CN105152862A - Method for extracting and preparing solanesol from potato leaf - Google Patents
Method for extracting and preparing solanesol from potato leaf Download PDFInfo
- Publication number
- CN105152862A CN105152862A CN201510582876.6A CN201510582876A CN105152862A CN 105152862 A CN105152862 A CN 105152862A CN 201510582876 A CN201510582876 A CN 201510582876A CN 105152862 A CN105152862 A CN 105152862A
- Authority
- CN
- China
- Prior art keywords
- ethanol
- salanesol
- extract
- potato leaf
- prepare
- 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
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for extracting and preparing solanesol from potato leaf. The method comprises the following steps: leaching the medicinal material powder with ethanol at 80 DEG C under reflux, concentrating the extracting solution, and carrying out two-step high-efficiency purification by macroporous resin column separation and preparative high performance liquid chromatography to obtain the solanesol with the purity of greater than 98%. The method has the advantages of simple technical steps and high purity, and can easily implement scale-up production.
Description
Technical field:
The present invention relates to a kind of method extracted from potato leaf and prepare Salanesol.
Background technology:
Salanesol is the important source material of pharmaceutical synthesis, is the irreplaceable key intermediate of synthesis ubiquinone class medicine.Current many developed countries have produced and must rely on highly purified Salanesol as raw material with the Coenzyme Q10 99.0 of widespread use.Coenzyme Q10 99.0 is applied very extensive in medicines and health protection and cosmetic field, and in recent years along with the Coenzyme Q10 99.0 suggestion raising of consumption and the increase day by day of demand on world market, the demand of world market to Salanesol also grows with each passing day.Therefore prepare high-purity solanesol for further investigation its pharmacological effect and related application significant.
The measuring method of Salanesol is more, all has a large amount of reports both at home and abroad, mainly contains tlc, vapor-phase chromatography, Thin-layer separation-coulometric titration, pillar layer separation weighting method, thin layer chromatography scanning etc., but be generally analytical scale and half preparative-scale, prepare flux very little.
Summary of the invention
The present invention aims to provide a kind of efficient preparation technology extracting from potato leaf and prepare Salanesol, and the content of Salanesol reaches more than 98%.
For achieving the above object, the technical solution used in the present invention is as follows:
From potato leaf, extract and prepare the method for Salanesol: a potato leaf extract, be separated and preparative high-performance liquid chromatographic two step efficiently purifying through macroporous resin column, obtain the Salanesol that purity is greater than 98%, its concrete steps are as follows:
(1) sample extraction:
Potato leaf was pulverized 20 mesh sieves, with ethanolic soln seepage pressure effects, merge ethanol extract, be concentrated into without alcohol taste, obtain ethanol extraction;
(2) resin column separation, impurity removal:
By step (1) ethanol extraction] cross macroporous resin, use water, 40% ethanol, 60% ethanol, 80% ethanol elution successively.Collect 80% ethanol elution thing, be concentrated into without alcohol taste, obtain crude extract.
(3) preparative high-performance liquid chromatographic is refined:
Thick thing dissolve with methanol solution after concentrated, filtering with microporous membrane, high performance liquid preparative chromatography are separated, with methanol/ethanol solution for eluent system, UV-detector 210nm detects, and collects and prepares chromatographic peak main in collection of illustrative plates, and the drying of respective streams part can obtain the Salanesol that purity is greater than 98%.
The detailed process of described step (1) is: the consumption of ethanol is 5-10 times of potato leaf, and diacolation time 6-9 hour, diacolation temperature was 80 DEG C.
The detailed process of described step (2) is: the macroporous resin of use is HZ-801.
The detailed process of described step (3) is: crude extract dissolve with methanol solution, and chromatographic column is Shim-packPREP-ODS chromatographic column (20mm × 250mm, 15 μm).Proportion of mobile phase is: methyl alcohol: ethanol (60:40, V/V), and flow rate of mobile phase is 10mL/min, and sample size is 300 μ L.
Extract from potato leaf extract with the present invention and prepare Salanesol tool and have the following advantages and improve:
1. present invention process is simple.Potato leaf extract prepares two step efficiently purifyings by resin isolation and preparative high performance liquid phase, can obtain highly purified product.Be conducive to maximum resource utilization.
2. present invention process very proper scale metallization processes production.The high performance liquid phase preparation method of development is fast preparation method, be applicable to the preparation of chemical reference substance in enormous quantities, pre-treatment step is had before efficient preparation, avoid the shortcoming that in batch preparation, the decline of preparative column post effect is too fast, moving phase used is not containing additive, can conveniently realize the recycling preparing solvent, reduce the cost of batch preparation.
Accompanying drawing explanation
Fig. 1, Salanesol preparation technology schema;
Fig. 2, Salanesol HPLC preparative chromatography figure (210nm);
Fig. 3, Salanesol HPLC analyze collection of illustrative plates (210nm);
Fig. 4, Salanesol APCI-MS collection of illustrative plates.
Embodiment
Embodiment 1
Potato leaf was pulverized 20 mesh sieves, with 10 times to potato foliage weight ethanolic soln seepage pressure effects 6 hours, merges ethanol extract, reclaim aqueous ethanolic solution, be concentrated into without alcohol taste, obtain ethanol extraction, ethanol extraction is crossed HZ-801 macroporous resin, use water, 40% ethanol, 60% ethanol, 80% ethanol elution successively, the eluate of above-mentioned final step after 80% ethanol elution is collected, above-mentioned obtained eluate is concentrated into without alcohol taste, makes crude extract, by above-mentioned obtained concentrated after crude extract first after through dissolve with methanol solution, through 0.45 μm of filtering with microporous membrane, high performance liquid preparative chromatography is separated, chromatographic column Shim-packPREP-ODS chromatographic column (20mm × 250mm, 15 μm), and then by proportion of mobile phase be: methyl alcohol: ethanol (60:40, V/V), flow rate of mobile phase is the methanol/ethanol eluant solution of 10mL/min, detect through UV-detector 210nm, sample size is 300 μ L, collection retention time is 26.5min-27.5min, collect and prepare chromatographic peak main in collection of illustrative plates, the Salanesol that purity is greater than 98% can be obtained after the drying of respective streams part.
Embodiment 2
Potato leaf is pulverized 20 mesh sieves, with 5 times to potato foliage weight ethanolic soln seepage pressure effects 9 hours, merges ethanol extract.Reclaim aqueous ethanolic solution, be concentrated into without alcohol taste, obtain ethanol extraction; Ethanol extraction is crossed macroporous resin HZ-801, use water, 40% ethanol, 60% ethanol, 80% ethanol elution successively.Collect 80% ethanol elution thing, gained elutriant is concentrated without alcohol taste.Crude extract dissolve with methanol solution after concentrated, through 0.45 μm of filtering with microporous membrane, high performance liquid preparative chromatography is separated, chromatographic column Shim-packPREP-ODS chromatographic column (20mm × 250mm, 15 μm).Proportion of mobile phase is: methyl alcohol: ethanol (60:40, V/V), and flow rate of mobile phase is that 10mL/min, UV-detector 210nm detect, and sample size is 300 μ L.Collection retention time is 26.5min-27.5min, collects and prepares chromatographic peak main in collection of illustrative plates, and the drying of respective streams part can obtain the Salanesol that purity is greater than 98%.
Embodiment 3
Potato leaf is pulverized 20 mesh sieves, with 7 times to potato foliage weight ethanolic soln seepage pressure effects 8 hours, merges ethanol extract.Reclaim aqueous ethanolic solution, be concentrated into without alcohol taste, obtain ethanol extraction; Ethanol extraction is crossed macroporous resin HZ-801, use water, 40% ethanol, 60% ethanol, 80% ethanol elution successively.Collect 80% ethanol elution thing, gained elutriant is concentrated without alcohol taste.Crude extract dissolve with methanol solution after concentrated, through 0.45 μm of filtering with microporous membrane, high performance liquid preparative chromatography is separated, chromatographic column Shim-packPREP-ODS chromatographic column (20mm × 250mm, 15 μm).Proportion of mobile phase is: methyl alcohol: ethanol (60:40, V/V), and flow rate of mobile phase is that 10mL/min, UV-detector 210nm detect, and sample size is 300 μ L.Collection retention time is 26.5min-27.5min, collects and prepares chromatographic peak main in collection of illustrative plates, and the drying of respective streams part can obtain the Salanesol that purity is greater than 98%.
Claims (7)
1. from potato leaf, extract and prepare a method for Salanesol, it is characterized in that, the method comprises the following steps:
(1) sample extraction:
Potato leaf was pulverized 20 mesh sieves, with ethanolic soln seepage pressure effects, merges ethanol extract, be concentrated into without alcohol taste, obtain ethanol extraction;
(2) resin column separation, impurity removal:
Step (1) ethanol extraction is crossed macroporous resin, uses water, 40% ethanol, 60% ethanol, 80% ethanol elution successively, collect 80% ethanol elution thing, above-mentioned obtained eluate is concentrated into without alcohol taste, makes crude extract;
(3) preparative high-performance liquid chromatographic is refined:
Crude extract obtained for step (2) is successively separated through dissolve with methanol, filtering with microporous membrane, high performance liquid preparative chromatography, again with methanol/ethanol solution for eluent system, UV-detector 210nm detects, collect and prepare chromatographic peak main in collection of illustrative plates, the drying of respective streams part can obtain the Salanesol that purity is greater than 98%, and the structural formula of Salanesol is as follows:
2. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: the consumption of described step (1) ethanol be the 5-10 of potato leaf doubly, diacolation time 6-9 hour.
3. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: the diacolation temperature of described step (1) is 80 DEG C.
4. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: the macroporous resin in described step (2) is HZ-801 macroporous resin.
5. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: in described step (3), chromatographic column is
Shim-packPREP-ODS chromatographic column (20mm × 250mm, 15 μm).
6. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: in described step (3), proportion of mobile phase is: methyl alcohol: ethanol (60:40, V/V).
7. a kind ofly as claimed in claim 1 extract from potato leaf and prepare the method for Salanesol, it is characterized in that: in described step (3), flow rate of mobile phase is 10mL/min, and sample size is 300 μ L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510582876.6A CN105152862A (en) | 2015-09-14 | 2015-09-14 | Method for extracting and preparing solanesol from potato leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510582876.6A CN105152862A (en) | 2015-09-14 | 2015-09-14 | Method for extracting and preparing solanesol from potato leaf |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105152862A true CN105152862A (en) | 2015-12-16 |
Family
ID=54793973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510582876.6A Pending CN105152862A (en) | 2015-09-14 | 2015-09-14 | Method for extracting and preparing solanesol from potato leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105152862A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111474253A (en) * | 2020-04-13 | 2020-07-31 | 中国计量大学 | Preparation method and application of solanesol standard sample |
-
2015
- 2015-09-14 CN CN201510582876.6A patent/CN105152862A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 杨玲娟等: "马铃薯叶中茄尼醇的RP-HPLC分析", 《食品工业科技》 * |
| 王栋良等: "大孔树脂法纯化茄尼醇的研究", 《河北医药》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111474253A (en) * | 2020-04-13 | 2020-07-31 | 中国计量大学 | Preparation method and application of solanesol standard sample |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102070690B (en) | Method for preparing adenosine, cordycepin and N6-(2-hydroxyethyl)adenosine simultaneously used as chemical reference substances | |
| CN102976909B (en) | Method for extracting and purifying 6-gingerol from ginger | |
| CN102924416B (en) | Method for separating and purifying monomeric compounds from ash bark | |
| CN101148410B (en) | Method for extracting high pure chicoric acid from Coneflower | |
| CN101759543B (en) | Method for extracting chalcone from fresh angelica keiskei | |
| CN114989185A (en) | Extraction and preparation method of cepharanthine | |
| CN101525328B (en) | Method for extracting alpha-mangostin from mangosteen fruit peel | |
| CN102617674B (en) | Preparation method of scopolin monomer in anisodus tanguticus root | |
| CN104693249A (en) | Method for simultaneously separating and preparing syringin and oleuropein from syringa oblate lindl. | |
| CN102399259B (en) | Method for separating and purifying liriope spicata saponin B | |
| CN102070683A (en) | Method for simultaneously preparing chemical reference substances of parishin, parishin B and parishin C | |
| CN104072456A (en) | Preparation method of high-purity salvianolic acid B | |
| CN105152862A (en) | Method for extracting and preparing solanesol from potato leaf | |
| CN102267877A (en) | Method for extracting and separating magnolol and honokiol from leaf of magnolia officinalis | |
| CN102503996A (en) | Method for extracting active constituent from Swertia mussotii plant | |
| CN104402949A (en) | Method for simultaneously separating and preparing syringoside and oleuropein from syringa oblata lindl | |
| CN101759641A (en) | Method for extracting and separating huperzine A from huperizia serrata | |
| CN103739648A (en) | Preparation method for mussaendoside U | |
| CN107473996A (en) | The extraction separation method of 4,5,9-trithiadodeca-1,6,11-triene 9-oxide in a kind of garlic | |
| CN102863381A (en) | Novel method for extracting huperzine A from huperzia serrata | |
| CN103242333A (en) | Method for purifying Chapa picrasin | |
| CN102391328B (en) | Method for simultaneously preparing chemical reference substances magnoloside A and magnoloside B | |
| CN105273015A (en) | Preparation method of high-purity paeoniflorin and albiflorin | |
| CN105348338A (en) | Method for extracting and separating paederosidic acid from Saprosma merrillii Lo | |
| CN103739649A (en) | Preparation method for mussaendoside G |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151216 |
|
| RJ01 | Rejection of invention patent application after publication |