CN1762956A - Supercritical column chromatography method for preparing general gingerol - Google Patents
Supercritical column chromatography method for preparing general gingerol Download PDFInfo
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- CN1762956A CN1762956A CNA200510018040XA CN200510018040A CN1762956A CN 1762956 A CN1762956 A CN 1762956A CN A200510018040X A CNA200510018040X A CN A200510018040XA CN 200510018040 A CN200510018040 A CN 200510018040A CN 1762956 A CN1762956 A CN 1762956A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The present invention discloses supercritical chromatographic separation process of preparing total gingerol, and features that total gingerol is prepared with ginger as material and through cleaning, slicing into thin chip, fast heliophobic stoving at low temperature, crushing, supercritical extraction, molecular distillation to eliminate water, and chromatographic separation.
Description
Affiliated technical field:
The present invention relates to a kind of preparation method of general gingerol, a kind of supercritical column chromatography of saying so more specifically prepares the method for general gingerol.
Background technology:
The art of this patent comes from country's 15 programs for tackling key problems in science and technology " original new drug and the modernization of Chinese medicine " special project: Chinese medical extract and quality standard research, its minute project name be called " Chinese medicine Rhizoma Zingiberis Recens extract and quality standard research ".One of problem target is by systematic study, to adapt to production of numerous domestic Chinese patent medicine and international market demand is prerequisite, set up the gingerol content production technique that is applicable to oral stdn Rhizoma Zingiberis Recens extract up to standard, foundation can be controlled the technical parameter and the index of each relevant link of production technique easy, effectively.
At present, known supercritical preparation process extracts ginger oil (resin) or other Chinese medicine essential oil, or other vegetables oil, and what go out by retrieval has:
Open (bulletin) number 1344788 open (bulletins) day 2002.04.17 applies for (patent) number 01135914.5
Open (bulletin) number 1346877 open (bulletins) day 2002.05.01 applies for (patent) number 01113910.2
Disclosed supercritical extraction content is all fine in known technology, and is also more comprehensive.In order to make prior art that good expansion and extension be arranged, the invention provides a kind of by ginger be raw material through clean, shave, the flash baking of lucifuge low temperature, pulverizing, supercritical extraction, molecular distillation dewaters, column chromatography for separation prepares general gingerol comparatively accurately proper preparation method.
Summary of the invention:
The present invention gets ginger to clean shave, through the flash baking of baking box lucifuge low temperature, pulverizes, and crosses 20～80 mesh sieves, preparation supercritical extraction material; The present invention has effectively stoped gingerol to meet light, has met hot decomposition.
The present invention is to be raw material with ginger through the ginger powder of special processes such as shave, low-temperature dark flash baking, pulverizing preparations, extracts through supercritical extraction technique, and purifies through the molecular distillation technique dehydration, directly obtains smart ginger oil.The smart ginger oil clear of the present invention's preparation, of light color, relative density is little, gingerol content height.
The present invention is that the smart ginger oil that obtains with present technique is a raw material, add proper silica gel H and mix sample, put into then with pack into the upper end of chromatography column of silica gel H of dry method, add a cover absorbent cotton, use benzene: ethyl acetate: sherwood oil (5: 3: 2) wash-out, thin layer detects, and collects the general gingerol fraction, and the reclaim under reduced pressure eluent promptly gets general gingerol.
Technical scheme:
The technical scheme that technical solution problem of the present invention is adopted is: get ginger and clean, go into the flash baking of 40～80 ℃ of lucifuge low temperature of conventional oven behind the shave; Get the ginger splices of oven dry and pulverize, cross 20～80 mesh sieves, in the supercritical extraction axe of packing into, carry out supercritical extraction and parsing by table 1 parameter, the extraction time is 3～6 hours, and carries out the molecular distillation purification that dewaters by table 2 parameter, reach the purpose that obtains smart ginger oil, it is 3～5% that smart ginger oil is collected rate; Get smart ginger oil and add proper silica gel H and mix sample, put into, add a cover absorbent cotton with pack into the upper end of chromatography column of silica gel H of dry method, use benzene: ethyl acetate: sherwood oil (5: 3: 2) wash-out, thin layer detects, and collects the general gingerol fraction, and the reclaim under reduced pressure eluent promptly gets general gingerol.
Table 1 extraction desorption parameter
| Pressure (MPa) | Temperature ℃ | CO2 flow (kg/h*kg) | |
| The extraction axe | 30～15 | 60～30 | 20～10 |
| Resolve axe | 16～4 | 65～35 |
Table 2 molecular distillation parameter
| Vacuum tightness (MPa) | Heating temperature ℃ | Cooling temperature ℃ |
| 0.08～G.07 | 60～80 | 20～15 |
Beneficial effect:
Ginger of the present invention is cleaned technology, can make harmful element (as: lead, arsenic, copper, chromium etc.) and the pesticide residue brought into because of clay in smart ginger oil of intermediates supercritical extract and the finished product general gingerol reduce to minimum.Ginger shave lucifuge low temperature rapid drying technology of the present invention can effectively stop gingerol chance light in the ginger drying process, meet hot decomposition; The dried ginger slice that this technology obtains pulverizes after supercritical extraction, and degreasing purifies and just can directly obtain smart ginger oil again, the smart ginger oil clear of acquisition, and of light color, relative density is little, gingerol content height; The traditional technology ginger is by the Jiang Nong monoblock or cut sheet and dry naturally, decompose because of gingerol in the drying process is a large amount of rotten, through the ginger oil thickness that supercritical extraction obtains, color depth, relative density is big, therefore is oleoresin ginger, needs the further degreasing smart ginger oil of back acquisition of refining.This process for super-critical extracting is compared with other Rhizoma Zingiberis Recens extract extraction process with the molecular distillation dewatering process, and this technology has been avoided high temperature and oxidation, has prevented the decomposition of leaching process gingerol, and extraction effect is good, general gingerol retention rate height; And steam distillation ginger oil yield is low, and gingerol content is low in the ginger oil, and ginger oil ginger characteristic perfume is poor; The gingerol retention rate is lower in the ginger ethanol extraction, and composition is more more assorted in the extract, and extract is the thick paste shape.Column chromatography for separation technology of the present invention, easy, quick, a step obtains the high purity general gingerol.
Embodiment and step:
Embodiments of the present invention and step are: get ginger 100kg, clean, be cut into the thick thin ginger splices of about 1mm, put conventional oven (or barn) immediately into, temperature is established to 40 ℃～80 ℃ oven dry, and drying course is answered lucifuge; Dried ginger slice after the oven dry enters masher and grinds the back and cross 20 orders～80 mesh sieves, and the residue sheet returns mill again, and sieve fine powder is down packed into and extracted extracting pressure 30MPa～15MPa, 60 ℃～30 ℃ of extraction temperature, CO in the extraction axe
2Flow 20kg/h*kg～10kg/h*kg, 3～6 hours continuous extraction time; Resolve axe pressure 16MPa～4MPa, between 65 ℃～35 ℃ of the resolution temperatures, heat separating funnel, make moisture and CO in the separating funnel with 60 ℃～80 ℃ hot water
2Emulsification shape essential oil dissolve and be liquid, stopped to heat bleed then 30～40 minutes, bleed off following moisture, then product oil is put in the clean container, transport the molecular distillation chamber to and carry out molecular distillation and dewater and obtain smart ginger oil; Molecular still vacuum tightness MPa 0.08～0.07Mpa, 60 ℃～80 ℃ of Heating temperatures, 20 ℃～15 ℃ of cooling temperatures, smart ginger oil yield is 3～5%.Get ginger oil 0.5kg, silica gel H (thin layer is used) 1.5kg, it is standby to mix sample; Cut-off footpath 37 * 32cm chromatography column, add silica gel H 10kg, add in the post, press evenly, with the sample of the mixing capital of packing into, compress, add a cover absorbent cotton, use benzene then: ethyl acetate: sherwood oil (5: 3: 2) wash-out, after thin layer detects, collect the general gingerol fraction, decompression 760mmHg reclaims eluent, promptly gets general gingerol.
Embodiment one
Get ginger 100kg, clean, be cut into the thick thin ginger splices of 1mm, put conventional oven (barn) immediately into, temperature is established to 60 ℃ of oven dry, drying course lucifuge; Dried ginger slice after the oven dry enters crosses 40 mesh sieves after masher grinds, and the residue sheet returns mill again, receives ginger powder 10.8kg, ginger powder yield 10.8%.
Embodiment two
Got the undersized ginger powder 10.8kg of 40 mesh sieves pack into the extraction axe in, extracting pressure is controlled at 20MPa, extraction temperature is controlled at 40 ℃, CO
2Flow control is at 12kg/h*kg, continuous extraction 4 hours; Resolve the axe pressure-controlling at 5Mpa, resolution temperature is controlled at 35 ℃; Molecular still vacuum tightness 0.08Mpa, 70 ℃ of Heating temperatures, 18 ℃ of cooling temperatures, product gets ginger oil 0.58kg through separating funnel heating bleed, and the ginger oil yield is 5.37%.
Embodiment three
Transport the ginger oil that extracts to the molecular distillation chamber and carry out molecular distillation and dewater, the molecular still vacuum degree control is at 0.08MPa, and heating and temperature control is at 70 ℃, and cooling temperature is controlled at 18 ℃, obtains smart ginger oil 0.51kg, and smart ginger oil yield is 4.72%.
Embodiment four
Get ginger oil 0.5kg, silica gel H (thin layer is used) 1.5kg, it is standby to mix sample.
Embodiment five
Cut-off footpath 37 * 32cm chromatography column adds silica gel H 10kg, adds in the post, presses evenly, with the sample of the mixing capital of packing into, compresses, and adds a cover absorbent cotton, uses benzene then: ethyl acetate: sherwood oil (5: 3: 2) wash-out, and applied sample amount is 1: 10 with the ratio of elution amount; Thin layer is collected general gingerol fraction 5000ml after detecting, and decompression 760mmHg reclaims eluent, promptly gets the 300g general gingerol, general gingerol recovery rate 60%.
Claims (8)
1. a supercritical column chromatography prepares the method for general gingerol, is raw material through cleaning, shave, the flash baking of lucifuge low temperature, being ground into fine powder, supercritical extraction, molecular distillation dewaters, column chromatography for separation prepares general gingerol comparatively accurately proper preparation method by ginger promptly; It is characterized in that: get ginger and clean, be cut into thin ginger splices, put conventional oven (or barn) immediately into, temperature is established to 40～80 ℃ of oven dry, and drying course is answered lucifuge; Dried ginger slice after the oven dry enters masher and grinds the back and cross 20～80 mesh sieves, and sieve fine powder is down packed into and extracted extracting pressure 30MPa～15MPa, 60 ℃～30 ℃ of extraction temperature, CO in the extraction axe
2Flow 20kg/h*kg～10kg/h*kg, 3～6 hours continuous extraction time; Resolve axe pressure 16MPa～4MPa, between 65 ℃～35 ℃ of the resolution temperatures; Molecular still vacuum tightness MPa 0.08～0.07Mpa, 60 ℃～80 ℃ of Heating temperatures, 20 ℃～15 ℃ of cooling temperatures; Smart ginger oil yield is 3～5%; Getting smart ginger oil adds proper silica gel H (thin layer with) to mix sample standby; Get the chromatography column dry method silica gel H of packing into,, add a cover absorbent cotton, use benzene, ethyl acetate, sherwood oil then the sample of the mixing capital of packing into, the elutriant wash-out that suitable proportion is made into, thin layer is collected the general gingerol fraction after detecting, and the reclaim under reduced pressure eluent promptly gets general gingerol.
2. a kind of supercritical column chromatography according to claim 1 prepares the method for general gingerol, it is characterized in that: get ginger 100kg, put conventional oven or barn into after cleaning, thinly slicing, temperature is established to 40～80 ℃ of air blast oven dry, and drying course is answered lucifuge.
3. a kind of supercritical column chromatography according to claim 1 prepares the method for general gingerol, it is characterized in that: the dried ginger slice after the oven dry enters crosses 20～80 mesh sieves after masher grinds, and the residue sheet returns mill again, and fine powder is standby down for sieve.
4. a kind of supercritical column chromatography according to claim 1 prepares the method for general gingerol, it is characterized in that: fine powder is packaged under the sieve goes into to extract in the axe, and extracting pressure is controlled at 30MPa～15MPa, and extraction temperature is controlled at 60 ℃～30 ℃, CO
2Flow control is at 20kg/h*kg～10kg/h*kg, 3～6 hours continuous extraction time.
5. a kind of supercritical column chromatography according to claim 1 prepares the method for general gingerol, it is characterized in that: resolve axe pressure 16MPa～4MPa, between 65 ℃～35 ℃ of the resolution temperatures; Hot water heating separating funnel with 60 ℃～80 ℃ makes moisture and CO in the separating funnel
2Emulsification shape essential oil dissolve and be liquid, stopped to heat bleed then 30～40 minutes, bleed off following moisture, then product oil is put in the clean container, transport the molecular distillation chamber to and carry out molecular distillation and dewater and obtain smart ginger oil.
6. a kind of overcritical post layer watchman's clapper according to claim 1 prepares the method for general gingerol, it is characterized in that: molecular still vacuum tightness 0.08MPa～0.07Mpa, and 60 ℃～80 ℃ of Heating temperatures, 20 ℃～15 ℃ of cooling temperatures, smart ginger oil yield is 3～5%.
7. a kind of overcritical post layer watchman's clapper according to claim 1 prepares the method for general gingerol, it is characterized in that: get smart ginger oil 0.5kg and add silica gel H (thin layer is used) 1.5kg, it is standby to mix sample.
8. a kind of supercritical column chromatography according to claim 1 prepares the method for general gingerol, it is characterized in that: get 37 * 32cm chromatography column, add silica gel H 10kg, add in the post, press evenly, with the sample of the mixing capital of packing into, compress, add a cover absorbent cotton, use benzene, ethyl acetate, sherwood oil (5: 3: 2) ratio to be made into the elutriant wash-out then, applied sample amount is 1: 10 with the ratio of elution amount, thin layer is collected general gingerol fraction 5000ml after detecting, and decompression 760mmHg reclaims eluent, promptly get general gingerol 300g, general gingerol recovery rate 60%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994997B (en) * | 2006-12-27 | 2010-04-07 | 中国药科大学 | Method for separating and purifying 6-gingerol |
| CN102604742A (en) * | 2012-03-26 | 2012-07-25 | 河南中烟工业有限责任公司 | Perfume essential oil for tobacco and preparation method and application thereof |
| CN101530607B (en) * | 2009-04-13 | 2013-11-20 | 金华职业技术学院 | Method for extracting gingerol type material from ginger with high efficiency |
| CN108740332A (en) * | 2018-05-29 | 2018-11-06 | 华南农业大学 | A kind of folium eucalypti polyphenol feed addictive and preparation method thereof improving meat quality |
| CN108740331A (en) * | 2018-05-29 | 2018-11-06 | 华南农业大学 | A kind of folium eucalypti polyphenol feed addictive and preparation method thereof improving fish body meat |
| CN112138131A (en) * | 2020-10-11 | 2020-12-29 | 成都克洛玛生物科技有限公司 | Preparation method and application of total gingerol external preparation |
| CN115947652A (en) * | 2022-12-30 | 2023-04-11 | 无锡江大百泰科技有限公司 | Method for extracting 6-gingerol from ginger |
-
2005
- 2005-09-26 CN CNA200510018040XA patent/CN1762956A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994997B (en) * | 2006-12-27 | 2010-04-07 | 中国药科大学 | Method for separating and purifying 6-gingerol |
| CN101530607B (en) * | 2009-04-13 | 2013-11-20 | 金华职业技术学院 | Method for extracting gingerol type material from ginger with high efficiency |
| CN102604742A (en) * | 2012-03-26 | 2012-07-25 | 河南中烟工业有限责任公司 | Perfume essential oil for tobacco and preparation method and application thereof |
| CN108740332A (en) * | 2018-05-29 | 2018-11-06 | 华南农业大学 | A kind of folium eucalypti polyphenol feed addictive and preparation method thereof improving meat quality |
| CN108740331A (en) * | 2018-05-29 | 2018-11-06 | 华南农业大学 | A kind of folium eucalypti polyphenol feed addictive and preparation method thereof improving fish body meat |
| CN108740331B (en) * | 2018-05-29 | 2022-06-21 | 华南农业大学 | Eucalyptus leaf polyphenol feed additive for improving fish meat quality and preparation method thereof |
| CN112138131A (en) * | 2020-10-11 | 2020-12-29 | 成都克洛玛生物科技有限公司 | Preparation method and application of total gingerol external preparation |
| CN115947652A (en) * | 2022-12-30 | 2023-04-11 | 无锡江大百泰科技有限公司 | Method for extracting 6-gingerol from ginger |
| CN115947652B (en) * | 2022-12-30 | 2024-05-10 | 无锡江大百泰科技有限公司 | Method for extracting 6-gingerol from ginger |
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