CN101259247B - Method for continuously extracting various active ingredient in turmeric - Google Patents
Method for continuously extracting various active ingredient in turmeric Download PDFInfo
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- CN101259247B CN101259247B CN200810027604XA CN200810027604A CN101259247B CN 101259247 B CN101259247 B CN 101259247B CN 200810027604X A CN200810027604X A CN 200810027604XA CN 200810027604 A CN200810027604 A CN 200810027604A CN 101259247 B CN101259247 B CN 101259247B
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Abstract
The present invention relates to a method for continuously extracting the effective components of turmeric, which is the method for extracting the effective components with strong thermal sensitivity and easy degradation from the rhizome of the plant turmeric. The present invention discloses that supercritical carbon dioxide is used for extracting by a continuous depressurization analytic technology firstly; filtrate is processed for recovering entrainer and then for standing, which is filtered to obtain curcumin and filtrate; the filtrate is processed for molecular distillation to obtain turmeric essential oil and turmeric fatty oil. The method for continuously extracting the effective components of turmeric can be applied to continuous industrialized operation; various kinds of the effective components of the turmeric are extracted and separated from the turmeric, which has guaranteed quality, short production period, high yield, safe production and strictly controlled environment and sanitation.
Description
Technical field
The present invention relates to the extraction of effective ingredient in the plant Rhizoma Curcumae Longae rhizome.
Background technology
Rhizoma Curcumae Longae is a zingiberaceous plant Rhizoma Curcumae Longae rhizome, ground such as main product Sichuan, Fujian.Rhizoma Curcumae Longae has choleretic effect on pharmacology, there is contraction in the uterus, and hypotensive effect is arranged, and staphylococcus aureus is had antibacterial action preferably, and the various skin fungus is had different inhibitory action, and the Rhizoma Curcumae Longae decoct has analgesic activity, so the medical value of Rhizoma Curcumae Longae is very high.The Rhizoma Curcumae Longae rhizome contains volatile oil 4.0～6.0%, and the main component in the oil is a turmerone 58%, aryl turmerone, zingiberene 25%, phellandrene, Cedrene 1%, cineole 1%, Borneolum Syntheticum 0.5%; Yellow substance is a tart curcumin 1.8～5.4% etc., contains fatty oil 1.74～3.32% in addition.
At present, relevant turmeric effective ingredient extracts, European patent Ep0726074A1 takes alcohol extraction, 5% a small amount of supercritical carbon dioxide makes to obtain under the modifier extract of Rhizoma Curcumae Longae, the reuse supercritical carbon dioxide extraction, the method of the etoh solvent in the extract, but this method is only limited to extraction, does not relate to separation, the purification of turmeric effective ingredient and with an organic solvent can cause environmental pollution in a large number.Chinese patent 01107480.9 adopts supercritical carbon dioxide extraction, extract is after falling liquid film concentrates recovery ethanol, the crystallization that is placed with most of curcumin through room temperature is separated out, the curcumin paste that filters wetly enters the supercritical carbon dioxide extraction drying again, isolate volatile oil, through parsing, the dry curcumin powder that gets.This patent can and be separated volatile oil and curcumin powder to Rhizoma Curcumae Longae extraction, a kind ofly has very much the fatty oil of medical value really not separate but have in addition, and this is an one.It two is can be when the entrainer in resolving technology and extract and the carbon dioxide separation by this patented method, and a large amount of entrainers, carbon dioxide are gone to the space, workshop, contaminated environment and hidden danger is arranged.So it is feasible that this patented method goes to implement from experimental viewpoint, promptly be only limited to device and be the supercritical carbon dioxide extraction apparatus below 24 liters, fail to be applied to the big production of industry, other has the curcumin in the relevant Rhizoma Curcumae Longae, Rhizoma Curcumae Longae essential oil, Rhizoma Curcumae Longae fatty oil all is the easy degradation materials of temperature-sensitive, oxidation deactivation under light and normality, two above technical schemes all do not relate to the technical data record of this respect, obviously, similar variation has appearred in their extract and separator in manufacturing process, be subjected to influence qualitatively.
Summary of the invention.
The purpose of this invention is to provide the method that various effective ingredient extract continuously in a kind of Rhizoma Curcumae Longae, the extraction from Rhizoma Curcumae Longae of its energy industrialization continued operation is also isolated the different various turmeric effective ingredients of effect, quality assurance, produce the weak point same period, the recovery rate height, production safety, environmental health is strictly controlled.
Technical solution of the present invention is:
A, supercritical carbon dioxide extraction
1., the Rhizoma Curcumae Longae coarse powder places supercritical extraction reactor, keeps extracting pressure 30Mpa to 45Mpa, 30 ℃ to 60 ℃ of extraction temperature are used entrainer, the mass ratio of entrainer consumption and raw material inventory is 1: 1 to 6: 1, the extraction time is 4 hours;
2., adopting continuous decompressive analysis technology to keep resolving pressure is 6Mpa to 20Mpa, 40 ℃ to 60 ℃ of resolution temperatures carry out secondary and resolve, and obtain extracting I liquid under one-level is resolved, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide;
3., extraction I liquid chamber temperature lucifuge leaves standstill after 24 hours lucifuge and filters, the curcumin paste, reach filtrate;
4., the curcumin paste places supercritical extraction reactor to carry out the supercritical carbon dioxide drying, extracting pressure 20Mpa to 25Mpa, 30 ℃ to 40 ℃ of extraction temperature, dry 2 hours the curcumin crystallization;
B, with above filtering filtrate and extraction II liquid at vacuum 5Pa to 10Pa, carry out molecular distillation under the condition that temperature is 110 ℃ to 130 ℃, obtain Rhizoma Curcumae Longae essential oil and Rhizoma Curcumae Longae fatty oil.
More than of the present invention:
A, supercritical carbon dioxide extraction
1., the Rhizoma Curcumae Longae coarse powder places supercritical extraction reactor, keeps extracting pressure 30Mpa, 35 ℃ of extraction temperature are used entrainer, the mass ratio of entrainer consumption and raw material inventory is 6: 1, the extraction time is 4 hours;
2., to adopt continuous decompressive analysis technology to keep one-level to resolve pressure be 15Mpa, secondary is resolved pressure 6Mpa, 60 ℃ of resolution temperatures, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide;
3., extraction I liquid chamber temperature lucifuge leaves standstill after 24 hours lucifuge and filters, the curcumin paste, reach filtrate;
4., the curcumin paste places supercritical extraction reactor to carry out the supercritical carbon dioxide drying, extracting pressure 25Mpa, 35 ℃ of extraction temperature, dry 2 hours the curcumin crystallization;
B, with above filtering filtrate and extraction II liquid at vacuum 5Pa, carry out molecular distillation under the condition that temperature is 120 ℃, obtain Rhizoma Curcumae Longae essential oil and Rhizoma Curcumae Longae fatty oil.
Entrainer of the present invention is ethanol, methanol or acetone.
Continuous decompressive analysis technology of the present invention is to carry out twice parsing and increase the single raise resolver in secondary resolver outlet, secondary resolver structure and technological requirement condition are identical with the secondary resolver, the secondary resolver is kept conventional analysis condition to guarantee normally carrying out of extraction process, and the entrainer that contains solute and more carbon dioxide of wherein being resolved continues to flow to secondary resolver, make carbon dioxide separation be recycled to behind the extracting system again with entrainer continuously decompression emit.
Extract room temperature lucifuge of the present invention leaves standstill after 24 hours at the direct bag filter of crossing of lucifuge pipeline.
Present existing Rhizoma Curcumae Longae extractive technique mostly is solvent or vapor distillation and extracts.The former extracts curcumin, and because of with an organic solvent causing environmental pollution in a large number, the latter extracts Rhizoma Curcumae Longae volatile oil.The two can only extract the two one of turmeric effective ingredient, and extraction ratio is all very low, causes cost to improve the waste of Rhizoma Curcumae Longae resource.The only a few technology can obtain curcumin and turmeric oil two parts product simultaneously at present, but owing to parsing aspect technical limitations can't realize suitability for industrialized production and can't obtain Rhizoma Curcumae Longae fatty oil from Rhizoma Curcumae Longae.
By adopting supercritical carbon dioxide extraction and molecular distillation technology used in conjunction, adopt " continuous decompressive analysis technology " can get the different various turmeric effective ingredients of effect at above-mentioned shortcoming the present invention.This method can be applied to the big production of industry, oxidation deactivation and long problem of production cycle under decomposes, the photosynthesis have been solved in the traditional handicraft, the inventive method recovery rate height, the curcumin crystallization response rate 85%, Rhizoma Curcumae Longae essential oil yield 4.5%, Rhizoma Curcumae Longae fatty oil yield 5.2%, cost is low, fully utilized the Rhizoma Curcumae Longae resource, superior product quality.
" continuous decompressive analysis technology " of the present invention is such, adding entrainer in carbon dioxide is the common method of the following supercritical carbon dioxide extraction apparatus of domestic and international pilot-scale, but in industrialized unit, adopt organic solvent bigger difficulty to be arranged as entrainer.Mainly be because in resolution phase, that the pressure of carbon dioxide can not drop to is very low, and (industrially be generally 6.5～5.5MPa), carbon dioxide is generally bigger to the dissolubility of entrainer, under above-mentioned pressure it is also had suitable solvability.In addition, the solute of being resolved when the amount of the entrainer of resolving in resolver also extracts than routine is much more, and the solute that general extract will be resolved is 10% of a raw material weight, and uses above-mentioned technology, and the solute that resolve is 600% of a raw material weight.Emit as the entrainer decompression that will be dissolved with solute this moment,, must also can bleed off a large amount of carbon dioxide to reclaim, to regenerate entrainer and to obtain solute.According to the result of the test on 200L * 2 extraction equipments, take directly from extraction-container, to emit the method for entrainer, to emit the ethanol that 440-660 rises in 4 hours, the carbon dioxide that every still extraction is consumed is 5 times when not using entrainer.The carbon dioxide of emitting is in a large number being carried volatile entrainer secretly and is being spread in the workshop and also can cause potential safety hazard.
At above-mentioned phenomenon, we adopt " continuous decompressive analysis technology ", preferably resolve this problem.Promptly (operating pressure is that 6.5～5.5MPa) outlets increase the single raise resolver at the secondary resolver.The secondary resolver is kept conventional analysis condition to guarantee normally carrying out of extraction process, the entrainer that contains solute and more carbon dioxide of wherein being resolved then constantly flows to secondary resolver, through the conversion analysis condition, carbon dioxide is separated from entrainer to greatest extent and be recycled to extracting system after again with entrainer continuously decompression emit.This method reduces the volatilization of emission of carbon-dioxide and entrainer widely, the consumption of carbon dioxide only is 2/5 of direct blood pressure lowering discharging, the consumption of entrainer reduces more than one times, has saved a large amount of carbon dioxide and ethanol, has reduced cost significantly and has improved safety.The foundation of this method is achieved the technology of adding entrainer in the supercritical carbon dioxide extraction process first on the large industrialized unit scale.
The present invention is that initiation material is through pretreatment with the Chinese crude drug Rhizoma Curcumae Longae.Filter through supercritical carbon dioxide extraction earlier and obtain curcumin part and filtrate, filtrate obtains Rhizoma Curcumae Longae essential oil and Rhizoma Curcumae Longae fatty oil part through molecular distillation.Product quality is better than extractum shape curcumin and the synthetic dyestuff lemon yellow that prior art obtains; Curcumin can be used for the interpolation coloring agent of food, daily-use chemical industry and medical product.Rhizoma Curcumae Longae essential oil can be used for making anti-Japanese solarization cosmetics, wrinkle resistant anti-aging cosmetics, essence and flavoring agent; Rhizoma Curcumae Longae fatty oil, preliminary clinic trial show that this product has antifungal and promotes the tissue regeneration effect, and being used for the treatment of burn, scald, skin ulcer, cervical erosion has certain curative effect.
Curcumin crystallization determination of recovery rates method of the present invention: measure the content B of curcumin in certain medical material and the crystalline content A of curcumin that makes by medicinal material extract with high performance liquid chromatogram.The response rate=A/B
Rhizoma Curcumae Longae essential oil recovery rate assay method of the present invention: the weight A/ of Rhizoma Curcumae Longae essential oil makes the used medical material weight of Rhizoma Curcumae Longae essential oil.
Rhizoma Curcumae Longae fatty oil recovery rate assay method of the present invention: the weight A/ of Rhizoma Curcumae Longae fatty oil makes the used medical material weight of Rhizoma Curcumae Longae fatty oil oil.
Advantage of the present invention is that it can the industrialization continued operation extract and isolate the different various turmeric effective ingredients of effect from Rhizoma Curcumae Longae, the quality assurance, and with short production cycle, the recovery rate height, production safety, environmental health is strictly controlled.
The specific embodiment
Embodiment 1
70 kilograms of Rhizoma Curcumae Longae coarse powder (20 order) place 200 liters of supercritical extraction reactor to extract.Keep extracting pressure 30MPa, 35 ℃ of extraction temperature are used 90% ethanol entrainer, and the mass ratio of entrainer consumption and raw material inventory is 6: 1, the extraction time is 4 hours, adopting " continuous decompressive analysis technology " to keep one-level to resolve pressure is 15Mpa, and secondary is resolved pressure 6Mpa, 60 ℃ of resolution temperatures, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide.The room temperature lucifuge that reclaims extraction I liquid behind the ethanol leaves standstill after 24 hours in the filtration of the direct SAM-2S of mistake of lucifuge pipeline type bag filter, obtains the curcumin paste.This curcumin paste places extraction kettle to carry out the supercritical carbon dioxide drying, extracting pressure 25MPa, and 35 ℃ of extraction temperature, drying got curcumin crystallization (purity 99%, the response rate 85%) in 2 hours.Filtrate and extraction II liquid carry out molecular distillation at vacuum 5Pa under the condition that temperature is 120 ℃, obtain higher Rhizoma Curcumae Longae essential oil of aroma quality (yield 4.5%) and Rhizoma Curcumae Longae fatty oil (yield 5.2%).
Continuous decompressive analysis technology is to carry out twice parsing and increase the single raise resolver in secondary resolver outlet, secondary resolver structure and technological requirement condition are identical with the secondary resolver, the secondary resolver is kept conventional analysis condition to guarantee normally carrying out of extraction process, and the entrainer that contains solute and more carbon dioxide of wherein being resolved continues to flow to secondary resolver, make carbon dioxide separation be recycled to behind the extracting system again with entrainer continuously decompression emit.
Embodiment 2
70 kilograms of Rhizoma Curcumae Longae coarse powder (20 order) place 200 liters of supercritical extraction reactor to extract.Keep extracting pressure 40MPa, 30 ℃ of extraction temperature are used the methanol entrainer, and the mass ratio of entrainer consumption and raw material inventory is 4: 1, the extraction time is 4 hours, adopting " continuous decompressive analysis technology " to keep one-level to resolve pressure is 10Mpa, and secondary is resolved pressure 6Mpa, 50 ℃ of resolution temperatures, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide.The room temperature lucifuge behind the ethanol of reclaiming extraction I liquid leaves standstill after 24 hours the filtration at the direct SAM-2S of mistake of lucifuge pipeline type bag filter.Obtain the curcumin paste, this curcumin paste places extraction kettle to carry out the supercritical carbon dioxide drying, extracting pressure 20MPa, and 30 ℃ of extraction temperature, drying got curcumin crystallization (purity 95%, the response rate 83%) in 2 hours.Filtrate and extraction II liquid carry out molecular distillation at vacuum 8Pa under the condition that temperature is 130 ℃, obtain higher Rhizoma Curcumae Longae essential oil of aroma quality (yield 4.0%) and Rhizoma Curcumae Longae fatty oil (yield 5.0%).
Embodiment 3
70 kilograms of Rhizoma Curcumae Longae coarse powder (20 order) place 200 liters of supercritical extraction reactor to extract.Keep extracting pressure 45MPa, 60 ℃ of extraction temperature, the acetone entrainer, the mass ratio of entrainer consumption and raw material inventory is 1: 1, the extraction time is 4 hours, adopting " continuous decompressive analysis technology " to keep one-level to resolve pressure is 20Mpa, and secondary is resolved pressure 6Mpa, 40 ℃ of resolution temperatures, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide.The room temperature lucifuge behind the ethanol of reclaiming extraction I liquid leaves standstill after 24 hours the filtration at the direct SAM-2S of mistake of lucifuge pipeline type bag filter.Obtain the curcumin paste, this curcumin paste places extraction kettle to carry out the supercritical carbon dioxide drying, extracting pressure 25MPa, and 40 ℃ of extraction temperature, drying got curcumin crystallization (purity 99%, the response rate 80%) in 2 hours.Filtrate and extraction II liquid carry out molecular distillation at vacuum 10Pa under the condition that temperature is 110 ℃, obtain higher Rhizoma Curcumae Longae essential oil of aroma quality (yield 4.3%) and Rhizoma Curcumae Longae fatty oil (yield 5.0%).
Claims (5)
1. the method that various effective ingredient extract continuously in the Rhizoma Curcumae Longae: it is characterized in that
A, supercritical carbon dioxide extraction
1., the Rhizoma Curcumae Longae coarse powder places supercritical extraction reactor, keeps extracting pressure 30Mpa to 45Mpa, 30 ℃ to 60 ℃ of extraction temperature are used entrainer, the mass ratio of entrainer consumption and raw material inventory is 1: 1 to 6: 1, the extraction time is 4 hours;
2., adopting continuous decompressive analysis technology selected temperature between 40 ℃ to 60 ℃ is resolution temperature, under the situation of this temperature constant, change pressure, pressure limit is 6～20Mpa, the parsing time is 4 hours, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide;
3., extraction I liquid chamber temperature lucifuge leaves standstill after 24 hours lucifuge and filters, the curcumin paste, reach filtrate;
4., the curcumin paste places supercritical extraction reactor to carry out the supercritical carbon dioxide drying, extracting pressure 20Mpa to 25Mpa, 30 ℃ to 40 ℃ of extraction temperature, dry 2 hours the curcumin crystallization;
B, with above filtering filtrate and extraction II liquid at vacuum 5Pa to 10Pa, carry out molecular distillation under the condition that temperature is 110 ℃ to 130 ℃, obtain Rhizoma Curcumae Longae essential oil and Rhizoma Curcumae Longae fatty oil.
2. the method that various effective ingredient extract continuously in the Rhizoma Curcumae Longae according to claim 1 is characterized in that
A, supercritical carbon dioxide extraction
1., the Rhizoma Curcumae Longae coarse powder places supercritical extraction reactor, keeps extracting pressure 30Mpa, 35 ℃ of extraction temperature are used entrainer, the mass ratio of entrainer consumption and raw material inventory is 6: 1, the extraction time is 4 hours;
2., to adopt continuous decompressive analysis technology to keep one-level to resolve pressure be 15Mpa, secondary is resolved pressure 6Mpa, 60 ℃ of resolution temperatures, carrying out secondary resolves, under one-level is resolved, obtain extracting I liquid, under secondary is resolved, obtain extracting II liquid, on the secondary extraction-container, add secondary resolver and reclaim carbon dioxide;
3., extraction I liquid chamber temperature lucifuge leaves standstill after 24 hours lucifuge and filters, the curcumin paste, reach filtrate;
4., the curcumin paste places supercritical extraction reactor to carry out the supercritical carbon dioxide drying, extracting pressure 25Mpa, 35 ℃ of extraction temperature, dry 2 hours the curcumin crystallization;
B, with above filtering filtrate and extraction II liquid at vacuum 5Pa, carry out molecular distillation under the condition that temperature is 120 ℃, obtain Rhizoma Curcumae Longae essential oil and Rhizoma Curcumae Longae fatty oil.
3. the method for extracting continuously according to various effective ingredient in claim 1 or the 2 described Rhizoma Curcumae Longaes is characterized in that described entrainer is ethanol, methanol or acetone.
4. according to the continuous method of extracting of various effective ingredient in claim 1 or the 2 described Rhizoma Curcumae Longaes, it is characterized in that continuous decompressive analysis technology is to carry out twice parsing and increase the single raise resolver in secondary resolver outlet, secondary resolver structure and technological requirement condition are identical with the secondary resolver, the secondary resolver is kept conventional analysis condition to guarantee normally carrying out of extraction process, and the entrainer that contains solute and more carbon dioxide of wherein being resolved continues to flow to secondary resolver, make carbon dioxide separation be recycled to behind the extracting system again with entrainer continuously decompression emit.
5. the method for extracting continuously according to various effective ingredient in claim 1 or the 2 described Rhizoma Curcumae Longaes is characterized in that extract room temperature lucifuge leaves standstill after 24 hours at the direct bag filter of crossing of lucifuge pipeline.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102226131B (en) * | 2011-05-26 | 2013-08-21 | 华南理工大学 | Preparation method of myrtle essential oil and application of myrtle essential oil in Guangdong sausage |
| CN102408320B (en) * | 2011-08-30 | 2014-04-09 | 河南中大生物工程有限公司 | Method for extracting and separating curcumin and curcuma oil from carcuma longa |
| CN103071117B (en) * | 2013-01-18 | 2014-01-08 | 四川汇丰生物科技有限公司 | Method for extracting curcuma oil and curcumine from rhizoma curcumae longae |
| CN103184104B (en) * | 2013-03-21 | 2014-06-04 | 长春工业大学 | Method for extracting schisandra volatile oil with borneol serving as principal component through low temperature evaporation |
| CN103254050A (en) * | 2013-04-23 | 2013-08-21 | 苏州谷力生物科技有限公司 | Process for extracting curcumin |
| CN105496830A (en) * | 2014-09-24 | 2016-04-20 | 广州玖玖伍捌健康科技股份有限公司 | Preparation method of alpinia japonica extract and application thereof in personal care products |
| CN105695101A (en) * | 2016-03-17 | 2016-06-22 | 西双版纳版纳药业有限责任公司 | Zingiber purpureum Rosc. volatile oil extracted through supercritical carbon dioxide and preparation method and application of Zingiber purpureum Rosc. volatile oil |
| KR101870248B1 (en) * | 2016-11-18 | 2018-06-22 | 주식회사 뉴트리사이언스 | A method for preparing extract of curcuma xanthorrhiza roxb. |
| CN109456835A (en) * | 2018-11-30 | 2019-03-12 | 大连理工大学 | A kind of preparation method of redwood essential oil |
| CN110240541A (en) * | 2019-07-08 | 2019-09-17 | 哈尔滨工业大学 | It is a kind of to use vacuum couplings ultrasonic wave-supercritical CO2The method of extraction extraction curcumin |
| CN110862869A (en) * | 2019-11-15 | 2020-03-06 | 广东暨晴生物医药科技有限公司 | By using supercritical CO2Method for preparing folium artemisiae argyi essential oil and byproducts thereof by extraction and secondary molecular distillation processes |
| CN111789283B (en) * | 2020-07-10 | 2022-11-11 | 湖北中烟工业有限责任公司 | Tobacco stem multi-stage utilization method based on supercritical CO2 extraction technology |
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| CN1150924C (en) * | 2001-01-20 | 2004-05-26 | 广州美晨药业有限公司 | Supercritica CO2 extraction and separation method of effective components of curcumae longae rhizome |
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| CN1150924C (en) * | 2001-01-20 | 2004-05-26 | 广州美晨药业有限公司 | Supercritica CO2 extraction and separation method of effective components of curcumae longae rhizome |
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