CN109053835A - A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process - Google Patents
A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process Download PDFInfo
- Publication number
- CN109053835A CN109053835A CN201810915646.0A CN201810915646A CN109053835A CN 109053835 A CN109053835 A CN 109053835A CN 201810915646 A CN201810915646 A CN 201810915646A CN 109053835 A CN109053835 A CN 109053835A
- Authority
- CN
- China
- Prior art keywords
- sowthistle
- leaf ixeris
- ixeris seedling
- extract
- solution
- 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
- 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
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Saccharide Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
Present invention relates particularly to a kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process, belong to Chemistry for Chinese Traditional Medicine extraction purification technical field, technical problem to be solved improves the content of flavones glucoside extract in sowthistle-leaf ixeris seedling, and bind metal ion chelating method effectively improves luteolin -7-O- β-D-Glucose aldehydic acid glycosides (hereinafter referred to as LGU) purifying rate；A kind of technical solution of use are as follows: extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, comprising the following steps: sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；Above-mentioned raw materials are heated to reflux；Then using being filtered under diminished pressure, filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure；Extract after concentration is dry, obtain ixeri sonhifolia extract；A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, using metal ion-chelant method purified extract；Extraction and purifying of the present invention for flavonoid glycoside in sowthistle-leaf ixeris seedling, can effectively improve the purifying rate of flavonoid glycoside.
Description
Technical field
The present invention relates to Chemistry for Chinese Traditional Medicine extraction purification technical fields, and in particular to a kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its
Purification process.
Background technique
Sowthistle-leaf ixeris seedling, also known as babysbreath, irexis sonchifolia etc. mainly originate in the areas such as China northeast, North China.Sowthistle-leaf ixeris seedling taste
It is bitter, pungent, it is cool in nature, there is appetizing, removing toxic substances, synthetism effect is used for do not feel like eating, and fracture is had a toothache.Sowthistle-leaf ixeris seedling contains according to the literature
There are the chemical components such as flavones, lactones, adenosine.Chemical research shows luteolin -7-O- β-D-Glucose aldehydic acid in sowthistle-leaf ixeris seedling
Glycosides (hereinafter referred to as LGU) content highest has a variety of pharmacological activity.
The purification process of currently used flavone compound is mainly column chromatography, such as Adsorption column chro-matography and distribution column
Chromatography etc..The disadvantages of column chromatography has required solvent volume larger in use, and time-consuming.Metal reagent complexed-precipitation method
It is also more and more extensive in flavones purification art application as a kind of purification process emerging in recent years.Flavone compound energy
Enough and Mg2+、Ca2+、Zn2+Equal metal ions form chelate.This method is compared to the above to save the time, reduces organic
The use of solvent, so increasingly focused in recent years, using also more extensively, but this method is to sowthistle-leaf ixeris seedling Huang
The purifying rate of ketoside is to be improved.
Summary of the invention
The invention overcomes the deficiencies of the prior art, and provides flavonoid glycoside extractive contents in a kind of raising sowthistle-leaf ixeris seedling
Method, this extracting method bind metal ion chelating method can effectively improve the purifying rate of LGU.
In order to solve the above-mentioned technical problem, a kind of the technical solution adopted by the present invention are as follows: extraction side of sowthistle-leaf ixeris seedling flavonoid glycoside
Method, comprising the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned methanol soak is heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
Methanol solution is used to impregnate the sowthistle-leaf ixeris seedling time for 15min~30min in the step 1.
It is 2h~4h that the time is heated to reflux in the step 2.
A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, comprising the following steps:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
The amount for the glacial acetic acid being added in the step 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Purifying process research:
The LGU in sowthistle-leaf ixeris seedling sample is carried out using the property that LGU and metal ion are capable of forming chelate under alkaline condition
Purifying, and the influence of different pH, different metal ions to purification result has been investigated, select Mg2+、Zn2+And Ca2+, investigated difference
Each metal ion is to LGU content in the sequestering power and chelate of LGU in methanol solution under the conditions of pH.In pH=8~11 ranges
It is interior, Mg2+、Zn2+And Ca2+The LGU rate of transform and content in chelate are respectively 5.87%~86.61%, 3.44%~12.68%；
60.40%~89.42%, 3.25%~4.01%；71.25%~91.08%, 1.77%~3.85%.Wherein, the sequestering power of zinc is most
By force, LGU content improves limited more before purification but in chelate products, and the sequestering power of magnesium is slightly weak compared with other two metal ion species, but
LGU content improves a lot more before purification in chelate products, and LGU content is 2.24% in sowthistle-leaf ixeris seedling sample before purification, through Mg2+It is pure
After change, LGU content can reach 12.68% in product, and purification effect is significant, therefore choose Mg2+To LGU in sowthistle-leaf ixeris seedling sample into
Row purifying.The change of pH has large effect to purification effect, when in pH=9.0~9.5 ranges, Mg2+With sowthistle-leaf ixeris seedling sample shape
At chelate in LGU content reach high value, therefore determine that the Optimal pH of purifying should be 9.0~9.5, the best purifying work that determines
Skill are as follows: use Mg2+, purification effect is best when pH=9.0, and the content of LGU is 12.68% in purified product.
Compared with the prior art, the invention has the beneficial effects that:
One, the present invention extracts the flavonoid glycoside in sowthistle-leaf ixeris seedling using heating reflux method, and extraction process is quality controllable, and medicinal ingredient extracts
Rate is high, and stability is strong.
Two, the flavonoid glycoside that the present invention is extracted using heating reflux method, bind metal ion chelate the purifying process of method, make hardship
The purifying rate of plate flavonoid glycoside is high.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, comprising the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned raw materials are heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
Methanol solution is used to impregnate the sowthistle-leaf ixeris seedling time for 15min in the step 1.
It is 2h that the time is heated to reflux in the step 2.
A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, comprising the following steps:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
The amount for the glacial acetic acid being added in the step 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Embodiment 2
A kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, comprising the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned raw materials are heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
Methanol solution is used to impregnate the sowthistle-leaf ixeris seedling time for 30min in the step 1.
It is 4h that the time is heated to reflux in the step 2.
A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, comprising the following steps:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
The amount for the glacial acetic acid being added in the step 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Embodiment 3
A kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, comprising the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned raw materials are heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
Methanol solution is used to impregnate the sowthistle-leaf ixeris seedling time for 20min in the step 1.
It is 3h that the time is heated to reflux in the step 2.
A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, comprising the following steps:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
The amount for the glacial acetic acid being added in the step 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Embodiment 4
A kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, comprising the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned raw materials are heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
Methanol solution is used to impregnate the sowthistle-leaf ixeris seedling time for 25min in the step 1.
It is 2.5h that the time is heated to reflux in the step 2.
A kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract, comprising the following steps:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
The amount for the glacial acetic acid being added in the step 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Above embodiment is merely exemplary to illustrate the principle of the present invention and its effect, and is not intended to limit the present invention.For
Person skilled in the art all without departing from the spirit and scope of the present invention, modifies above-described embodiment or is improved.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by tool usually intellectual in all act technical fields
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (5)
1. a kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside, which comprises the following steps:
(1) sowthistle-leaf ixeris seedling is crushed, is impregnated with methanol solution；
(2) above-mentioned methanol soak is heated to reflux；
(3) then filtrate is collected, by Methanol Recovery in filtrate under condition of negative pressure using being filtered under diminished pressure；
(4) extract after concentration is dry, obtain ixeri sonhifolia extract.
2. a kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside according to claim 1, which is characterized in that adopted in the step 1
It is 15min~30min with the methanol solution immersion sowthistle-leaf ixeris seedling time.
3. a kind of extracting method of sowthistle-leaf ixeris seedling flavonoid glycoside according to claim 1, which is characterized in that add in the step 2
Hot return time is 2h~4h.
4. a kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract according to claim 1, which is characterized in that including following
Step:
(1) ixeri sonhifolia extract after weighing drying, being configured to concentration through supersonic oscillations with methanol is 1mg/mL solution, and
Glacial acetic acid is added in the solution, solution filtering is spare；
(2) sowthistle-leaf ixeris seedling filtrate 100mL is taken, the MgCl of 0.1mol/L is added thereto2Methanol solution 5mL, shake well 20min
Afterwards, it is 9.0 that the NaOH solution that 1.5mol/L is added dropwise, which adjusts solution ph, places 4h under the conditions of 4 DEG C after being sufficiently stirred；
(3) it filtering, precipitating is rinsed with the methanol of 20mL, after rinsing twice, (vacuum degree: 2.67kPa) is put into vacuum oven,
It is dried under reduced pressure at room temperature for 24 hours to get LGU-Mg2+Chelate.
5. a kind of purification process of sowthistle-leaf ixeris seedling flavones glucoside extract according to claim 4, which is characterized in that the step
The amount for the glacial acetic acid being added in 1 is that 0.1mL glacial acetic acid is added in every 100mg extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810915646.0A CN109053835A (en) | 2018-08-13 | 2018-08-13 | A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810915646.0A CN109053835A (en) | 2018-08-13 | 2018-08-13 | A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109053835A true CN109053835A (en) | 2018-12-21 |
Family
ID=64683807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810915646.0A Pending CN109053835A (en) | 2018-08-13 | 2018-08-13 | A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109053835A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116211986A (en) * | 2023-04-03 | 2023-06-06 | 北京安德普泰医疗科技有限公司 | A Curcumae rhizoma extract, and its preparation method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634875A (en) * | 2004-11-11 | 2005-07-06 | 中国人民解放军第二军医大学 | Process for rapid preparation of high pure pharmaceutical matters from patrinia villosa juss |
| CN103232504A (en) * | 2013-05-15 | 2013-08-07 | 南京泽朗医药科技有限公司 | Method for preparing cyanidenon-7-O-beta-D-glucuronide |
| CN104277083A (en) * | 2013-07-04 | 2015-01-14 | 河北以岭医药研究院有限公司 | Preparation method and application of luteolin-7-O-beta-D-glucuronide |
| CN105726600A (en) * | 2016-05-04 | 2016-07-06 | 通化华夏药业有限责任公司 | Method for extracting and purifying flavones and phenolic acids in medicinal material ixeris sonchifolia through metal ion chelation |
-
2018
- 2018-08-13 CN CN201810915646.0A patent/CN109053835A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634875A (en) * | 2004-11-11 | 2005-07-06 | 中国人民解放军第二军医大学 | Process for rapid preparation of high pure pharmaceutical matters from patrinia villosa juss |
| CN103232504A (en) * | 2013-05-15 | 2013-08-07 | 南京泽朗医药科技有限公司 | Method for preparing cyanidenon-7-O-beta-D-glucuronide |
| CN104277083A (en) * | 2013-07-04 | 2015-01-14 | 河北以岭医药研究院有限公司 | Preparation method and application of luteolin-7-O-beta-D-glucuronide |
| CN105726600A (en) * | 2016-05-04 | 2016-07-06 | 通化华夏药业有限责任公司 | Method for extracting and purifying flavones and phenolic acids in medicinal material ixeris sonchifolia through metal ion chelation |
Non-Patent Citations (1)
| Title |
|---|
| 韩文志 等: "苦碟子中黄酮苷的分离与结构鉴定", 《科研简报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116211986A (en) * | 2023-04-03 | 2023-06-06 | 北京安德普泰医疗科技有限公司 | A Curcumae rhizoma extract, and its preparation method and application |
| CN116211986B (en) * | 2023-04-03 | 2024-04-30 | 北京安德普泰医疗科技有限公司 | A Curcumae rhizoma extract, and its preparation method and application |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276679B (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN103333067B (en) | A kind of extracting method of high-purity chlorogenic acid | |
| CN103242279B (en) | Method for extracting and purifying flavonoid substances in hawthorn | |
| CN104666427A (en) | Method for extracting main active components of folium mori | |
| CN101265279B (en) | Method for extracting tannin from tarra bean-pod by micro-wave method | |
| CN105985315A (en) | Method for extracting nicotine from tobacco waste | |
| CN109053835A (en) | A kind of extraction of sowthistle-leaf ixeris seedling flavonoid glycoside and its purification process | |
| CN104119229A (en) | Technology for producing pure chlorogenic acid | |
| CN106565795A (en) | Method for extracting alkaloid from bitter gourds | |
| CN103463160A (en) | Preparation method of high-content total flavones of chrysanthemum | |
| CN113827626A (en) | Method for extracting ginkgolic acid by using waste liquid in processing process of ginkgo leaf extract | |
| CN105062687A (en) | Method for extracting eucalyptus oil and hydrolyzing tannin to prepare ellagic acid at the same time | |
| CN106038737B (en) | A kind of method that ultrasonic wave couples extraction Sorbus alnifolia flavones with double-aqueous phase system | |
| CN104450822A (en) | Method for producing theaflavin from tea polyphenol production wastewater | |
| CN112300234A (en) | Method for extracting isoflavone, isoflavone extracted by method and application of isoflavone | |
| CN106318617A (en) | Preparation method of low-As-content tree moss absolute oil | |
| CN105412167A (en) | Method for extracting and separating ginkgo flavone and ginkgolide from ginkgo leaves | |
| CN103833805A (en) | Process for refining glycyrrhizinic acid in liquorice | |
| CN103655642A (en) | Method for preparing ginkgo biloba extract | |
| CN102702287A (en) | Method for extracting purified oleuropein from olive leaves | |
| CN109771475A (en) | A method of extracting polyphenol from purple perilla seed shell | |
| CN111150765B (en) | Fingered citron flavone extract and separation and purification method thereof | |
| CN106344725A (en) | Method for extracting flavone from herba violae | |
| CN102805764A (en) | Novel process for extracting lotus alkaloid by microwave-assisted solvent method | |
| CN102127089B (en) | Method for extracting camptothecin |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181221 |
|
| RJ01 | Rejection of invention patent application after publication |