CN114835721A - Extraction method of cepharanthine - Google Patents
Extraction method of cepharanthine Download PDFInfo
- Publication number
- CN114835721A CN114835721A CN202210672747.6A CN202210672747A CN114835721A CN 114835721 A CN114835721 A CN 114835721A CN 202210672747 A CN202210672747 A CN 202210672747A CN 114835721 A CN114835721 A CN 114835721A
- Authority
- CN
- China
- Prior art keywords
- cepharanthine
- extraction
- organic solvent
- aqueous solution
- hydrochloric acid
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/22—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains four or more hetero rings
Abstract
The invention provides a cepharanthine extraction method, which takes Stephania delavayi Diels root as a raw material and adopts organic solvent or alkali-containing organic solvent-aqueous solution for extraction, or adopts hydrochloric acid aqueous solution for percolation extraction.
Description
Technical Field
The invention relates to a method for extracting a natural product, in particular to a method for extracting cepharanthine from root tuber of Stephania delavayi Diels, belonging to the field of natural product extraction.
Background
The Stephania delavayi Diels is the root tuber of Stephania Lour plant of Stephania of Menispermaceae, and the root tuber is large and exposed on the ground, so the famous Stephania delavayi Diels, mainly produced in Yangtze river basin and in southern regions, is a popular drug for folk. One of them is Stephania delavayi (Stephaniae Pigaea) which is mainly used for raising leucocyte, clearing away heat and toxic material, diminishing inflammation and relieving pain, venomous snake bite, innominate toxic swelling, etc. its main medicinal component Cepharanthine (Cepharanthine) content is higher, and it is used for radiotherapy of tumor patient or leucopenia caused by organic solvent of benzene, etc. it has obtained good effect, CN113046327A discloses that Cepharanthine shows extraordinary strong activity in the aspect of resisting new crown virus SARS COV 2, so that it has wide application prospect.
The molecular structural formula of cepharanthine is as follows:
in order to better develop and utilize the medicinal value of Stephania delavayi Diels, improve the yield of cepharanthine and reduce the production cost of cepharanthine, the extraction technology of cepharanthine needs to be deeply researched. The inventor researches the extraction and preparation method of cepharanthine for a long time, and surprisingly discovers that cepharanthine in medicinal materials can be well extracted by using a specific organic solvent or an alkali-containing aqueous solution thereof as an extraction solvent to extract the root powder of the glauca diomphalia Bates or by using a hydrochloric acid aqueous solution to perform percolation extraction, so that a high-content cepharanthine extract is obtained, and the invention is completed.
Disclosure of Invention
The technical scheme of the invention is as follows:
provides a method for extracting cepharanthine, which takes the root tuber of Stephania delavayi Diels as raw material and adopts organic solvent or organic solvent-aqueous solution containing alkali to extract, or adopts 0.2 percent hydrochloric acid aqueous solution to extract by percolation.
Further, the organic solvent is selected from methanol, acetone, ethyl acetate or dichloroethane, the organic solvent content of the alkali-containing organic solvent-aqueous solution is 70-90% (v/v), the alkali is NaOH or KOH, and the dosage of the alkali is 0.5% of the weight of the medicinal materials.
In some embodiments, the extraction method comprises the steps of:
(1) preparing medicinal materials: crushing dried roots of the mountain tortoise, and sieving the crushed roots by a sieve of 10-40 meshes;
(2) extraction: adding organic solvent or alkali-containing organic solvent-water solution 8-10 times the weight of the medicinal materials into the pulverized radix Stephaniae Epigaeae powder, reflux-extracting for three times, each for 2-3 hr in the first two times, and extracting for 1-2 hr in the third time;
(3) concentration: and (3) combining the extracting solutions in the step (2), and concentrating under reduced pressure to remove the solvent to obtain the cepharanthine extract.
In other embodiments, the percolation extraction of the aqueous hydrochloric acid solution comprises the steps of:
(1) preparing medicinal materials: crushing dried roots of the mountain tortoise, and sieving the crushed roots by a sieve of 10-40 meshes;
(2) soaking: adding 3 times of 0.2% hydrochloric acid aqueous solution into the pulverized radix Stephaniae Epigaeae powder, soaking for 10-15 hr while maintaining pH 2-6;
(3) and (3) percolation: percolating the medicinal powder with 15-20 times of 0.1% hydrochloric acid aqueous solution at 50 deg.C, and controlling the flow rate at 0.2-0.4 times of medicinal powder volume/hr;
(4) neutralizing: adjusting the pH of the percolate to be neutral by using 5 percent NaOH or KOH solution;
(5) concentration: and concentrating the neutral percolate to obtain the cepharanthine extract.
The HPLC detection method of the cepharanthine content comprises the following steps:
firstly, chromatographic conditions:
1. a chromatographic column: kromasil 4.6X 250mm 5 μm;
2. mobile phase: a: acetonitrile, B: triethylamine-water solution with pH 8, 70% a, 30% B isocratic elution;
3. flow rate: 1.0 ml/min;
4. detection wavelength: 283 nm;
5. sample introduction amount: 10 mu l of the mixture;
6. column temperature: at 30 ℃.
Secondly, sample preparation:
1. preparing a reference substance: precisely weighing 5mg of cepharanthine reference substance in a 100ml volumetric flask, adding 50ml of methanol, ultrasonically dissolving for 10min, adding 45ml of methanol, ultrasonically dissolving for 20min, cooling, and adding methanol to reach a constant volume of 100 ml.
2. Preparing a test article: precisely weighing a proper amount of a sample (the sample amount is determined according to the content) into a 100ml volumetric flask, adding 50ml of methanol, ultrasonically dissolving for 10min, adding 45ml of methanol, ultrasonically dissolving for 20min, cooling, and adding methanol to fix the volume to 100 ml.
Third, sample determination
The determination method comprises precisely sucking about 10ml of each of the reference solution and the sample solution, discarding the primary filtrate, injecting into liquid chromatograph, quantifying with 20 μ l quantitative loop, determining, and calculating cepharanthine content with external standard method.
Fourthly, calculating the content:
wherein: m Standard sample -is the weight of the cepharanthine standard,
C standard sample The content of the cepharanthine standard substance,
A sample (I) -is the area of the peak of the sample,
A standard sample -is the peak area of the cepharanthine standard,
M sample (I) -is the sample weight.
The method for extracting cepharanthine from the Stephania delavayi Diels provided by the invention has the following advantages:
(1) the method can well extract cepharanthine from Stephania delavayi Diels medicinal material, greatly increase cepharanthine yield, and reduce cepharanthine production cost;
(2) the treatment process is simple and easy to implement, the cost is low, and the economic value is obvious;
(3) reduces the use amount of Stephania cepharantha in the production of Stephania cepharantha and saves resources.
Detailed Description
The present invention is described in further detail with reference to the following examples, but the present invention is not limited thereto, and any equivalent replacement in the field made in accordance with the present disclosure is included in the scope of the present invention.
Example 1
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken, crushed into coarse powder of 30-40 meshes, 1000kg of 100% methanol is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 2 hours, the third time of extraction is carried out for 1 hour, the three extracting solutions are combined, the solvent is removed by decompression concentration, 10.5kg of cepharanthine extract is obtained, and the cepharanthine content is 3%.
Example 2
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken and crushed into 20-30 meshes of coarse powder, 800kg of 80% (v/v) methanol-water solution containing 0.5kg of NaOH prepared in advance is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 2 hours, the third time of extraction is carried out for 1 hour, the three extracting solutions are combined, the solvent is removed by decompression concentration, and 13kg of cepharanthine extract is obtained, and the cepharanthine content is 2.4%.
Example 3
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken, crushed into coarse powder of 30-40 meshes, 1000kg of 100% acetone is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 3 hours, the third time of extraction is carried out for 2 hours, the three extracting solutions are combined, the solvent is removed by decompression concentration, 10.3kg of cepharanthine extract is obtained, and the cepharanthine content is 3.1%.
Example 4
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken and crushed into 20-30 meshes of coarse powder, 800kg of 70% (v/v) acetone-water solution which is prepared in advance and contains 0.5kg of KOH is added for reflux extraction for three times, the first two times of extraction are carried out for 2 hours respectively, the third time of extraction is carried out for 1 hour, the three extracting solutions are combined, the solvent is removed by decompression concentration, 14kg of cepharanthine extract is obtained, and the cepharanthine content is 2.35%.
Example 5
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken, crushed into coarse powder of 30-40 meshes, 1000kg of 100% ethyl acetate is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 3 hours, the third time of extraction is carried out for 2 hours, the three extracting solutions are combined, and the solvent is removed by decompression concentration, so that 9.5kg of cepharanthine extract is obtained, and the cepharanthine content is 3.3%.
Example 6
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken and crushed into 20-30 meshes of coarse powder, 800kg of 90% (v/v) ethyl acetate-water solution which is prepared in advance and contains 0.5kg of NaOH is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 3 hours, the third time of extraction is carried out for 2 hours, the three extracting solutions are combined, the solvent is removed by decompression concentration, 12kg of cepharanthine extract is obtained, and the cepharanthine content is 2.8%.
Example 7
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken, crushed into coarse powder of 30-40 meshes, 1000kg of 100% dichloroethane is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 3 hours, the third time of extraction is carried out for 2 hours, the three extracting solutions are combined, the solvent is removed by decompression concentration, 7kg of cepharanthine extract is obtained, and the cepharanthine content is 4.1%.
Example 8
100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%) is taken and crushed into coarse powder of 30-40 meshes, 900kg of 90% (v/v) dichloroethane-water solution which is prepared in advance and contains 0.5kg of NaOH is added for reflux extraction for three times, the first two times of extraction are respectively carried out for 3 hours, the third time of extraction is carried out for 2 hours, the three extracting solutions are combined, the solvent is removed by concentration under reduced pressure, 11.2kg of cepharanthine extract is obtained, and the cepharanthine content is 2.8%.
Example 9
Taking 100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%), crushing into coarse powder of 30-40 meshes, adding 300kg of 0.2% hydrochloric acid aqueous solution, soaking for 12 hours, and keeping the pH value at 4.0 in the soaking process; after soaking, using 1600kg of 0.2% hydrochloric acid aqueous solution to perform percolation extraction at 50 ℃, and controlling the flow rate at 180 liters/hour; adjusting pH of the percolate with 2% NaOH solution to neutral, and concentrating to dry to obtain cepharanthine extract 8kg with cepharanthine content of 4.0%.
Example 10
Taking 100kg of dried Stephania delavayi Diels medicinal material (the cepharanthine content is 0.35%), crushing into 20-30 meshes of coarse powder, adding 400kg of 0.3% hydrochloric acid aqueous solution, soaking for 10 hours, and keeping the pH value at 2.0 in the soaking process; after soaking, percolating and extracting with 2000kg of 0.2% hydrochloric acid water solution at 50 ℃ with the flow rate controlled at 160 l/h; adjusting pH of the percolate with 2% NaOH solution to neutral, and concentrating to dry to obtain cepharanthine extract 8.8kg with cepharanthine content of 3.8%.
Claims (4)
1. A method for extracting cepharanthine is characterized in that root tuber of Stephania delavayi Diels is used as raw material, and organic solvent or organic solvent-aqueous solution containing alkali is used for extraction, or 0.2% hydrochloric acid aqueous solution is used for percolation extraction.
2. The extraction method according to claim 1, wherein the organic solvent is selected from methanol, acetone, ethyl acetate or dichloroethane, the alkali-containing organic solvent-aqueous solution has an organic solvent content of 70-90% (v/v), and the alkali is NaOH or KOH, and is used in an amount of 0.5% by weight of the medicinal material.
3. The extraction method according to claim 1 or 2, characterized by comprising the steps of:
(1) preparing medicinal materials: crushing dried roots of the mountain tortoise, and sieving the crushed roots by a sieve of 10-40 meshes;
(2) extraction: adding organic solvent or alkali-containing organic solvent-water solution 8-10 times the weight of the medicinal materials into the pulverized radix Stephaniae Epigaeae powder, reflux-extracting for three times, each for 2-3 hr in the first two times, and extracting for 1-2 hr in the third time;
(3) concentration: and (3) combining the extracting solutions in the step (2), and concentrating under reduced pressure to remove the solvent to obtain the cepharanthine extract.
4. The extraction method according to claim 1, characterized in that said percolation extraction of the aqueous solution of hydrochloric acid comprises the following steps:
(1) preparing medicinal materials: crushing dried roots of the mountain tortoise, and sieving the crushed roots by a sieve of 10-40 meshes;
(2) soaking: adding 3 times of 0.2% hydrochloric acid aqueous solution into the pulverized radix Stephaniae Epigaeae powder, soaking for 10-15 hr while maintaining pH 2-6;
(3) and (3) percolation: percolating the medicinal powder with 15-20 times of 0.1% hydrochloric acid aqueous solution at 50 deg.C, and controlling the flow rate at 0.2-0.4 times of medicinal powder volume/hr;
(4) neutralizing: adjusting the pH of the percolate to be neutral by using 5 percent NaOH or KOH solution;
(5) concentration: and concentrating the neutral percolate to obtain the cepharanthine extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672747.6A CN114835721A (en) | 2022-06-15 | 2022-06-15 | Extraction method of cepharanthine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210672747.6A CN114835721A (en) | 2022-06-15 | 2022-06-15 | Extraction method of cepharanthine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114835721A true CN114835721A (en) | 2022-08-02 |
Family
ID=82574037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210672747.6A Pending CN114835721A (en) | 2022-06-15 | 2022-06-15 | Extraction method of cepharanthine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114835721A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115349446A (en) * | 2022-10-19 | 2022-11-18 | 云南植虫药生物科技有限公司 | Method for producing cepharanthine by using tortoise callus |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891750A (en) * | 2010-05-06 | 2010-11-24 | 中国科学院昆明植物研究所 | Preparation method of stephanine and hydrochloride thereof |
| CN102146083A (en) * | 2011-03-10 | 2011-08-10 | 云南汉德生物技术有限公司 | Method for separating and extracting cepharanthine |
| CN104031058A (en) * | 2014-06-30 | 2014-09-10 | 施佩蓓 | Production method of cepharanthin |
| CN106167493A (en) * | 2016-07-06 | 2016-11-30 | 河北大学 | The preparation method of novel cepharanthine and the application on medicine thereof |
-
2022
- 2022-06-15 CN CN202210672747.6A patent/CN114835721A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891750A (en) * | 2010-05-06 | 2010-11-24 | 中国科学院昆明植物研究所 | Preparation method of stephanine and hydrochloride thereof |
| CN102146083A (en) * | 2011-03-10 | 2011-08-10 | 云南汉德生物技术有限公司 | Method for separating and extracting cepharanthine |
| CN104031058A (en) * | 2014-06-30 | 2014-09-10 | 施佩蓓 | Production method of cepharanthin |
| CN106167493A (en) * | 2016-07-06 | 2016-11-30 | 河北大学 | The preparation method of novel cepharanthine and the application on medicine thereof |
Non-Patent Citations (5)
| Title |
|---|
| JIN HU-I ZI，等: "Alkaloids from Stephania epigaea", 《中国天然药物》, vol. 5, no. 2, pages 112 - 114 * |
| JUN-JIANG LV，等: "Cytotoxic Bisbenzylisoquinoline Alkaloids from Stephania epigaea", 《J. NAT. PROD.》, vol. 76, pages 926 - 932 * |
| 左爱学，等: "民族药物河谷地不容的生物碱成分研究", 《云南民族大学学报（自然科学版）》, vol. 20, no. 1, pages 17 - 19 * |
| 李兴: "千金藤属植物地不容的生药学及化学成分研究", 《西南大学硕士学位论文》, pages 27 * |
| 邹月芝，等: "地不容中提取千金藤素方法的改进", 《药学情报通讯》, vol. 6, no. 1, pages 7 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115349446A (en) * | 2022-10-19 | 2022-11-18 | 云南植虫药生物科技有限公司 | Method for producing cepharanthine by using tortoise callus |
| CN115349446B (en) * | 2022-10-19 | 2022-12-27 | 云南省农业科学院药用植物研究所 | Method for producing cepharanthine by using tortoise callus |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102875562B (en) | Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen | |
| CN103435486A (en) | Novel method for preparing high-purity chlorogenic acid in honeysuckle | |
| CN102234245A (en) | Method for preparing sulforaphane | |
| CN114835721A (en) | Extraction method of cepharanthine | |
| CN108299453B (en) | Method for separating psoralen, isopsoralen and bakuchiol from fructus psoraleae | |
| CN109851646A (en) | A kind of glutinous rehmannia effective component extraction separation method and the Catalpol and polysaccharide of extraction | |
| CN101591680B (en) | Method for extracting oxidized resveratrol | |
| CN108865904B (en) | Hirsutella sinensis expanding culture medium, hirsutella sinensis cultured by same and culture method | |
| CN111848358A (en) | Method for preparing high-purity cannabidiol by combining macroporous resin enrichment with dynamic axial compression column system | |
| CN103356740B (en) | Preparation method of baicalein and scutellaria baicalensis flavone total-aglycone extractives | |
| CN102558191A (en) | Method for extracting wedelolactone from yerbadetajo herb | |
| CN108218948A (en) | A kind of preparation method of Sodium Aescinate | |
| CN101492350B (en) | Method for producing D-pinit from plant locust | |
| CN102600247A (en) | Corydalis saxicola bunting alkaloid extract and preparation method thereof, as well as extraction method of dehydrocavidine | |
| CN104829474A (en) | Method for preparing glycine betaine chemical reference substances from boxthorn leaves | |
| Wu et al. | Preparation of paeoniflorin from the stems and leaves of Paeonia lactiflora Pall.‘Zhongjiang’through green efficient microwave-assisted extraction and subcritical water extraction | |
| CN111484500A (en) | Preparation method of tetrandrine | |
| CN107753531B (en) | Wenwang-herba violae extract and application thereof in preparing anti-cancer drugs | |
| CN108997359A (en) | A method of chlorophyll is extracted from stevioside production waste residue | |
| CN104688798B (en) | A kind of preparation method and application of rosy clouds grass extract | |
| CN109925351A (en) | The extracting method of polyphenols in a kind of leaves of Hawthorn | |
| CN108938677A (en) | A kind of Sargassum polycystum extract and the preparation method and application thereof with treatment breast cancer effect | |
| CN110123862B (en) | Preparation method of honeysuckle extract | |
| CN115197235B (en) | Method for preparing stephanine by enzymolysis extraction | |
| CN110204588B (en) | Method for preparing astragaloside |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |