CN101407743A - Method for extracting and separating curcuma oil - Google Patents
Method for extracting and separating curcuma oil Download PDFInfo
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- CN101407743A CN101407743A CNA200810032183XA CN200810032183A CN101407743A CN 101407743 A CN101407743 A CN 101407743A CN A200810032183X A CNA200810032183X A CN A200810032183XA CN 200810032183 A CN200810032183 A CN 200810032183A CN 101407743 A CN101407743 A CN 101407743A
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Abstract
The invention relates to a method for extracting and separating turmeric oil, which comprises the step of extracting the turmeric oil from curcumas by using supercritical CO2, and is characterized in that the method also comprises the following steps: adopting first-step molecular distillation to separate curcumin and grease in the turmeric oil obtained by using the supercritical CO2 method; obtaining almost colorless turmeric essential oil under the conditions of operating pressure of 10 to 20Pa, distillation temperature of 70 to 90 DEG C, the rotation speed of a blade applicator of 200 to 300r/min and distillates of more than 75.0 percent. Adopting supercritical CO2 extraction and two-level molecular distillation, the method can effectively keep the natural ingredients of the turmeric oil, without bringing any pollution to the environment. In addition, the method also realizes the separation of oxygenous sesquiterpene from sesquiterpene in the turmeric oil, which can be used directly as raw materials in the fields such as the cosmetics, food and pharmacy where different amounts of the oxygenous sesquiterpene and the sesquiterpene are needed.
Description
Technical field
The present invention relates to the extraction separation of turmeric oil, particularly the two-stage molecular distillation separates the novel method that contains oxygen sesquiterpene and sesquiterpene in the turmeric oil.
Background technology
Turmeric is a kind of traditional medicinal material of medicine-food two-purpose, has the broken stasis of blood, promoting the circulation of qi, disappears long-pending and lenitive effect and anticancer, antiearly pregnancy, anticoagulation, anti-oxidant and physiologically active such as protect the liver.The main chemical compositions of turmeric is turmeric yellow and turmeric oil.Be mainly monoterpenes, sesquiterpenoids and derivative thereof in the turmeric oil, reach materials such as pressing olein as turmerone, dehydroturmerone, phellandrene, limonene, camphor, Curgerenone, Curcumenol, curdione, curcuma zedoary enol, curcumene, zingiberene.Modern pharmacology studies show that, that turmeric oil has is anticancer, anti-mutation, eliminate the phlegm, ease pain, effect such as hemostasis, anti-inflammatory.
Contain the main chemical compositions that oxygen sesquiterpene and sesquiterpene are turmeric oils, containing the oxygen sesquiterpene gives off a strong fragrance, it is fragrant composition of being of turmeric oil, be the main component that turmeric oil is pharmacologically active simultaneously, contain the effective constituent that the oxygen sesquiterpene all is a cholagogic as the turmerone in the turmeric oil, aryl turmerone etc., so contain the oxygen sesquiterpene and sesquiterpene is the important source material of makeup, food and medicine industry.
Molecular distillation technique is a kind ofly to utilize the difference of each component differing molecular motion mean free path of mixture and carry out isolating novel liquid-liquid separation technology, is widely used in perfume industry.Supercritical CO
2The principle of fluid extraction (SFE) sepn process is to utilize the dissolving power of supercutical fluid and the relation of its density, promptly utilizes pressure and temperature that the influence of supercutical fluid dissolving power is carried out.Under supercritical state, supercutical fluid is contacted with material to be separated, it is extracted the composition of polarity size, boiling point height and molecular weight size selectively successively.Certainly, the resulting extract of corresponding each pressure range can not be single, but the mixing element that can control condition obtains optimum proportion, method by decompression, intensification makes supercutical fluid become common gases then, being extracted material then separates out fully or substantially, separate the purpose of purifying thereby reach, so supercritical CO
2The fluid extraction process is combined by extraction and sepn process.
(fine chemistry industry, 2006,23 (6): 553-557) utilize supercritical CO such as Han Rongwei
2Abstraction technique and molecular distillation technique separation and purification Flos Rosae Rugosae quintessence oil, the massfraction that is fragrant composition Ester surpasses 50%; (fine chemistry industry, 2008,25 (1): 48-53) adopt supercritical CO such as Zhang Jun
2Abstraction technique separates the purification Flos Lonicerae volatile oil with molecular distillation technique, the massfraction that is fragrant composition surpasses 40%; (Chinese Journal of Pharmaceuticals, 2003,34 (3): 125-127) utilize supercritical CO such as Wang Fasong
2Abstraction technique and molecular distillation technique have been studied the separation and purification of gingerol class and terpene component in the Rhizoma Zingiberis oil.
Turmeric oil is used steam distillation (Zhang Liankui etc. usually, CN87101355A) or solvent method extract, generally obtain as extracting a kind of by product in the turmeric yellow technology, (Chinese oil such as Liu Shuxing, 2004,29 (4): 18-20) and (Chinese medicinal materials, 1997 such as Ge Fahuan, 20 (7): 345-350) utilize supercritical methanol technology to extract turmeric oil, do not contain separating of oxygen sesquiterpene and sesquiterpene in the turmeric oil but all relate to.
Summary of the invention
The turmeric oil extraction and separation method that the purpose of this invention is to provide a kind of good separating effect.Simultaneously, the present invention also will provide a kind of new turmeric oil extract, has realized that the oxygen sesquiterpene that contains in the turmeric oil separates with sesquiterpene.
A kind of extraction and separation method of turmeric oil comprises and uses supercritical CO
2From the turmeric raw material, extract turmeric oil, also comprise following steps: adopt the one-level molecular distillation to separate and use supercritical CO
2Turmeric yellow and grease in the turmeric oil that method obtains, when working pressure is 10-20Pa, distillation temperature is 70-90 ℃, the blade applicator rotating speed is 200-300r/min, steams the thing amount greater than 75.0%, obtains almost colourless turmeric essential oil.
According to embodiments of the invention, after the one-level molecular distillation, also adopt the secondary molecular distillation to separate the one-level molecular distillation and steam thing, when distillation temperature is 50 ℃, the blade applicator rotating speed is 250r/min, distillation pressure is 80-260Pa, steams to contain the oxygen sesquiterpene in the thing and sesquiterpene is respectively 20.6-30.8% and 53.1-59.1%, steams to contain the oxygen sesquiterpene in the excess and sesquiterpene is respectively 56.4-58.8% and 27.6-30.7%.
Have in the prior art openly though extract turmeric oil with supercritical process, the present invention proposes a preferred version.Use supercritical CO
2The condition of extracting turmeric oil from the turmeric raw material is: extracting pressure 30Mpa, 45 ℃ of extraction temperature, CO
2Flow 40L/h carries out the dynamic circulation extraction under the condition of extraction time 120min.
Before the further preferential extraction, the extraction kettle of earlier curcuma powder of pulverizing being packed into, at pressure 10Mpa, the state static state that temperature is 30 ℃ presets.
According to above-mentioned method, can obtain two kinds of new turmeric oil extracts.Contain oxygen sesquiterpene and sesquiterpene in a kind of extract and be respectively 20.6-30.8% and 53.1-59.1%; Contain oxygen sesquiterpene and sesquiterpene in another extract and be respectively 56.4-58.8% and 27.6-30.7%.
Like this under the purity condition contain the oxygen sesquiterpene or the sesquiterpene extract can be directly as makeup, food, medicine and other fields raw material.
The distinguishing feature of above-mentioned technology is to adopt the two-stage molecular distillation, has realized the refining of turmeric oil on the one hand, and the turmeric essential oil that obtains is become almost colourless by pale brown look, give off a strong fragrance, and has realized containing in the turmeric oil separating of oxygen sesquiterpene and sesquiterpene simultaneously.
One of above-mentioned process program distinguishing feature is that static state presets-dynamic circulation extraction combination extraction turmeric oil, has effectively improved the extraction yield of turmeric oil, and extraction yield is greater than 8.8%.
Adopt supercritical CO
2The extraction turmeric oil, adopt the refining turmeric essential oil that obtains of two-stage molecular distillation to become almost colourless then by original pale brown look, aromatic flavour, realized simultaneously containing the separating of oxygen sesquiterpene and sesquiterpene in the turmeric oil, the dissolvent residual, the extraction yield that overcome traditional extraction separation existence are not high, the extraction that the not high shortcoming of quality, above-mentioned technology relate to turmeric oil with separate environmental friendliness.
Description of drawings
The separation process scheme figure that contains oxygen sesquiterpene and sesquiterpene in Fig. 1 turmeric oil.
Embodiment
Embodiment 1
Take by weighing curcuma powder 100g, the barrel of packing into is put extraction kettle into, the pressurization that heats up, at pressure 10Mpa, the state static state that temperature is 30 ℃ presets 15min, then with the curcuma powder of static treatment at extracting pressure 30Mpa, 45 ℃ of extraction temperature, CO
2Flow 40L/h carries out the dynamic circulation extraction under the condition of extraction time 120min.The yield 8.9% of turmeric oil.The 40mL turmeric oil adds in the molecular still, at working pressure 10Pa, and 80 ℃ of distillation temperatures, 2 ℃ of condensing temperatures, feeding rate 3mL/min, 45 ℃ of feeding temperatures, the condition of blade applicator rotating speed 300r/min is carried out molecular distillation, and steaming the thing amount is 81.1%.The one-level molecular distillation steams thing and carries out the secondary molecular distillation, when distillation pressure is 260Pa, when 50 ℃ of distillation temperatures and blade applicator rotating speed are 250r/min, steam and contain the oxygen sesquiterpene in the thing and sesquiterpene is respectively 20.6% and 59.1%, steam and contain the oxygen sesquiterpene in the excess and sesquiterpene is respectively 56.4% and 30.7%.
Embodiment 2
Take by weighing curcuma powder 50g, the barrel of packing into is put extraction kettle into, the pressurization that heats up, at pressure 10Mpa, the state static state that temperature is 30 ℃ presets 15min, then with the curcuma powder of static treatment at extracting pressure 30Mpa, 45 ℃ of extraction temperature, CO
2Flow 40L/h carries out the dynamic circulation extraction under the condition of extraction time 120min.The yield 8.8% of turmeric oil.Supercritical CO
2The turmeric oil of extraction adds in the molecular still, at working pressure 15Pa, and 85 ℃ of distillation temperatures, 2 ℃ of condensing temperatures, feeding rate 3mL/min, 45 ℃ of feeding temperatures, the condition of blade applicator rotating speed 300r/min is carried out molecular distillation, and it is 78.0% that molecular distillation steams thing.The one-level molecular distillation steams thing and carries out the secondary molecular distillation, when distillation pressure is 80Pa, when 50 ℃ of distillation temperatures and blade applicator rotating speed are 250r/min, steam and contain the oxygen sesquiterpene in the thing and sesquiterpene is respectively 30.8% and 53.7%, steam and contain the oxygen sesquiterpene in the excess and sesquiterpene is respectively 58.8% and 28.4%.
Embodiment 3
Take by weighing curcuma powder 150g, the barrel of packing into is put extraction kettle into, the pressurization that heats up, at pressure 10Mpa, the state static state that temperature is 30 ℃ presets 15min, then with the curcuma powder of static treatment at extracting pressure 30Mpa, 45 ℃ of extraction temperature, CO
2Flow 40L/h carries out the dynamic circulation extraction under the condition of extraction time 120min.The yield 8.9% of turmeric oil.Supercritical CO
2The turmeric oil of extraction adds in the molecular still, at working pressure 20Pa, and 85 ℃ of distillation temperatures, 2 ℃ of condensing temperatures, feeding rate 3mL/min, 45 ℃ of feeding temperatures, the condition of blade applicator rotating speed 300r/min is carried out molecular distillation, and it is 75.0% that molecular distillation steams thing.The one-level molecular distillation steams thing and carries out the secondary molecular distillation, when distillation pressure is 160Pa, when 50 ℃ of distillation temperatures and blade applicator rotating speed are 250r/min, steam and contain the oxygen sesquiterpene in the thing and sesquiterpene is respectively 27.8% and 56.7%, steam and contain the oxygen sesquiterpene in the excess and sesquiterpene is respectively 57.1% and 30.4%.
Claims (9)
1, a kind of extraction and separation method of turmeric oil comprises and uses supercritical CO
2From the turmeric raw material, extract turmeric oil, it is characterized in that this method also comprises following steps: adopt the one-level molecular distillation to separate and use supercritical CO
2Turmeric yellow and grease in the turmeric oil that method obtains, when working pressure is 10-20Pa, distillation temperature is 70-90 ℃, the blade applicator rotating speed is 200-300r/min, steams the thing amount greater than 75.0%, obtains almost colourless turmeric essential oil.
2, the extraction and separation method of turmeric oil according to claim 1, it is characterized in that after the one-level molecular distillation, also adopt the secondary molecular distillation to separate the one-level molecular distillation and steam thing, when distillation temperature is 50 ℃, the blade applicator rotating speed is 250r/min, distillation pressure is 80-260Pa, steams to contain the oxygen sesquiterpene in the thing and sesquiterpene is respectively 20.6-30.8% and 53.1-59.1%, steams to contain the oxygen sesquiterpene in the excess and sesquiterpene is respectively 56.4-58.8% and 27.6-30.7%.
3, the extraction and separation method of turmeric oil according to claim 1 is characterized in that the said supercritical CO of using
2The condition of extracting turmeric oil from the turmeric raw material is: extracting pressure 30Mpa, 45 ℃ of extraction temperature, CO
2Flow 40L/h carries out the dynamic circulation extraction under the condition of extraction time 120min.
4, extraction and separation method according to claim 3, before it is characterized in that extracting, the extraction kettle of earlier curcuma powder of pulverizing being packed into, at pressure 10Mpa, the state static state that temperature is 30 ℃ presets.
5, a kind of extract wherein contains oxygen sesquiterpene and sesquiterpene and is respectively 20.6-30.8% and 53.1-59.1%.
6, extract according to claim 5 is characterized in that it is to obtain according to the method for claim 2.
7, a kind of extract wherein contains oxygen sesquiterpene and sesquiterpene and is respectively 56.4-58.8% and 27.6-30.7%.
8, extract according to claim 7 is characterized in that it is to obtain according to the method for claim 2.
9, the described extract of one of claim 5 to 8 is as the purposes of makeup, food, medicine and other fields raw material.
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| CN200810032183XA CN101407743B (en) | 2008-08-28 | 2008-08-28 | Method for extracting and separating curcuma oil |
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| CN200810032183XA CN101407743B (en) | 2008-08-28 | 2008-08-28 | Method for extracting and separating curcuma oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260592A (en) * | 2010-12-24 | 2011-11-30 | 陈国英 | Extraction method of ginger oil |
| CN103071117A (en) * | 2013-01-18 | 2013-05-01 | 四川汇丰生物科技有限公司 | Method for extracting curcuma oil and curcumine from rhizoma curcumae longae |
| CN103243007A (en) * | 2013-04-03 | 2013-08-14 | 邢海明 | Alcoholic beverage and preparation method of alcoholic beverage |
| CN103409241A (en) * | 2013-08-09 | 2013-11-27 | 丽江先锋食品开发有限公司 | Preparation method of herbal elsholtzia essential oil |
| CN110711190A (en) * | 2019-09-20 | 2020-01-21 | 广西科学院 | Terpenoid inhibitor for resisting fish diseases and preparation method and application thereof |
| CN113080249A (en) * | 2021-04-27 | 2021-07-09 | 贵州理工学院 | Application method of Zingiber corallinum Hance essential oil in preparing edible spray for prolonging shelf life of vegetables and fruits |
| CN114149393A (en) * | 2021-12-10 | 2022-03-08 | 海南碧凯药业有限公司 | Sesquiterpene compound and preparation method thereof |
-
2008
- 2008-08-28 CN CN200810032183XA patent/CN101407743B/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260592A (en) * | 2010-12-24 | 2011-11-30 | 陈国英 | Extraction method of ginger oil |
| CN103071117A (en) * | 2013-01-18 | 2013-05-01 | 四川汇丰生物科技有限公司 | Method for extracting curcuma oil and curcumine from rhizoma curcumae longae |
| CN103243007A (en) * | 2013-04-03 | 2013-08-14 | 邢海明 | Alcoholic beverage and preparation method of alcoholic beverage |
| CN103409241A (en) * | 2013-08-09 | 2013-11-27 | 丽江先锋食品开发有限公司 | Preparation method of herbal elsholtzia essential oil |
| CN103409241B (en) * | 2013-08-09 | 2015-09-16 | 丽江先锋食品开发有限公司 | A kind of preparation method of Elsholtzia cilita essential oil |
| CN110711190A (en) * | 2019-09-20 | 2020-01-21 | 广西科学院 | Terpenoid inhibitor for resisting fish diseases and preparation method and application thereof |
| CN110711190B (en) * | 2019-09-20 | 2023-08-25 | 广西科学院 | Terpenoid inhibitor for resisting fish diseases and preparation method and application thereof |
| CN113080249A (en) * | 2021-04-27 | 2021-07-09 | 贵州理工学院 | Application method of Zingiber corallinum Hance essential oil in preparing edible spray for prolonging shelf life of vegetables and fruits |
| CN114149393A (en) * | 2021-12-10 | 2022-03-08 | 海南碧凯药业有限公司 | Sesquiterpene compound and preparation method thereof |
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| CN101407743B (en) | 2011-04-20 |
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