterygii alcohol extract, Notopterol, Rhizoma Et Radix Notopterygii phenol and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102366429A (en) * | 2007-08-07 | 2012-03-07 | 北京北大维信生物科技有限公司 | Application of extract of Chinese herbal medicine notopterygium root in preparing medicines for reducing weight and fat or medicines having effect of inhibiting lipase activity |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102366429A (en) * | 2007-08-07 | 2012-03-07 | 北京北大维信生物科技有限公司 | Application of extract of Chinese herbal medicine notopterygium root in preparing medicines for reducing weight and fat or medicines having effect of inhibiting lipase activity |
Non-Patent Citations (4)
| Title |
|---|
| Discovery of cyclooxygenase inhibitors from medicinal plants used to treat inflammation;Hongmei Cao等;《Pharmacological Research》;20101231;第61卷;第519-524页 * |
| 中药羌活质量标准研究;陈燕等;《药物分析杂志》;20101231;第30卷(第5期);946-947、949页 * |
| 张文学.中药羌活的化学成分研究.《山西中医学院学报(中药制剂工程与技术)》.2008,第9卷(第4期), * |
| 羌活的化学成分;李丽梅等;《中国天然药物》;20070930;第5卷(第5期);第352页 * |
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Address after: 610045 Sichuan city of Chengdu province Wuhou District Wuhou New Town Road No. 8 West two CMC Vuko Patentee after: CHENGDU PUSH BIO-TECHNOLOGY CO., LTD. Address before: 610045 Sichuan city of Chengdu province Wuhou District Vuko two West Road No. 8 Patentee before: Pusi Biological Science & Technology Co., Ltd., Chengdu |