CN105903227A - Lavender absolute oil and preparation method thereof - Google Patents

Abstract

The invention relates to the technical field of lavender absolute, which is a kind of lavender absolute and a preparation method thereof; the following steps are carried out: the first step is to select lavender extract, and the lavender extract and the mass percentage are 93% to 98%. The ethanol aqueous solution is shaken and mixed according to the mass ratio of 0.9:1.8 to 1.1:2.2 to obtain a mixed solution; in the second step, the mixed solution is allowed to stand at -5°C to -10°C for 2 hours to 5 hours to obtain a frozen mixed solution. The extract extracted by subcritical equipment is used in the present invention to extract lavender absolute through the separation and extraction process in the later stage, which contains not only volatile but also non-volatile aromatic compounds, and linalool and linalyl acetate in the extracted absolute The content of camphor is obviously increased, the content of camphor is reduced, and the head, base and tail are better than the absolute oil of atmospheric distillation. Its fragrance is more full, long and stable, and the loss of small molecular compounds is less. the best raw materials.

Description

Absolute oil of lavender and preparation method thereof

technical field

The invention relates to the technical field of lavender absolute, and relates to a lavender absolute and a preparation method thereof.

Background technique

Liu Xiaocao from South China University of Technology and others carried out enzymatic hydrolysis-subcritical water extraction of active ingredients of ginger, the results show that: enzymatic hydrolysis-subcritical water extraction process, the most suitable temperature is 120 ℃; the best extraction pressure is 8MPa; The amount of enzyme added is 0.3%; the amount of feed is 100%; the extraction time is 20 minutes; the yield of active ingredients in sand ginger essential oil is about 10% higher than that of SWE method; The best process conditions are: static extraction, extraction time 30min, pressure 2 MPa, 100-150°C continuous temperature program, petroleum ether as extraction solvent, extraction 2 times; under this condition, the yield of onion essential oil is 0.362% , the content of sulfur compounds is 97.36g/kg. It is said that the designed 2L subcritical water extraction device has a high degree of automation and is easy to operate; South China University of Technology Guo Juan and others have carried out research on subcritical water extraction of essential oils in dried Zanthoxylum bungeanum, and the optimal process determined is; raw material particle size 0.5mm, extraction Time 40min, 100-150 ℃ continuous temperature program, pressure 5MPa; under these conditions, the extraction yield of Zanthoxylum bungeanum essential oil is 5.42%. At the same time, an oxidation test was carried out on Zanthoxylum bungeanum essential oil; Guo Keyong of Fuzhou University and others conducted a study on the extraction of pyrethrin extract with supersubcritical CO ₂ , and the optimized process conditions were: extraction pressure 20MPa, extraction temperature 25°C, CO ₂ The gas velocity is 100HL/h; the test shows that the entrainer can enhance the extraction effect; the Chinese patent document with the publication number of 101096614 discloses the subcritical extraction technology of rose essential oil vacuum water dispersing flushing and steaming invented by Yunnan Leisen Technology Company Lin Chengjie and others. Its characteristics are as follows: : Advanced head fragrance adsorption, and then use vacuum boiling method to expand the oily rose oil glands; then extract rose essential oil by superimposing method of steaming with water and rectification, and then analyze the adsorbed top fragrance. The content of the above documents listed shows that domestic research on the subcritical extraction process of sand ginger essential oil, onion essential oil, dried pepper essential oil, rose essential oil, and pyrethrin extract has been reported in the literature, but the research on the subcritical extraction process of lavender absolute oil There is no literature report.

The content of absolute linalool and linalyl acetate obtained by atmospheric distillation in the existing process is relatively low, and its content of camphor is relatively high.

Contents of the invention

The invention provides a kind of lavender absolute and preparation method thereof, overcomes above-mentioned deficiencies in the prior art, and it can effectively solve the low content of linalool and linalyl acetate in the absolute oil obtained by atmospheric distillation in the existing process, and The problem with its higher content of camphor.

One of the technical solutions of the present invention is achieved by the following measures: a kind of lavender absolute, obtained by the following method: the first step, choose lavender extract, the lavender extract and mass percentage are 93% to 98% % ethanol aqueous solution is mixed according to the mass ratio of 0.9:1.8 to 1.1:2.2 to obtain a mixed solution; in the second step, the mixed solution is allowed to stand at -5°C to -10°C for 2 hours to 5 hours to obtain a frozen mixed solution; In the third step, the frozen mixed solution is filtered through a 300-mesh to 400-mesh filter cloth, and then the filtrate is obtained after suction filtration with a Buchner funnel; in the fourth step, the filtrate is recovered to obtain the lavender absolute oil of the present invention after recovering the ethanol aqueous solution.

The following is a further optimization or/and improvement to one of the technical solutions of the above invention:

The above-mentioned lavender extract is obtained by the following method: the first step is to select lavender flowers; the second step is to put lavender flowers into a subcritical extraction kettle under the conditions that the extraction pressure is 2Mpa to 4Mpa and the extraction temperature is 30°C to 40°C The extraction agent R134a is introduced into the subcritical extraction kettle through a booster pump with a flow rate of 8 g/min to 12 g/min for continuous extraction for 1 hour to 2 hours to obtain the lavender fluid; the third step is to extract the lavender fluid from the subcritical extraction kettle The medium flows into a subcritical separation kettle and is lowered to normal temperature and pressure for separation to obtain lavender extract.

The above-mentioned method for reclaiming the aqueous ethanol solution is to reclaim the aqueous ethanol solution for 1 hour to 5 hours with a rotary evaporator at 40 degrees Celsius to 45 degrees Celsius, a rotating speed of 12 rpm to 14 rpm, and a vacuum of 0.07Mpa to 0.08Mpa.

The lavender extract and the 95% ethanol aqueous solution are shaken and mixed for 20 minutes to 40 minutes.

The filter paper used in the above-mentioned Buchner funnel is qualitative filter paper.

The second technical scheme of the present invention is achieved by the following measures: a preparation method of lavender absolute, carried out according to the following steps: the first step, choose lavender extract, and the lavender extract and mass percentage are 93 % to 98% ethanol aqueous solution in a mass ratio of 0.9:1.8 to 1.1:2.2 and then shake and mix to obtain a mixed solution; the second step is to freeze the mixed solution at -5°C to -10°C for 2 hours to 5 hours Mixed solution; in the third step, the frozen mixed solution is filtered through 300 order to 400 order filter cloth, and then the filtrate is obtained after suction filtration with a Buchner funnel; in the fourth step, the filtrate obtains lavender absolute oil of the present invention after reclaiming the ethanol aqueous solution .

The following is a further optimization or/and improvement to the second technical solution of the above invention:

The above-mentioned lavender extract is obtained by the following method: the first step is to select lavender flowers; the second step is to put lavender flowers into a subcritical extraction kettle under the conditions that the extraction pressure is 2Mpa to 4Mpa and the extraction temperature is 30°C to 40°C The extraction agent R134a is introduced into the subcritical extraction kettle through a booster pump with a flow rate of 8 g/min to 12 g/min for continuous extraction for 1 hour to 2 hours to obtain the lavender fluid; the third step is to extract the lavender fluid from the subcritical extraction kettle The medium flows into the subcritical separation kettle and is lowered to normal temperature for separation to obtain lavender extract.

The above-mentioned method for reclaiming the aqueous ethanol solution is to reclaim the aqueous ethanol solution for 1 hour to 5 hours with a rotary evaporator at 40 degrees Celsius to 45 degrees Celsius, a rotating speed of 12 rpm to 14 rpm, and a vacuum of 0.07Mpa to 0.08Mpa.

The lavender extract and the 95% ethanol aqueous solution are shaken and mixed for 20 minutes to 40 minutes.

The filter paper used in the above-mentioned Buchner funnel is qualitative filter paper.

The extract extracted by subcritical equipment is used in the present invention to extract lavender absolute through the separation and extraction process in the later stage, which contains not only volatile but also non-volatile aromatic compounds, and linalool and linalyl acetate in the extracted absolute The content of camphor is obviously increased, the content of camphor is reduced, and the head, base and tail are better than the absolute oil of atmospheric distillation. Its fragrance is more full, long and stable, and the loss of small molecular compounds is less. the best raw materials.

detailed description

The present invention is not limited by the following examples, and specific implementation methods can be determined according to the technical solutions of the present invention and actual conditions.

Embodiment 1, the preparation method of this lavender absolute oil is obtained according to the following steps: the first step, choose lavender extract, and the ethanol aqueous solution that the mass percentage content is 93% to 98% by lavender extract and mass percentage is 0.9 : 1.8 to 1.1: 2.2 After shaking and mixing, the mixed solution is obtained; in the second step, the frozen mixed solution is obtained after standing at -5°C to -10°C for 2 hours to 5 hours; in the third step, the frozen mixed solution is After 300 order to 400 order filter cloth filter, obtain filtrate after carrying out suction filtration with Buchner funnel again; The 4th step, filtrate obtains lavender absolute oil of the present invention after reclaiming ethanol aqueous solution.

Embodiment 2, the preparation method of this lavender absolute oil is obtained according to the following steps: the first step, choose lavender extract, and the ethanol aqueous solution that the mass percentage content is 93% to 98% by lavender extract and mass percentage is 0.9 : 1.8 to 1.1: 2.2 After shaking and mixing, the mixed solution is obtained; the second step is to stand the mixed solution at -5°C or -10°C for 2 hours or 5 hours to obtain the frozen mixed solution; the third step is to freeze the mixed solution through After 300 order or 400 order filter cloths filter, obtain filtrate after carrying out suction filtration with Buchner funnel again; The 4th step, filtrate obtains lavender absolute oil of the present invention after reclaiming ethanol aqueous solution.

Embodiment 3, as above-mentioned embodiment optimization, this lavender extract is obtained by the following method: the first step, selects lavender fresh flowers; Second step, puts lavender fresh flowers into subcritical extraction kettle, is 2Mpa to 4Mpa at extraction pressure , under the conditions of extraction temperature 30°C to 40°C, the extraction agent R134a is introduced into the subcritical extraction kettle through a booster pump with a flow rate of 8 g/min to 12 g/min for continuous extraction for 1 hour to 2 hours to obtain lavender fluid; the third The first step is to flow the lavender fluid from the subcritical extraction kettle into the subcritical separation kettle and lower it to normal temperature for separation to obtain lavender extract.

Embodiment 4, as the optimization of the above examples, the method of recovering the ethanol aqueous solution is to use a rotary evaporator at 40 degrees Celsius to 45 degrees Celsius, the rotating speed is 12 rpm to 14 rpm, and the vacuum is 0.07Mpa to 0.08Mpa. Ethanol in water for 1 hour to 5 hours.

Example 5, as an optimization of the above example, the mixing time of lavender extract and 95% ethanol aqueous solution by mass percentage is 20 minutes to 40 minutes.

Embodiment 6, as the optimization of the above embodiment, the filter paper used in the Buchner funnel is qualitative filter paper.

Embodiment 7, this lavender absolute oil is obtained by the following preparation method: the first step, the lavender fresh flowers are sent in the extraction kettle, and the extraction agent R134a is introduced into the separation tank with a booster pump, and the extraction pressure is 2Mpa, and the extraction temperature is 30°C. Under the condition of ℃, carry out continuous extraction for 1 hour to obtain lavender fluid, wherein the flow rate of extractant R134a is 8 g/min, and the extractant R134a fluid flowing out from the extraction tank is directly released from the separation tank to normal temperature and pressure, so that the extraction The agent R134a is separated from the lavender fluid to obtain the lavender extract, and the lavender extract and the ethanol aqueous solution with a mass percentage of 93% to 98% are mixed according to the mass ratio of 0.9:1.8 to 1.1:2.2 to obtain a mixed solution; the second step , put the mixed solution at a temperature of -5°C for 3 hours and freeze it to obtain the frozen mixed solution; the third step is to filter the frozen mixed solution with a 300-mesh filter cloth and qualitative filter paper with a Buchner funnel to obtain the filtrate; the fourth step is to obtain the filtrate The filtrate reclaims the ethanol aqueous solution, and with a rotary evaporator at 40 degrees Celsius, the rotating speed is 12 to 14 rev/min, and the vacuum is 0.07Mpa to reclaim the ethanol aqueous solution for 2 hours to obtain lavender absolute.

Embodiment 8, the lavender absolute oil is obtained by the following preparation method: the first step, the lavender fresh flowers are sent into the extraction kettle, and the extraction agent R134a is introduced into the separation tank with a booster pump, and the extraction pressure is 3Mpa, and the extraction temperature is 35 Under the condition of ℃, carry out continuous extraction for 1.5 hours to obtain lavender fluid, wherein the flow rate of extractant R134a is 10 g/min, and the extractant R134a fluid flowing out from the extraction tank is directly released from the separation tank to normal temperature and pressure, so that the extraction The agent R134a is separated from the lavender fluid to obtain the lavender extract, and the lavender extract and the ethanol aqueous solution with a mass percentage of 93% to 98% are mixed according to the mass ratio of 0.9:1.8 to 1.1:2.2 to obtain a mixed solution; the second step , put the mixed solution at -7°C for 4 hours and freeze it to obtain the frozen mixed solution; the third step is to filter the frozen mixed solution with a 300-mesh filter cloth and qualitative filter paper with a Buchner funnel to obtain the filtrate; the fourth step is to obtain the filtrate The filtrate reclaims the aqueous ethanol solution, and at 42 degrees Celsius with a rotary evaporator, the rotating speed is 12 to 14 rpm, and the vacuum is 0.075Mpa to reclaim the aqueous ethanol solution for 2.5 hours to obtain lavender absolute.

Embodiment 9, the lavender absolute oil is obtained by the following preparation method: the first step, the lavender fresh flowers are sent into the extraction kettle, and the extraction agent R134a is introduced into the separation tank with a booster pump, and the extraction pressure is 4Mpa, and the extraction temperature is 40°C. Under the condition of ℃, carry out continuous extraction for 2 hours to obtain lavender fluid, wherein the flow rate of extractant R134a is 12 g/min, and the extractant R134a fluid flowing out from the extraction tank is directly released from the separation tank to normal temperature and pressure, so that the extraction The agent R134a is separated from the lavender fluid to obtain the lavender extract, and the lavender extract and the ethanol aqueous solution with a mass percentage of 93% to 98% are mixed according to the mass ratio of 0.9:1.8 to 1.1:2.2 to obtain a mixed solution; the second step , put the mixed solution at -10°C for 3 hours and freeze it to obtain the frozen mixed solution; the third step is to filter the frozen mixed solution with a 400-mesh filter cloth and qualitative filter paper with a Buchner funnel to obtain the filtrate; the fourth step is to The filtrate reclaims the aqueous ethanol solution, uses a rotary evaporator at 45 degrees Celsius, the rotating speed is 12 to 14 rpm, and the vacuum degree is 0.075Mpa to reclaim the aqueous ethanol solution for 2 hours to obtain lavender absolute.

The representative component content of the lavender absolute of the present invention that embodiment 7 obtains is shown in Table 1; The representative component content of the lavender absolute of the present invention that embodiment 8 obtains is shown in Table 2; The present invention that embodiment 9 obtains The representative component content of invention lavender absolute is shown in table 3; As can be seen from table 1, table 2 and table 3, the lavender absolute that the present invention obtains not only contains volatile, and contains nonvolatile aromatic certain class Compounds, the content of effective substances linalool and linalyl acetate has been greatly improved compared with the existing atmospheric distillation extraction process, the most critical restrictive index camphor content has been greatly reduced, and the extracted absolute oil, top incense The fragrance, base fragrance and tail fragrance are all better than the absolute oil distilled at atmospheric pressure. Its fragrance is more full, long and stable, and the loss of small molecular compounds is less. It is the best raw material for blending high-end perfume and top-quality essential oil. The lavender resources have increased the utilization rate of lavender, and the extractant is recycled, which is environmentally friendly, low-consumption, and pollution-free.

In summary, the lavender absolute that the present invention obtains not only contains volatility, but also contains non-volatile aromatic certain compounds, wherein the content of effective substance linalool and linalyl acetate is greatly improved, the most critical The restrictive index camphor content has decreased to a large extent. The extracted absolute oil, head fragrance, base fragrance, and tail fragrance are all better than the essential oils distilled at atmospheric pressure. The fragrance is fuller, longer and stable, and the loss of small molecular compounds is less. It is the best raw material for blending high-grade perfume and essential oil. The lavender resources are rationally used in the production process, which improves the utilization rate of lavender. The extractant is recycled, which is environmentally friendly, low-consumption, and pollution-free.

The above technical features constitute the embodiment of the present invention, which has strong adaptability and implementation effect, and non-essential technical features can be increased or decreased according to actual needs to meet the needs of different situations.

Claims (10)

1. a lavender absolute oil, it is characterised in that obtain as follows: the first step, chooses lavender medicinal extract, by lavender After medicinal extract and the ethanol water that weight/mass percentage composition is 93% to 98% mix for 0.9:1.8 to 1.1:2.2 concussion in mass ratio Obtain mixed liquor；Second step, obtains freezing mixture after mixed liquor is stood 2 hours to 5 hours at-5 DEG C to-10 DEG C；3rd Step, by freezing mixture after 300 mesh to 400 mesh filter-cloth filterings, then obtains filtrate after carrying out suction filtration with Buchner funnel；4th Step, obtains lavender absolute oil of the present invention after the recovered ethanol water of filtrate.

Lavender absolute oil the most according to claim 1, it is characterised in that lavender medicinal extract obtains as follows: first Step, chooses lavender fresh flower；Second step, puts into lavender fresh flower in subcritical abstraction still, extracting pressure be 2Mpa extremely 4Mpa, is that 8 gram/minute are to 12 Grams Per Minutes by extractant R134a by force (forcing) pump flow under conditions of extraction temperature 30 DEG C to 40 DEG C Clock importing subcritical abstraction still carries out continuous extraction and within 1 hour, obtains lavender fluid to 2 hours；3rd step, flows lavender Body flows in subcritical separating still from subcritical abstraction still is down under normal temperature separate, and obtains lavender medicinal extract.

Lavender absolute oil the most according to claim 1 and 2, it is characterised in that reclaim the method for ethanol water for rotating Evaporimeter is at 40 degrees Celsius to 45 degrees Celsius, and rotating speed is 12 revs/min to 14 revs/min, and vacuum is 0.07Mpa to 0.08Mpa bar Ethanol water is reclaimed 1 hour to 5 hours under part.

4. according to the lavender absolute oil described in claim 1 or 2 or 3, it is characterised in that lavender medicinal extract and weight/mass percentage composition Be 95% ethanol water concussion incorporation time be 20 minutes to 40 minutes.

5. according to the lavender absolute oil described in claim 1 or 2 or 3 or 4, it is characterised in that filter paper used in Buchner funnel is Qualitative filter paper.

6. the preparation method of a lavender absolute oil according to claim 1, it is characterised in that carry out in the steps below: the One step, chooses lavender medicinal extract, by lavender medicinal extract and ethanol water that weight/mass percentage composition is 93% to 98% in mass ratio For obtaining mixed liquor after 0.9:1.8 to 1.1:2.2 concussion mixing；Second step, stands 2 hours by mixed liquor at-5 DEG C to-10 DEG C Freezing mixture is obtained after 5 hours；3rd step, by freezing mixture after 300 mesh to 400 mesh filter-cloth filterings, then uses Bu Shi Funnel obtains filtrate after carrying out suction filtration；4th step, obtains lavender absolute oil of the present invention after the recovered ethanol water of filtrate.

The preparation method of lavender absolute oil the most according to claim 6, it is characterised in that lavender medicinal extract is as follows Obtain: the first step, choose lavender fresh flower；Second step, puts into lavender fresh flower in subcritical abstraction still, in extracting pressure is 2Mpa to 4Mpa, under conditions of extraction temperature 30 DEG C to 40 DEG C by extractant R134a by force (forcing) pump flow be 8 gram/minute extremely 12 gram/minute importing subcritical abstraction stills carry out continuous extraction and within 1 hour, obtains lavender fluid to 2 hours；3rd step, will smoke Clothing grass fluid flows in subcritical separating still from subcritical abstraction still is down under normal temperature separate, and obtains lavender medicinal extract.

8. according to the preparation method of the lavender absolute oil described in claim 6 or 7, it is characterised in that reclaim the side of ethanol water Method for Rotary Evaporators at 40 degrees Celsius to 45 degrees Celsius, rotating speed is 12 revs/min to 14 revs/min, vacuum be 0.07Mpa extremely Ethanol water is reclaimed 1 hour to 5 hours under the conditions of 0.08Mpa.

9. according to the preparation method of the lavender absolute oil described in claim 6 or 7 or 8, it is characterised in that lavender medicinal extract and matter Measuring the ethanol water concussion incorporation time that percentage composition is 95% is 20 minutes to 40 minutes.

10. according to the preparation method of the lavender absolute oil described in claim 6 or 7 or 8 or 9, it is characterised in that in Buchner funnel Filter paper used is qualitative filter paper.