CN105669799A - Method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin - Google Patents
Method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin Download PDFInfo
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- CN105669799A CN105669799A CN201510980882.7A CN201510980882A CN105669799A CN 105669799 A CN105669799 A CN 105669799A CN 201510980882 A CN201510980882 A CN 201510980882A CN 105669799 A CN105669799 A CN 105669799A
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- exchange resin
- cation exchange
- flos lonicerae
- chromatographic column
- lonicerae extract
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin, wherein the method includes the steps of: a) soaking the cation exchange resin with an ethanol solution being 20% in volume fraction for packing a column; b) packing the treated cation exchange resin treated in the step a) as a filler in the chromatographic column; c) with an equilibrium liquid, equilibrating the chromatographic column for loading the sample; d) dissolving a crude product of a honeysuckle extract in deionized water to prepare a honeysuckle extract solution; e) injecting the honeysuckle extract solution into the chromatographic column; and f) eluting the target substance from the chromatographic column with an eluent. The method is simple in operation, is less in energy consumption, is short in time consumption, is low in cost and is high in purity. The method overcomes the defects of complex steps and operations, high cost, low yield and low purity of a conventional process.
Description
Technical field
The present invention relates to a kind of method separating the disconnected Semen Strychni glycoside hemiacetal lactone of Flos Lonicerae extract iridoid apoplexy due to endogenous wind table, particularly a kind of method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table, belongs to medical industry purification technique field.
Background technology
Flos Lonicerae, have another name called Radix Ophiopogonis, containing chlorogenic acid, luteolin glycosides, the pharmacological components such as iridoids, to Hemolytic streptococcus, the various pathogens such as staphylococcus aureus and upper respiratory tract infection Causative virus etc. have stronger restraint, additionally also can enhancing immunity, antiearly pregnancy, hepatoprotective, antitumor, antiinflammatory, antipyretic, blood sugar lowering, hemostasis (blood coagulation), suppress intestinal absorption cholesterol etc., the disconnected Semen Strychni glycoside hemiacetal lactone of the table of its iridoid apoplexy due to endogenous wind is a kind of compound of up-to-date and more difficult extraction, there is various active, antibacterial, blood sugar lowering, antitumor, the effect of the aspects such as treatment hepatitis B. wherein the inhibitory action of bacterial biof iotalm is highlighted, there is very big medical value, be a kind of novel medicinal natural extract compound. at present on the market but without the large-scale production of this type product and sale, it is critical only that and be extremely difficult to purity requirement, hinder the yield of this type of new compound.
Summary of the invention
The present invention seeks to: for the problems referred to above, it is provided that a kind of method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table, method is simple to operate, and energy consumption is little, and consuming time short, cost is low, and purity is high. Overcoming conventional process numerous and diverse, troublesome poeration, cost is high, and yield is little, the problem that purity is not high.
The technical scheme is that a kind of method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table, it is characterised in that the method comprises the following steps:
A, use 20% alcoholic solution cation exchange resin is soaked, post to be installed;
B, will load in chromatographic column as filler through the step a cation exchange resin processed;
C, utilize balance liquid that chromatographic column is balanced, treat loading;
D, by Flos Lonicerae extract dissolving crude product in deionized water, obtain Flos Lonicerae extract solution;
Described step d and described step a, step b, step c order in no particular order;
E, the step d Flos Lonicerae extract solution prepared is injected in described chromatographic column;
F, utilize eluent that object is eluted from described chromatographic column.
The present invention, on the basis of technique scheme, also includes following preferred version:
In described step c, utilize balance liquid that chromatographic column is balanced 2～3 column volumes.
The model of described cation exchange resin is CGC50*4.
In described step f, described eluent is electrical conductivity is the sodium-chloride water solution of 800us/cm.
In described step c, described balance liquid is electrical conductivity is the sodium-chloride water solution of 6ms/cm.
The method also comprises the steps:
G, according to collection of illustrative plates show information be collected, purity to be detected;
Component information after h, liquid phase analysis purification.
The invention have the advantage that
1, the present invention utilizes the repeatedly different fillers that type of elution instead of prior art to repeat eluting, and Financial cost and time cost are greatly reduced.
2, eluting solvent used in the present invention is simple, nontoxic, and low price is conducive to industrial mass production. Furthermore the purity after separation purification of the present invention is higher, exceed the highest purity that can reach of present technology.
3, the present invention can reduce the operating time in a large number, and efficiency is high, it is possible to saves substantial amounts of man power and material, meets industrialized production requirement.
Accompanying drawing explanation
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below the accompanying drawing used required during embodiment is described is briefly described, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is the analysis collection of illustrative plates of the disconnected Semen Strychni glycoside hemiacetal lactone of table in the embodiment of the present invention. In this figure, horizontal axis representing time, its unit is min; The longitudinal axis represents uv absorption height, and its unit is ultraviolet absorption value mAu; Curve is uv absorption wavelength curve, above data mainly show the percentage composition of each component in the retention time of sample and sample. This width figure indicates the purity finally making sample, and in figure, 6.5min main peak is the disconnected Semen Strychni glycoside hemiacetal lactone of table, it can be seen that the purity of the disconnected Semen Strychni glycoside hemiacetal lactone of table is more than 98%.
Detailed description of the invention
Below in conjunction with specific embodiment, such scheme is described further. Should be understood that these embodiments to be an illustration for the present invention and be not limited to restriction the scope of the present invention. The implementation condition adopted in embodiment can do further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
This method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table that this enforcement is disclosed, comprises the following steps:
A, filler pre-treatment: cation exchange resin is soaked by the alcoholic solution using mass fraction to be 20%, post to be installed.
Specification and the model of described cation exchange resin are not limit, and all can reach ideal effect, the cation exchange resin that this example specifically adopts model to be CGC50*4.
B, will load in chromatographic column as filler through the step a cation exchange resin processed.
The selection of chromatographic column, separation case can select suitable blade diameter length ratio per sample. Dress post process can utilize deionized water to be compressed by equipment, until compacting.
C, balance: utilize balance liquid that chromatographic column is balanced, generally balance 2～3 column volumes, treat loading after balance. In this example, this balance liquid is electrical conductivity is the sodium-chloride water solution of 6ms/cm.
D, by Flos Lonicerae extract dissolving crude product in deionized water, obtain Flos Lonicerae extract solution.
Described step d and step a, step b, step c order in no particular order, namely step d can carry out before step a or step b or step c, it is also possible to carries out after step a or step b or step c, and the order of step a, step b and step c is fixed.
E, loading: the step d Flos Lonicerae extract solution prepared is injected in described chromatographic column. According to bed volume and packing volume etc., best applied sample amount need to be selected.
F, utilize eluent that object is eluted from chromatographic column. In this example, this eluent is electrical conductivity is the sodium-chloride water solution of 800us/cm.
In order to disconnected for the table in object Semen Strychni glycoside hemiacetal lactone centralized collection be got up, this example has also carried out following steps:
G, the Semen Strychni glycoside hemiacetal lactone that breaks according to collection of illustrative plates display information his-and-hers watches are collected, purity to be detected.
H is as it is shown in figure 1, by the component information after liquid phase analysis purification, it can be seen that the purity of the disconnected Semen Strychni glycoside hemiacetal lactone of table is more than 98%.
Certainly, above-described embodiment only for technology design and the feature of the present invention are described, its object is to allow people will appreciate that present disclosure and to implement according to this, can not limit the scope of the invention with this. All equivalent transformations done according to the spirit of main technical schemes of the present invention or modification, all should be encompassed within protection scope of the present invention.
Claims (6)
1. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table, it is characterised in that the method comprises the following steps:
A, use 20% alcoholic solution cation exchange resin is soaked, post to be installed;
B, will load in chromatographic column as filler through the step a cation exchange resin processed;
C, utilize balance liquid that chromatographic column is balanced, treat loading;
D, by Flos Lonicerae extract dissolving crude product in deionized water, obtain Flos Lonicerae extract solution;
Described step d and described step a, step b, step c order in no particular order;
E, the step d Flos Lonicerae extract solution prepared is injected in described chromatographic column;
F, utilize eluent that object is eluted from described chromatographic column.
2. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table according to claim 1, it is characterized in that: in described step c, utilize balance liquid that chromatographic column is balanced 2～3 column volumes.
3. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table according to claim 1, it is characterised in that: the model of described cation exchange resin is CGC50*4.
4. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table according to claim 1, it is characterized in that: in described step f, described eluent is electrical conductivity is the sodium-chloride water solution of 800us/cm.
5. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table according to claim 1, it is characterized in that: in described step c, described balance liquid is electrical conductivity is the sodium-chloride water solution of 6ms/cm.
6. the method utilizing the disconnected Semen Strychni glycoside hemiacetal lactone of cation exchange resin separation Flos Lonicerae extract iridoid apoplexy due to endogenous wind table according to claim 1, it is characterised in that the method also comprises the steps:
G, according to collection of illustrative plates show information be collected, purity to be detected;
Component information after h, liquid phase analysis purification.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510980882.7A CN105669799A (en) | 2015-12-24 | 2015-12-24 | Method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510980882.7A CN105669799A (en) | 2015-12-24 | 2015-12-24 | Method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin |
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| CN105669799A true CN105669799A (en) | 2016-06-15 |
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| CN201510980882.7A Pending CN105669799A (en) | 2015-12-24 | 2015-12-24 | Method of separating epivogeloside from iridoids in extracts of honeysuckles through cation exchange resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117284A (en) * | 2016-07-11 | 2016-11-16 | 山东省分析测试中心 | The method of six kinds of iridoid glycoside constituents in Extraction and enrichment Flos Lonicerae while of a kind of |
| CN112973806A (en) * | 2021-02-09 | 2021-06-18 | 珠海高新区维得力生物工程有限公司 | Chromatographic separation filler applied to fructo-oligosaccharide, preparation process and chromatographic separation device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085795A (en) * | 2006-06-07 | 2007-12-12 | 石家庄汉康生化药品有限公司 | Honeysuckle extract and its preparation method and application |
-
2015
- 2015-12-24 CN CN201510980882.7A patent/CN105669799A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085795A (en) * | 2006-06-07 | 2007-12-12 | 石家庄汉康生化药品有限公司 | Honeysuckle extract and its preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| CHANTAL BERGERON，等: "FLAVONOIDS FROM PYROLA ELLIPTICA", 《PHYTOCHEMISTRY》 * |
| VOKATSOA CHRISTIAN RAKOTONDRAMASY，等: "Regioselective and Stereospecific Amination of Iridoids: Conversion of Aucubin into Aminoside Antibiotic Analogues", 《J. NAT. PROD.》 * |
| 何敏: "金银花对细菌生物膜的抑制作用及其化学成分研究", 《长春中医药大学硕士学位论文》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106117284A (en) * | 2016-07-11 | 2016-11-16 | 山东省分析测试中心 | The method of six kinds of iridoid glycoside constituents in Extraction and enrichment Flos Lonicerae while of a kind of |
| CN106117284B (en) * | 2016-07-11 | 2019-01-11 | 山东省分析测试中心 | A kind of method of six kinds of iridoid glycoside constituents in while Extraction and enrichment honeysuckle |
| CN112973806A (en) * | 2021-02-09 | 2021-06-18 | 珠海高新区维得力生物工程有限公司 | Chromatographic separation filler applied to fructo-oligosaccharide, preparation process and chromatographic separation device |
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Application publication date: 20160615 |
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