CN1410522A - Method of extracting essential oil and natural benzaldehyde from fruit skin and fruit pulp of garlic fruit - Google Patents
Method of extracting essential oil and natural benzaldehyde from fruit skin and fruit pulp of garlic fruit Download PDFInfo
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- CN1410522A CN1410522A CN 02139271 CN02139271A CN1410522A CN 1410522 A CN1410522 A CN 1410522A CN 02139271 CN02139271 CN 02139271 CN 02139271 A CN02139271 A CN 02139271A CN 1410522 A CN1410522 A CN 1410522A
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- malania oleifera
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- natural benzaldehyde
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Abstract
A process for extracting refined oil and natural benzaldehyde from the peel and pulp for oily malania includes such steps as steam-distilling to extract refined oil of oily malania, and refricting, separating and purifying the said refined oil to obtain natural benzaldehyde. Its advantages are abundant raw material source, high output rate, and low cost.
Description
Technical field
The invention belongs to method field from plant extract spices essential oil and natural benzaldehyde.
Background technology
Natural benzaldehyde has been widely used at food, beverage, tobacco industry, medicine industry, and traditional production method is to extract from Semen Armeniacae Amarum, and the natural benzaldehyde fragrance that this method is produced is good, but cost is very high, valuable product.For reducing production costs, the phenyl aldehyde of also useful in recent years Oleum Cinnamomi cracking production food grade, but the phenyl aldehyde of producing with this method is good not as the natural benzaldehyde that extracts from Semen Armeniacae Amarum aspect natural characteristic, has influenced its range of application.Therefore, new raw material that seek to produce natural benzaldehyde is one of focus of paying special attention to of spices circle.
Malania oleifera (Malania Oleifera Chun et Lee) popular name root or bark of Nepal Mallotus is xylophyta, and kalimeris wood belongs to, and Olacaceae is distributed in Guangxi and Yunnan Province.Its kind benevolence contains abundant Vegetable oil lipoprotein (being malania oleifera oil), patent application " a kind of method of producing thibetolide from malania oleifera oil " (application number 01132701.4) discloses a kind of method of utilizing malania oleifera kind benevolence, reach pericarp more than 55%, pulp as yet not by fine utilization but account for malania oleifera fruit total mass, more do not see the report that extracts spices essential oil and natural benzaldehyde from the fruit pulp of malania oleifera.
Summary of the invention
The technical problem to be solved in the present invention is the thick product that extracts the malania oleifera essential oil the pericarp, pulp from fresh malania oleifera or contain phenyl aldehyde, and and then rectifying separation purify and obtain the high-purity natural phenyl aldehyde.
The present invention solves the problems of the technologies described above with following technical scheme: extract the malania oleifera essential oil with steam distillation from the fruit pulp of fresh malania oleifera, vapor pressure is 0.05~0.5Mpa when extracting essential oil, distillation time 20 minutes~3 hours; Under normal pressure or decompression the malania oleifera essential oil is purified with the rectification method rectifying separation, obtain the high-purity natural phenyl aldehyde, when adopting rectification under vacuum, vacuum tightness is 1~760mmHg.
Also can adopt leaching of organic solvent room temperature or heating and refluxing extraction to the fruit pulp of fresh malania oleifera, again the oily matter rectifying of being rich in phenyl aldehyde that obtains be made highly purified natural benzaldehyde after the organic solvent in the extracting solution is reclaimed.Organic solvent can be single or blended ether, sherwood oil, ethyl acetate, benzene, toluene, methyl alcohol, ethanol, acetone, chloroform etc., and usage quantity is a solvent: the fruit pulp of fresh malania oleifera=0.05~10 (mass ratio).The time of room temperature leaching can be 10 minutes~24 hours, and the heating and refluxing extraction time can be 20 minutes~4 hours.
With fruit pulp extraction malania oleifera essential oil and the natural benzaldehyde of method of the present invention from malania oleifera, to compare with natural benzaldehyde with from Semen Armeniacae Amarum, extracting Semen Armeniacae Amarum oil, raw material sources are abundant, the extraction yield height, production cost is low.When using steam distillation to extract the spices essential oil, the essential oil oil yield surpasses 0.6%, and natural benzaldehyde content reaches (vapor-phase chromatography) more than 85% in the essential oil; When adopting organic solvent extraction (extraction), oily matter yield>0.9%, wherein phenyl aldehyde content>76% (vapor-phase chromatography).
Embodiment
No matter be to adopt steam distillation to extract the malania oleifera essential oil, or contain the oily matter of phenyl aldehyde with organic solvent extraction (extraction), the pericarp of raw material malania oleifera, pulp can directly be put into extraction equipment, also can put into extraction equipment after crushed, can also after squeezing the juice juice and slag separately be put into extraction equipment and extraction equipment respectively.When adopting steam distillation, the pressure-controlling of water vapour between 0.05~0.5Mpa, distillation time 20 minutes~3 hours, selection of process parameters is relevant with the raw material situation.After having extracted the malania oleifera essential oil, adopt normal pressure or rectification under vacuum method to carry out rectifying separation purification natural benzaldehyde to the malania oleifera essential oil.As adopting rectification under vacuum, vacuum degree control is between 1~760mmHg.
When adopting organic solvent extraction (extraction), can room temperature leach, also can heating and refluxing extraction, the former leaching time can be 10 minutes~24 hours, the latter's extraction time can be 20 minutes~4 hours.Under normal pressure or decompression, reclaim the oily matter that solvent obtains containing phenyl aldehyde, at last with normal pressure or rectification under vacuum method rectifying separation purification natural benzaldehyde.Organic solvent can be one or both and the above mixture in ether, sherwood oil, ethyl acetate, benzene, toluene, methyl alcohol, ethanol, acetone, the chloroform, and usage quantity is: solvent: the fruit pulp of fresh malania oleifera=0.05~10 (mass ratio).Situation when the concrete time of leaching or heating and refluxing extraction enters extraction with raw material is relevant.
Embodiment 1:
Put into the steam distillation still after the fruit pulp of the fresh malania oleifera of 2000 grams is pulverized, carried out steam distillation under the normal pressure 2 hours, the profit that steams left standstill 48 hours, profit was separated obtaining the flaxen essential oil of 14.6 grams then with separator.The essential oil yield is 14.6/2000=0.73%, and the phenyl aldehyde content of essential oil is 85.7% (vapor-phase chromatography).Adopt the rectification method rectifying separation to obtain the natural benzaldehyde of 11 grams 98% to the gained essential oil under the normal pressure.
Embodiment 2:
The fruit pulp of the fresh malania oleifera of 2000 grams is directly put into the steam distillation still, carries out steam distillation under the normal pressure 3 hours, and the profit that steams left standstill 48 hours, then oily water separation is obtained the flaxen essential oil of 12.4 grams.The essential oil yield is 12.4/2000=0.62%, and the phenyl aldehyde content of essential oil is 85.5% (vapor-phase chromatography).In vacuum tightness is under the 10mmHg, adopts rectification under vacuum method rectifying separation to obtain the natural benzaldehyde of 9.5 grams 98% to the gained essential oil.
Embodiment 3:
The fruit pulp of the fresh malania oleifera of 2000 grams is pulverized and is squeezed the juice, twice of 500ml extracted with diethyl ether of juice, slag is at room temperature with 8 hours twice of 1000ml ether leaching, combining extraction liquid and leaching liquid, the heating recovery ether, obtain green oily matter 18.2 grams, the oily matter yield is 18.2/2000=0.91%, and its phenyl aldehyde content is 76.2% (vapor-phase chromatography).Adopt the rectification method rectifying separation to obtain the natural benzaldehyde of 11.5 grams 98% to obtaining oily matter under the normal pressure.
Embodiment 4:
The fruit pulp of the fresh malania oleifera of 2000 grams is pulverized and is squeezed the juice, twice of 500ml extracted with diethyl ether of juice, 3 hours twice of 1000ml ether heating and refluxing extraction of slag, combining extraction liquid and extracting solution, the heating recovery ether, obtain green oily matter 18.5 grams, the oily matter yield is 18.5/2000=0.925%, its phenyl aldehyde content 76.2% (vapor-phase chromatography).Adopt the rectification method rectifying separation to obtain the natural benzaldehyde of 11.5 grams 98% to obtaining oily matter under the normal pressure.
Claims (3)
1, a kind of fruit pulp from malania oleifera extracts the method for essential oil, it is characterized in that extracting the malania oleifera essential oil with steam distillation from the fruit pulp of fresh malania oleifera, and the distillatory vapor pressure is 0.05~0.5Mpa, distillation time 20 minutes~3 hours.
2, a kind of pericarp from malania oleifera, pulp extract the method for natural benzaldehyde, it is characterized in that from the fruit pulp of malania oleifera, extracting the malania oleifera essential oil with steam distillation, the vapor pressure of steam distillation is 0.05~0.5Mpa, distillation time 20 minutes~3 hours, under normal pressure or decompression, obtaining malania oleifera essential oil rectifying separation is purified again, obtain the high-purity natural phenyl aldehyde.
3, a kind of method of extracting natural benzaldehyde from the fruit pulp of malania oleifera is characterized in that:
(1) with the natural benzaldehyde in the fruit pulp of leaching of organic solvent room temperature or heating and refluxing extraction malania oleifera, organic solvent can be single or blended ether, sherwood oil, ethyl acetate, benzene, toluene, methyl alcohol, ethanol, acetone, chloroform etc., and usage quantity is: solvent: the fruit pulp of fresh malania oleifera=0.05~10 (mass ratio); The time of room temperature leaching can be 10 minutes~24 hours; The time of heating and refluxing extraction can be 20 minutes~4 hours;
(2) heating recovery organic solvent under normal pressure or the decompression, the oily matter of natural benzaldehyde is rich in acquisition;
(3) purify with the method rectifying separation of normal pressure or rectification under vacuum and be rich in the oily matter of natural benzaldehyde, obtain the high-purity natural phenyl aldehyde.
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CN 02139271 CN1188381C (en) | 2002-11-09 | 2002-11-09 | Method of extracting essential oil and natural benzaldehyde from fruit skin and fruit pulp of garlic fruit |
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CN 02139271 CN1188381C (en) | 2002-11-09 | 2002-11-09 | Method of extracting essential oil and natural benzaldehyde from fruit skin and fruit pulp of garlic fruit |
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CN1410522A true CN1410522A (en) | 2003-04-16 |
CN1188381C CN1188381C (en) | 2005-02-09 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102174095A (en) * | 2011-01-24 | 2011-09-07 | 昆明理工大学 | Malania oleifera lectin and method for preparing same |
CN109991359A (en) * | 2018-01-02 | 2019-07-09 | 苏州玉森新药开发有限公司 | A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions |
CN110331043A (en) * | 2019-07-31 | 2019-10-15 | 云南天宏香精有限公司 | A kind of mouth containing flavouring essence for tobacco and its preparation method and application |
CN114410379A (en) * | 2021-12-17 | 2022-04-29 | 太仓市宝马油脂设备有限公司 | Preparation process of low-temperature cold-pressed original-fragrance garlic fruit oil |
-
2002
- 2002-11-09 CN CN 02139271 patent/CN1188381C/en not_active Expired - Fee Related
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102174095A (en) * | 2011-01-24 | 2011-09-07 | 昆明理工大学 | Malania oleifera lectin and method for preparing same |
CN102174095B (en) * | 2011-01-24 | 2013-07-31 | 昆明理工大学 | Malania oleifera lectin and method for preparing same |
CN109991359A (en) * | 2018-01-02 | 2019-07-09 | 苏州玉森新药开发有限公司 | A kind of method of quality control of the Chinese medicine composition with cough-suppressing phlegm-dispelling functions |
CN109991359B (en) * | 2018-01-02 | 2021-07-13 | 苏州玉森新药开发有限公司 | Quality control method of Chinese medicinal composition with cough relieving and phlegm eliminating effects |
CN110331043A (en) * | 2019-07-31 | 2019-10-15 | 云南天宏香精有限公司 | A kind of mouth containing flavouring essence for tobacco and its preparation method and application |
CN114410379A (en) * | 2021-12-17 | 2022-04-29 | 太仓市宝马油脂设备有限公司 | Preparation process of low-temperature cold-pressed original-fragrance garlic fruit oil |
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CN1188381C (en) | 2005-02-09 |
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