CN102559385A - Production process method for extracting peppermint oil with supercritical carbon dioxide - Google Patents
Production process method for extracting peppermint oil with supercritical carbon dioxide Download PDFInfo
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- CN102559385A CN102559385A CN2010105868686A CN201010586868A CN102559385A CN 102559385 A CN102559385 A CN 102559385A CN 2010105868686 A CN2010105868686 A CN 2010105868686A CN 201010586868 A CN201010586868 A CN 201010586868A CN 102559385 A CN102559385 A CN 102559385A
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Abstract
The invention relates to a production process method for extracting peppermint oil with supercritical carbon dioxide. The method comprises the following operation steps of: selection of raw materials: picking the used peppermint from Liu'an region, Anhui Province, and picking the overground parts of peppermint in late each year; and extraction of essential oil: putting a dry peppermint sample into an extraction kettle, and collecting the peppermint oil by regulating the extraction pressure, the extraction temperature, the extraction time and the flow of carbon dioxide. Compared with the traditional extraction method, the method has high oil yield of extracting the peppermint oil. The kinds of compounds contained in the peppermint oil obtained through the method is more than the kinds of the peppermint oil extracted through the traditional steam method, and the natural scent of the peppermint can be really reflected. The extraction time of the peppermint oil is greatly shortened, the energy consumption is less than that of the traditional steam extraction method, the oil yield is increased to the maximum extent, and the purposes of energy saving and emission reduction is furthest realized. A solvent used in the method is carbon dioxide, and the solvent has stabile property, low cost and no toxicity, does not burn and can be recycled.
Description
Technical field
The invention belongs to plants essential oil abstraction technique field, be specifically related to be used for the spearmint oil extracting production process method of Labiatae mint.
Background technology
Peppermint is one of China's traditional Chinese medicine commonly used, is again a kind of important spice berry.Spearmint oil dispelling wind, heat radiation, toxicide effect are used to treat common cold due to wind-heat, headache, hot eyes, swelling and pain in the throat, toothache etc.Contain volatile oil in peppermint stem, the leaf, wherein main effective constituent is Therapeutic Mineral Ice.As large conventional Chinese medicine, only the Chinese patent medicine commonly used that contains peppermint, spearmint oil and Therapeutic Mineral Ice that records of " Chinese people republic pharmacopeia " (2010 editions one one) just has kind more than 40.Spearmint oil, Therapeutic Mineral Ice are widely used in fields such as medical and health, daily-use chemical industry, food-processing.
Shortcomings such as at present, the extraction to Herba Menthae Haplocalycis volatile oil is main with wet distillation mainly both at home and abroad, and is low but traditional technology exists oil yield, and it is big to consume energy.
Summary of the invention
Low in order to solve the oil yield that traditional technology exists, problem such as it is big to consume energy, the present invention provides a kind of supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique.
Supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique comprises following operation steps:
The selection of A, raw material
Used peppermint is picked up from the Lu'an Prefecture, Anhui Province, adopts its over-ground part the annual last ten-days period in July;
The extraction of B, essential oil
Get the peppermint dry sample extraction kettle of packing into, through regulating extracting pressure, extraction temperature, the flow of extraction time and carbonic acid gas, collection spearmint oil.
C, the spearmint oil of collecting is analyzed
Use chromatographic column to be the ZB-WAX fused-silica capillary column, 80 ℃ of column temperatures, constant temperature 2 minutes; Temperature programming: 5 ℃/minute rise to 110 ℃, keep 1 minute; 3 ℃/minute rise to 150 ℃, keep 1 minute; 6 ℃/minute rise to 170 ℃; 240 ℃ of temperature of vaporization chamber; Carrier gas is the nitrogen of concentration 99.99%; 240 ℃ of detected temperatures (FID); Splitting ratio 20:1; Sample size 0.2 microlitre.
The method of calculation of D, spearmint oil content
TK-10 content * 100% in TK-10 content (%)=percentage extraction * spearmint oil in the sample.
According to above-mentioned supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique,
1.1. supercritical extraction can be near room temperature (35～50 ℃) and CO
2Extract under gas shrouds, prevented the oxidation and the loss of heat-sensitive substance effectively.
1.2 be a kind of process for extracting of clean environment firendly.Whole process is without organic solvent, and the vehicle substance of the exhausted noresidue of extract has guaranteed 100% pure natural property.
1.3. extraction unites two into one with separating, and has improved efficient, has reduced cost.Because the decline or the variation of temperature of pressure, make CO
2Become two (gas-liquid separations) and separate immediately mutually rapidly with extract, improved usefulness and reduced cost.
1.4. security is higher.CO
2Be a kind of inactive gas, chemical reaction do not take place in the extraction process, and belong to non-flammable gases, tasteless, odorless, nontoxic.
1.5 CO
2Gas price is cheap, and purity is high, produces easily, and can recirculation use aborning, thereby reduced cost effectively.
1.6 the simple easy master of technology, and the speed of extraction is fast.Pressure and temperature can become the parameter of regulating extraction process, through changing the purpose that temperature and pressure reaches extraction.
Useful technique effect of the present invention embodies in the following areas:
1. the process method oil yield that supercritical carbon dioxide extraction method of the present invention extracts spearmint oil is higher than the oil yield of conventional method of extraction extraction spearmint oil.
2. the spearmint oil that uses supercritical carbon dioxide extraction is analyzed, found that the kind analogy of contained compound is many with the kind of the spearmint oil of traditional method for extracting, can reflect the natural flavor of peppermint itself more really.
3. can shorten the extraction time of spearmint oil greatly with supercritical carbon dioxide extraction method, energy consumption is littler much than traditional water steam extraction method, has farthest accomplished not only to have improved oil yield but also accomplished energy-saving and emission-reduction.
4. the solvent that uses in this method is carbonic acid gas, and it is not only a kind of very strong solvent when supercutical fluid, comparatively speaking, stable in properties, low price, nontoxic, do not burn, can be recycled.
Embodiment
Below in conjunction with embodiment, the present invention is done to describe further.
Embodiment:
Supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique comprises following operation steps:
The selection of A, raw material
Used peppermint is picked up from Anhui six peaces, adopts its over-ground part in late July, 2009, identifies through Institute of Botany, Chinese Academy of Sciences.
The extraction of B, essential oil
Adopt supercritical CO
2Extraction process (SCDE) extracts volatile oil from peppermint.Regulate extraction temperature and separation temperature to set(ting)value.Turn on pump is forced into the extracting pressure of setting, and regulates CO
2Flow.After the extraction time that reaches the experiment setting, regulate reducing valve, be decompressed to normal pressure.Collect spearmint oil, use anhydrous Na
2SO
4Dehydration is filtered, and weighs, and calculates oil yield, and measures TK-10 content.Adopting supercritical CO
2Identify 54 kinds of compositions altogether in the volatile oil that extraction process extracts, its staple is pulegone, piperitone, linolic acid muriate etc.
C. process optimization process
(1) experiment of single factor is by above-mentioned extracting process, and adjusting extracting pressure respectively is 8,10,12,15 and 18 MPa; 35,45,55 and 65 ℃ of extraction temperature; CO2 flow 20,30,40 and 50 L/ hours, the extraction time was 0.5,1.0,1,5,2,0 and 2.5 hour, carries out experiment of single factor.
(2) orthogonal experiment is pressed (3) orthogonal table contrived experiment, slective extraction pressure (A), extraction temperature (B), CO: flow (c) and extraction time (D) 4 factors, and it is 8,10 and 12 MPa that extracting pressure is set; Extraction temperature is 40,50 and 60 ℃; The CO2 flow is 20,30 and 40 L/ hours; The extraction time is 1.0,1.5 and 2.0 hours.Carry out orthogonal experiment by above-mentioned extracting process.
(3) analytical conditions for gas chromatography TK-10 reference substance is available from Nat'l Pharmaceutical & Biological Products Control Institute.
Chromatographic condition: chromatographic column is ZB-WAX fused-silica capillary column (30 m * 0,25 mm * 0,25 mm); 80 ℃ of column temperatures, constant temperature 2 minutes.Temperature programming: 5 ℃/minute rise to 110 ℃, keep 1 minute; 3 ℃/minute rise to 150 ℃, keep 1 minute; 6 ℃/minute rise to 170 ℃.240 ℃ of temperature of vaporization chamber; Carrier gas is high pure nitrogen (99,99%); 240 ℃ of detected temperatures (FID); Splitting ratio 20:1; Sample size 2 μ L (ethyl acetate solution).
The method of calculation of D, TK-10 content
TK-10 content * 100% in TK-10 content (%)=percentage extraction * spearmint oil in the sample.
Result and analysis
The experiment of single factor result
1.1 extracting pressure is a supercritical CO to the pressure that influences of percentage extraction and TK-10 content
2One of most important parameter in the extraction process.When extraction temperature one timing, along with the increase of extracting pressure, the density of supercutical fluid increases, thereby dissolving power is strengthened.Can find out from table 1, at 55 ℃ of extraction temperature, CO
2Under flow 30 L/ hours, the condition of 1.5 hours extraction time, when extracting pressure was increased to 10MPa from 8MPa, TK-10 content increased very fast in the sample; But after pressure increased to 10MPa, TK-10 content began to reduce in the sample.Therefore, extracting pressure should be chosen to be 10MPa.
1.2 extraction temperature also has considerable influence to the temperature that influences of percentage extraction and TK-10 content to effect of extracting.On the one hand, along with the rising of temperature, the supercritical flow volume density constantly reduces, the also corresponding decline of its dissolving power, thus cause extracting the minimizing of quantity; On the other hand, temperature raises the volatility that is extracted solute is increased, and impels extract to exist
Concentration in the overcritical gas phase increases, thereby extraction quantity is increased.Can find out from table 2, at extracting pressure 10MPa, CO
2Under flow 30L/ hour, the condition of 1.5 hours extraction time, along with the increase of temperature, the corresponding increase of spearmint oil percentage extraction; After temperature arrived 55 ℃, TK-10 content increased slowly in the sample.Therefore, extraction temperature is selected in 55 ℃ and is advisable.
Table 1 extracting pressure is to the influence of spearmint oil percentage extraction and TK-10 content
Table 2 extraction temperature is to the influence of spearmint oil percentage extraction and TK-10 content
1.3 CO
2Flow is to the influence of percentage extraction and TK-10 content.Supercritical CO
2In the extraction process, CO
2Flow is seen table 3 to the influence of spearmint oil percentage extraction.CO
2The variation of flow is complicated to the influence of supercritical fluid extraction process, the influence that extraction is produced favourable and unfavorable 2 aspects.When strengthening CO
2During flow, flow velocity is accelerated, and the extraction liquid residence time shortens, CO
2With extract minimizing duration of contact, be unfavorable for extraction; Along with CO
2The increase of flow, the mass transfer effect of extraction process strengthens, supercritical CO
2Can promptly dissolved solute be worn away from stock chart, thereby improve extracting power.
Can find out that from table 3 under extracting pressure 10MPa, 55 ℃ of extraction temperature, the condition of 1.5 hours extraction time, TK-10 content is along with CO in the sample
2Flow increases and increases progressively, but after flow was increased to a certain degree, TK-10 content increase trend was gradually slow in the sample.Consider CO
2Flow increased senior general and caused CO
2Consume the increase of increase and production cost, therefore, CO
2Flow is chosen to be 3OL/ hour.
Table 3 CO
2Flow is to the influence of spearmint oil percentage extraction and TK-10 content
1.4 the extraction time is to the influence of percentage extraction and TK-10 content
Can find out by table 4, at extracting pressure 10 MPa, extraction temperature 55%, CO
2Flow is under 3O L/ hour the condition, and along with the increase of extraction time, TK-10 content increases in the sample, but when the extraction time is increased to 1.5 hours after, TK-10 content begins minimizing in the sample.Therefore, the extraction selection of time was advisable in 1.5 hours.
The table 4 extraction time is to the influence of spearmint oil percentage extraction and TK-10 content
Orthogonal experiment results
According to the experiment of single factor result, design the experiment of 4 factors, 3 horizontal quadratures, orthogonal experiment design and result see table 5.Visible by table 5, to the influence factor of TK-10 content in the peppermint sample from big to being followed successively by extracting pressure, extraction temperature, extraction time, CO for a short time
2Flow.The extraction conditions that TK-10 content is the highest in the peppermint sample is A B C D, and promptly extracting pressure is that 10MPa, extraction temperature are 50 ℃, CO
2, flow is that 30L/ hour, extraction time are 1.5 hours.
Table 5 spearmint oil supercritical CO
2The orthogonal experiment design and the result of extraction
The technology summary
Extracting pressure is the important factor that influences spearmint oil percentage extraction and TK-10 content.When extracting pressure was 10MPa, spearmint oil was the clear oily matter of reddish-brown; When extracting pressure reached 15MPa, the gained spearmint oil was a sap green, and this is because part chlorophyll together is extracted out with volatile oil; When extracting pressure surpassed 20MPa, what from separating still, be separated to was the sap green paste, rather than oily matter, and this is that materials such as the chlorophyll in the peppermint, wax and resin are extracted in a large number because of hypertonia.Therefore, at the supercritical CO of spearmint oil
2In the extraction process, extracting pressure is unsuitable too high.
The extraction time is also bigger to the influence of TK-10 content.At supercritical CO
2In the extraction process, TK-10 at first is extracted out, and the speed that other compositions are extracted out is slower.So after extraction after a while, along with the increase of extraction time, the TK-10 total amount that is extracted does not out have to change basically, and the total amount of spearmint oil is increasing, therefore, TK-10 content reduces on the contrary in the spearmint oil.
Supercritical CO
2Extraction is during spearmint oil, and 4 factors are followed successively by extracting pressure, extraction temperature, extraction time, CO from high to low to the influence degree of TK-10 content in the peppermint sample
2Flow.The highest extraction conditions of TK-10 content is extracting pressure 10MPa, 50 ℃ of extraction temperature, CO in the peppermint sample
2Flow 30L/ hour and 1.5 hours extraction time.
In actual production, spearmint oil mainly is to extract through steam distillation to obtain, and its spearmint oil yield and TK-10 content are all lower; Comparatively speaking, utilize supercritical CO
2Abstraction technique not only can improve the oil yield and the TK-10 content of spearmint oil, can also effectively keep natural flavor and the color and luster of peppermint.
Claims (2)
1. supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique is characterized in that comprising following operation steps:
1.1 the selection of raw material
Used peppermint is picked up from the Lu'an Prefecture, Anhui Province, adopts its over-ground part the annual last ten-days period in July;
1.2 the extraction of essential oil
Get the peppermint dry sample extraction kettle of packing into, through regulating extracting pressure, extraction temperature, the flow of extraction time and carbonic acid gas, collection spearmint oil;
1.3 the spearmint oil to collecting is analyzed
Use chromatographic column to be ZB-WAX fused-silica capillary column (30 m * 0,25 mm * 0,25 mm), 80 ℃ of column temperatures, constant temperature 2 minutes; Temperature programming: 5 ℃/minute rise to 110 ℃, keep 1 minute; 3 ℃/minute rise to 150 ℃, keep 1 minute; 6 ℃/minute rise to 170 ℃; 240 ℃ of temperature of vaporization chamber; Carrier gas is the nitrogen of concentration 99.99%; 240 ℃ of detected temperatures (FID); Splitting ratio 20:1; Sample size 0.2 microlitre.
2. supercritical carbon dioxide extraction spearmint oil producing and manufacturing technique according to claim 1 is characterized in that:
2.1 supercritical extraction can be near room temperature (35～50 ℃) and CO
2Extract under gas shrouds, prevented the oxidation and the loss of heat-sensitive substance effectively;
2.2 be a kind of process for extracting of clean environment firendly; Whole process is without organic solvent, and the vehicle substance of the exhausted noresidue of extract has guaranteed 100% pure natural property;
2.3 extraction unites two into one with separating, and has improved efficient, has reduced cost; Because the decline or the variation of temperature of pressure, make CO
2Become two (gas-liquid separations) and separate immediately mutually rapidly with extract, improved usefulness and reduced cost;
2.4 security is higher, CO
2Be a kind of inactive gas, chemical reaction do not take place in the extraction process, and belong to non-flammable gases, tasteless, odorless, nontoxic;
2.5 CO
2Gas price is cheap, and purity is high, produces easily, and can recirculation use aborning, thereby reduced cost effectively;
2.6 the simple easy master of technology, and the speed of extraction is fast; Pressure and temperature can become the parameter of regulating extraction process, through changing the purpose that temperature and pressure reaches extraction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104274634A (en) * | 2014-08-14 | 2015-01-14 | 杭州方回春堂国药馆有限公司 | Compound plant essential oil for refreshing, restoring consciousness, diminishing swelling and relieving itching and preparation method of compound plant essential oil |
| CN104560400A (en) * | 2014-12-26 | 2015-04-29 | 江苏省中国科学院植物研究所 | Method for extracting peppermint oil |
| CN106318636A (en) * | 2016-08-28 | 2017-01-11 | 广西灏源盛世生物科技有限公司 | Extracting method for mint essential oil |
| CN112175713A (en) * | 2020-09-30 | 2021-01-05 | 云南贝泰妮生物科技集团股份有限公司 | Preparation process of prinsepia utilis royle oil with long oxidation induction time |
-
2010
- 2010-12-14 CN CN2010105868686A patent/CN102559385A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104274634A (en) * | 2014-08-14 | 2015-01-14 | 杭州方回春堂国药馆有限公司 | Compound plant essential oil for refreshing, restoring consciousness, diminishing swelling and relieving itching and preparation method of compound plant essential oil |
| CN104560400A (en) * | 2014-12-26 | 2015-04-29 | 江苏省中国科学院植物研究所 | Method for extracting peppermint oil |
| CN106318636A (en) * | 2016-08-28 | 2017-01-11 | 广西灏源盛世生物科技有限公司 | Extracting method for mint essential oil |
| CN112175713A (en) * | 2020-09-30 | 2021-01-05 | 云南贝泰妮生物科技集团股份有限公司 | Preparation process of prinsepia utilis royle oil with long oxidation induction time |
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Application publication date: 20120711 |