CN107721927A - A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata - Google Patents
A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata Download PDFInfo
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- CN107721927A CN107721927A CN201711071368.7A CN201711071368A CN107721927A CN 107721927 A CN107721927 A CN 107721927A CN 201711071368 A CN201711071368 A CN 201711071368A CN 107721927 A CN107721927 A CN 107721927A
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- bletilla striata
- extraction purification
- extraction
- alcohol
- coarse powder
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D221/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00
- C07D221/02—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00 condensed with carbocyclic rings or ring systems
- C07D221/04—Ortho- or peri-condensed ring systems
- C07D221/18—Ring systems of four or more rings
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Abstract
The invention discloses a kind of method of the extraction purification bletilla striata alcohol from the bletilla striata, comprise the following steps：By bletilla striata stem tuber with coarse powder is ground into after sterile saline cleaning, drying, addition sterile distilled water progress is closed to swell, and filters moisture content, obtains expanding coarse powder；The coarse powder of expansion is mixed with 88 95% ethanol, alpha amylase is added, refluxing extraction 3 times under microwave heating condition, merges extract solution, once afford a destainer；A destainer in above-mentioned steps is filtered, centrifuged, is depressurized, crystallization, recycles petroleum ether to extract repeatedly 3 times, secondary eluent is eluted to obtain by extract is secondary, concentration, dries, bletilla striata alcohol is made.The method of extraction purification bletilla striata alcohol from the bletilla striata of the present invention is carried out in aseptic condition, nontoxic pollution-free；Extraction rate is fast simultaneously, and purity is high, can effectively increase production efficiency as qualitative, quantitative reference substance.
Description
【Technical field】
The invention belongs to the extractive technique field of natural products effective ingredient, and in particular to one kind extraction purification from the bletilla striata
The method of bletilla striata alcohol.
【Background technology】
The bletilla striata, also known as Lian Jicao, Gan Gen, give free of charge, indocalamus orchid, Zhu Lan, purple blue, purple a species of orchid, hundred large bamboo hats with a conical crown and broad brim, perennial herb bulbous plant
(root tuber), plant is high 18-60 centimetres, is mainly distributed on China, Japan and Upper Myanmar.The main florescence in spring, but according to each
The difference of ground weather, late Winter Solstice early summer may all bloom.The bletilla striata has extensive medical value and Ornamental value.It is mainly used in restraining
Hemostasis, detumescence and promoting granulation.Flower has the colors such as purplish red, white, blue, yellow and powder, can potted plant indoor appreciation, can also intersperse in the flower more covered
One jiao of platform, flower border or garden.
The bletilla striata have anastalsis, whitening spot-removing, convergence go acne print, anti-oxidant, detumescence and promoting granulation, protection gastric mucosa, antibacterial,
Treat effect lungy and effect.Wherein, the dihydro phenanthro- pyran compounds bletilla striata alcohol contained in the bletilla striata, bletilla striata alcohol immersion liquid
There is inhibitory action to staphylococcus aureus, hay bacillus, Bacillus tuberculosis；Infusion has suppression to microsporon audouini
Effect；3 biphenyl classes and 2 double hydrogen phenanthrene class compounds contained by the bletilla striata are read staphylococcus aureus, hay bacillus, white
Pearl bacterium ATCC1057 and trichophyte QM248 have inhibitory action.
Research on the bletilla striata focuses mostly in breeding technology, and the patent ratio of the preparation method of disclosed bletilla striata alcohol and technique
Less, publication CN104997701A " oral care product with anti-helicobacter pylori of the alcohol extracting thing containing the bletilla striata " is open
A kind of extracting method of bletilla striata alcohol, comprises the following steps：Crush, alcohol reflux extract, be filtered under diminished pressure, refluxing extraction, concentration,
Bletilla striata alcohol extracting thing is made, this method is relatively simple, and extraction efficiency is higher, and operability is stronger, it is easy to accomplish industrialized production.
The problem of method of bletilla striata alcohol extracting at present is present be：It is more single using extracting method technique so that in extract
Contained impurity component is more, and purity is low, viscosity deficiency, and index of refraction is low so that bletilla striata alcohol extracting thing is difficult to as qualitative, quantitative
Reference substance.
【The content of the invention】
The method of a kind of extraction purification bletilla striata alcohol from the bletilla striata provided by the invention, to solve current bletilla striata alcohol extracting purity
It is low, it is difficult to the problems such as meeting the requirement as qualitative, quantitative reference substance.
To solve above technical problem, the present invention uses following technical method：
A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata, comprises the following steps：
S1：By bletilla striata stem tuber with coarse powder is ground into after sterile saline cleaning, drying, sterile distilled water is added in 45-
Carried out at 50 DEG C it is closed swell, filter moisture content, obtain expand coarse powder；
S2：The coarse powder of expansion is mixed with 88-95% ethanol, regulation pH of mixed is 5.5-6.5, adds alphalise starch
Enzyme, refluxing extraction 3 times under microwave heating condition, microwave frequency control is 450-550W, merges extract solution, adjusts extract solution
PH value to 6.5-7, temperature control is 35-45 DEG C, by extract solution by decolorization and impurity removal by active carbon, is filtrated to get a destainer；
S3：Destainer in step S2 is filtered, centrifuged, is crystallized after vacuum-concentrcted, solid-liquid in crystallization process
Than for 1:5-7 (W/V), crystal wash crystalline substance to brown color and obtain coarse-grain, and coarse-grain adds the 3-5 times of distilled water measured dissolving, recycles 6-8 times
The petroleum ether of amount extracts 3 times repeatedly, by extract again by decolorization and impurity removal by active carbon, is filtrated to get secondary decolourization liquid, gained
Secondary decolourization liquid is placed in 60-65 Rotary Evaporators, and concentration volume is dried to 5-8%, the bletilla striata is made under 0.9-1.1MPa
Alcohol.
Preferably, in step S1, the sterile saline concentration is 4-5.5%.
Preferably, in step S1, the closed when a length of 24-32h to swell.
Preferably, in step S1, the addition of the sterile distilled water should can submerge coarse powder.
Preferably, in step S2, the ratio of the ethanol mixing of the coarse powder and 88-95% is 1:8-12.
Preferably, in step S2, the alpha-amylase is middle warm type amylase or high temperature modification amylase, and its addition is mixed
Close the 0.1% of liquid mass fraction.
Preferably, in step S2, the temperature of the microwave heating should be controlled at 92-95 DEG C
Preferably, in step S2, a length of 10-15min when the refluxing extraction is extracted.
Preferably, in step S3, the rotating speed of the centrifugation is 600r/min.
Preferably, in step S3, the temperature of the drying is 75-80 DEG C, a length of 3-5h when drying.
The invention has the advantages that：
A kind of method of extraction purification bletilla striata alcohol from the bletilla striata provided by the invention is carried out in aseptic condition, nontoxic no dirt
Dye, the purity of bletilla striata alcohol is effectively ensure that, prepared bletilla striata alcohol purity is high, reaches 99.21-99.62%, product meets conduct
The requirement of qualitative, quantitative reference substance；This method production efficiency is high simultaneously, it is easy to accomplish industrialized production.
【Embodiment】
It is specifically described with reference to specific embodiment.
Embodiment 1
A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata, comprises the following steps：
S1：Coarse powder is ground into after being 4% sterile saline cleaning, drying with concentration by bletilla striata stem tuber, adds sterile steaming
Distilled water simultaneously makes it submerge coarse powder, and the closed 24h that swells is carried out at 45 DEG C, filters moisture content, obtains expanding coarse powder；
S2：The coarse powder of expansion and 88% ethanol are pressed 1:8 ratio mixing, regulation pH of mixed are 5.5, are added suitable
In the middle warm type or thermal-stable α-amylase of mixed liquor mass fraction 0.1%, refluxing extraction 3 times, micro- under microwave heating condition
Wave frequency rate control is 450W, extracts 10min every time, while by controlling microwave irradiation amount by heating and temperature control at 92 DEG C, is closed
And extract solution, the pH value of extract solution is adjusted to 6.5, and temperature control is 35 DEG C, and extract solution is passed through into decolorization and impurity removal by active carbon, filtering
Obtain a destainer；
S3：Extract solution in step S2 is filtered, by filtrate be put into centrifuge and under 600r/min rotating speed from
The heart separates, and is crystallized after vacuum-concentrcted, and solid-to-liquid ratio is 1 in crystallization process:5 (W/V), crystal are washed crystalline substance to brown color and obtained slightly
Crystalline substance, coarse-grain add the distilled water dissolving of 3 times of amounts, recycle the petroleum ether of 6 times of amounts to extract repeatedly 3 times, by extract again by work
Property carbon decoloring removal of impurities, be filtrated to get secondary decolourization liquid, gained secondary decolourization liquid is placed in 60 Rotary Evaporators, under 0.9MPa
Concentration volume dries 3h under conditions of being 75 DEG C in temperature, 99.60% bletilla striata alcohol is made to 5%.
Embodiment 2
A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata, comprises the following steps：
S1：Coarse powder is ground into after being 5% sterile saline cleaning, drying with concentration by bletilla striata stem tuber, adds sterile steaming
Distilled water simultaneously makes it submerge coarse powder, and the closed 28h that swells is carried out at 48 DEG C, filters moisture content, obtains expanding coarse powder；
S2：The coarse powder of expansion and 90% ethanol are pressed 1:10 ratio mixing, regulation pH of mixed are 6, are added suitable
In the middle warm type or thermal-stable α-amylase of mixed liquor mass fraction 0.1%, refluxing extraction 3 times, micro- under microwave heating condition
Wave frequency rate control is 500W, extracts 12min every time, while by controlling microwave irradiation amount by heating and temperature control at 93 DEG C, is closed
And extract solution, the pH value of extract solution is adjusted to 6.8, and temperature control is 40 DEG C, and extract solution is passed through into decolorization and impurity removal by active carbon, filtering
Obtain a destainer；
S3：Extract solution in step S2 is filtered, by filtrate be put into centrifuge and under 600r/min rotating speed from
The heart separates, and is crystallized after vacuum-concentrcted, and solid-to-liquid ratio is 1 in crystallization process:6 (W/V), crystal are washed crystalline substance to brown color and obtained slightly
Crystalline substance, coarse-grain add the distilled water dissolving of 4 times of amounts, recycle the petroleum ether of 7 times of amounts to extract repeatedly 3 times, by extract again by work
Property carbon decoloring removal of impurities, be filtrated to get secondary decolourization liquid, gained secondary decolourization liquid is placed in 62 Rotary Evaporators, dense under 1MPa
Contracting volume dries 4h under conditions of being 77 DEG C in temperature, 99.25% bletilla striata alcohol is made to 6%.
Embodiment 3
A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata, comprises the following steps：
S1：Coarse powder is ground into after being 5.5% sterile saline cleaning, drying with concentration by bletilla striata stem tuber, is added sterile
Distilled water simultaneously makes it submerge coarse powder, and the closed 32h that swells is carried out at 50 DEG C, filters moisture content, obtains expanding coarse powder；
S2：The coarse powder of expansion and 95% ethanol are pressed 1:12 ratio mixing, regulation pH of mixed are 6.5, add phase
When in the middle warm type or thermal-stable α-amylase of mixed liquor mass fraction 0.1%, refluxing extraction 3 times under microwave heating condition,
Microwave frequency control is 550W, extracts 15min every time, while by controlling microwave irradiation amount by heating and temperature control at 95 DEG C,
Merge extract solution, adjust the pH value of extract solution to 7, temperature control is 45 DEG C, and extract solution is passed through into decolorization and impurity removal by active carbon, filtering
Obtain a destainer；
S3：Extract solution in step S2 is filtered, by filtrate be put into centrifuge and under 600r/min rotating speed from
The heart separates, and is crystallized after vacuum-concentrcted, and solid-to-liquid ratio is 1 in crystallization process:7 (W/V), crystal are washed crystalline substance to brown color and obtained slightly
Crystalline substance, coarse-grain add the distilled water dissolving of 5 times of amounts, recycle the petroleum ether of 8 times of amounts to extract repeatedly 3 times, by extract again by work
Property carbon decoloring removal of impurities, be filtrated to get secondary decolourization liquid, gained secondary decolourization liquid is placed in 65 Rotary Evaporators, under 1.1MPa
Concentration volume dries 5h under conditions of being 80 DEG C in temperature, 99.48% bletilla striata alcohol is made to 8%.
The bletilla striata alcohol prepared by 1-3 of the embodiment of the present invention, its purity respectively reaches 99.60%, 99.25%,
99.48%, purity is higher.Preferably to verify feature of the bletilla striata alcohol of the method preparation of the present invention as qualitative and quantitative, take
Concentration but undried bletilla striata alcohol prepared by embodiment 1-3 carry out the test of index of refraction using abbe's refractometer, while with open
Embodiment 1-3 in patent CN104997701A " oral care product with anti-helicobacter pylori of the alcohol extracting thing containing the bletilla striata "
Bletilla striata alcohol condensed cream prepared by bletilla striata alcohol preparation method as a comparison case, according under identical conditions equivalent extract solution be concentrated into
The condition of equivalent volumes fraction is carried out, the index of refraction of the bletilla striata alcohol after test concentration, while tests its viscosity, as a result such as following table institute
Show.
Index of refraction and viscosity are to weigh the important physical constant of organic compound, can reflect the pure of organic compound
Degree, is drawn, the bletilla striata alcohol index of refraction and ratio of viscosities prior art prepared by embodiments of the invention have by above-mentioned test data
Obvious raising, can meet the requirement as qualitative quantitative control product.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations, for person of an ordinary skill in the technical field, is not departing from
On the premise of present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention by being submitted
Claims determine scope of patent protection.
Claims (10)
- A kind of 1. method of the extraction purification bletilla striata alcohol from the bletilla striata, it is characterised in that comprise the following steps：S1：By bletilla striata stem tuber with coarse powder is ground into after sterile saline cleaning, drying, sterile distilled water is added at 45-50 DEG C Lower progress is closed to swell, and filters moisture content, obtains expanding coarse powder；S2：The coarse powder of expansion is mixed with 88-95% ethanol, regulation pH of mixed is 5.5-6.5, adds alpha-amylase, Refluxing extraction 3 times under microwave heating condition, microwave frequency control is 450-550W, merges extract solution, adjusts the pH value of extract solution To 6.5-7, temperature control is 35-45 DEG C, by extract solution by decolorization and impurity removal by active carbon, is filtrated to get a destainer；S3：Destainer in step S2 is filtered, centrifuged, is crystallized after vacuum-concentrcted, solid-to-liquid ratio is in crystallization process 1:5-7 (W/V), crystal wash crystalline substance to brown color and obtain coarse-grain, and coarse-grain adds the 3-5 times of distilled water measured dissolving, what 6-8 times of recycling was measured Petroleum ether extracts 3 times repeatedly, by extract again by decolorization and impurity removal by active carbon, is filtrated to get secondary decolourization liquid, gained is secondary Destainer is placed in 60-65 Rotary Evaporators, and concentration volume is dried to 5-8%, bletilla striata alcohol is made under 0.9-1.1MPa.
- 2. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S1, institute It is 4-5.5% to state sterile saline concentration.
- 3. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S1, institute State the closed when a length of 24-32h to swell.
- 4. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S1, institute Coarse powder should can be submerged by stating the addition of sterile distilled water.
- 5. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S2, institute The ratio for stating coarse powder and 88-95% ethanol mixing is 1:8-12.
- 6. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S2, institute It is middle warm type amylase or high temperature modification amylase to state alpha-amylase, and its addition is the 0.1% of mixed liquor mass fraction.
- 7. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S2, institute Stating the temperature of microwave heating should control at 92-95 DEG C.
- 8. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S2, institute A length of 10-15min when stating refluxing extraction extraction.
- 9. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S3, institute The rotating speed for stating centrifugation is 600r/min.
- 10. the method for the extraction purification bletilla striata alcohol according to claim 1 from the bletilla striata, it is characterised in that：In step S3, institute Dry temperature is stated as 75-80 DEG C, a length of 3-5h when drying.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711071368.7A CN107721927A (en) | 2017-11-03 | 2017-11-03 | A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711071368.7A CN107721927A (en) | 2017-11-03 | 2017-11-03 | A kind of method of the extraction purification bletilla striata alcohol from the bletilla striata |
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| CN107721927A true CN107721927A (en) | 2018-02-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111419765A (en) * | 2020-04-01 | 2020-07-17 | 广州今盛美精细化工有限公司 | Bletilla striata extract and application thereof in preparation of cosmetics |
| CN113304088A (en) * | 2021-05-26 | 2021-08-27 | 上海辉文生物技术股份有限公司 | Preparation method of bletilla striata extract with repairing and whitening effects and bletilla striata extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104997701A (en) * | 2015-08-17 | 2015-10-28 | 杭州华胄科技有限公司 | Oral care product containing bletilla striata alcohol extract and having anti-Hp (helicobacter pylori) efficacy |
-
2017
- 2017-11-03 CN CN201711071368.7A patent/CN107721927A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104997701A (en) * | 2015-08-17 | 2015-10-28 | 杭州华胄科技有限公司 | Oral care product containing bletilla striata alcohol extract and having anti-Hp (helicobacter pylori) efficacy |
Non-Patent Citations (4)
| Title |
|---|
| CHEMICAL ABSTRACTS SERVICE (CAS): "DATABASE Registry", 《STNEXT[ONLINE]》 * |
| MASAE YAMAKI等: "THREE DIHYDROPHENANTHROPYRANS FROM BLETILLA STRIATA.", 《PHYTOCHEMISTRY》 * |
| REN，JIE等: "Two new phenanthrene glycosides from Liparis regnieri Finet and their antibacterial activities.", 《PHYTOCHEMISTRY LETTERS》 * |
| SHUZO TAKAGI等: "Antimicrobial agents from Bletilla striata.", 《PHYTOCHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111419765A (en) * | 2020-04-01 | 2020-07-17 | 广州今盛美精细化工有限公司 | Bletilla striata extract and application thereof in preparation of cosmetics |
| CN113304088A (en) * | 2021-05-26 | 2021-08-27 | 上海辉文生物技术股份有限公司 | Preparation method of bletilla striata extract with repairing and whitening effects and bletilla striata extract |
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