CN101129316A - Ligaloes perfumes and method of producing the same - Google Patents

Ligaloes perfumes and method of producing the same Download PDF

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Publication number
CN101129316A
CN101129316A CNA2007101211283A CN200710121128A CN101129316A CN 101129316 A CN101129316 A CN 101129316A CN A2007101211283 A CNA2007101211283 A CN A2007101211283A CN 200710121128 A CN200710121128 A CN 200710121128A CN 101129316 A CN101129316 A CN 101129316A
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parts
ligaloes
perfumes
organic solvent
linaloe oil
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CN101129316B (en
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戴好富
梅文莉
吴娇
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Hainan Modern Agriculture And Forestry Development Holding Group Co ltd
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Institute of Tropical Bioscience and Biotechnology Chinese Academy of Tropical Agricultural Sciences
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Abstract

The invention discloses a linaloe perfume and making method, which is composed of 2. 5-8. 5wt% linaloe oil and 95-105wt% spirit, wherein the linaloe oil is extracted benzine with sesquiterpenes, benzyl acetone, p-methoxy benzyl acetone. The invention has simple preparing technique and formulation with peculiar scent and sedative and tranquilizing effect, which releases working pressure and mood with wide applying scale and good market developing prospect.

Description

A kind of Ligaloes perfumes and preparation method thereof
Technical field
The present invention relates to a kind of perfume and preparation method thereof, particularly about a kind of perfume by Lignum Aquilariae Resinatum preparation and preparation method thereof.
Background technology
Lignum Aquilariae Resinatum (agarwood) is traditional rare medicinal herbs of China, Japan, India and other countries in Southeast Asia and famous and precious natural perfume material, for thymelaeceae (Thymelaeaceae) plant Lignum Aquilariae Resinatum (Aquilaria agallocha Roxb.) or Lignum Aquilariae Resinatum Aquilaria sinensis (Lour.) Gilg.] contain the xylem of face cream.Ground such as the former main product India and Malaysia, China is called the import Lignum Aquilariae Resinatum; Provinces and regions such as latter's main product China Hainan, Guangdong and Guangxi are called homemade Lignum Aquilariae Resinatum or TUCHENXIANG.Lignum Aquilariae Resinatum is the spice of the common approval of the world's five big religions, is usually used in the religious rites, is used for tranquil people's thought and spirit.
Along with the raising of living standards of the people, perfume has become daily necessities gradually from a kind of luxury goods, has begun to come in huge numbers of families' the daily life.Though perfume on the market is of a great variety at present, increase novel perfume kind, particularly increase perfume with certain drug action, remain the problem that vast researcher is demanded urgently finishing in this area.
Summary of the invention
The purpose of this invention is to provide a kind of is that raw material is made with Lignum Aquilariae Resinatum, has Ligaloes perfumes of tranquilizing effect and preparation method thereof.
Ligaloes perfumes provided by the present invention, it is that the ethanol that 2.5~8.5 parts linaloe oil and parts by weight are 95~105 parts is formed by parts by weight; Wherein the optimum weight umber of linaloe oil is 4 parts, and the optimum weight umber of ethanol is 100 parts.
The concentration of described ethanol is 90%~100%.
A kind of method for preparing Ligaloes perfumes, it may further comprise the steps:
1) getting parts by weight is 2.5~8.5 parts linaloe oil, is dissolved in parts by weight and is in 95~105 parts the ethanol; The concentration of described ethanol is 90%~100%.
2) alcoholic solution with step 1 filters, and gained filtrate is Ligaloes perfumes.
The extracting method of described linaloe oil can be various, and for example steam distillation, organic solvent extraction method or supercritical carbon dioxide extraction method all can.
The technology of described steam distillation is: get the Lignum Aquilariae Resinatum raw material after the pulverizing, put it among the steam distillation device, utilize steam distillation to extract, the extract that obtains is linaloe oil.
The technology of described organic solvent extraction method is following two classes: A, get the Lignum Aquilariae Resinatum raw material after the pulverizing, add extremely just submergence medical material of organic solvent, adopt the water-bath reflow method to extract then, extract altogether 3 times, each 1~3h that extracts is obtaining linaloe oil behind the reclaim under reduced pressure organic solvent with extracting solution under the water-bath again; B, get the Lignum Aquilariae Resinatum raw material after the pulverizing, add organic solvent, adopt cold-maceration to extract then, extract altogether 3 times, extract 5~7d at every turn, again extracting solution is being obtained linaloe oil behind the reclaim under reduced pressure organic solvent under the water-bath to submergence medical material just.Organic solvent in the described organic solvent extraction method is: petroleum ether, normal hexane, chloroform, ether or ethyl acetate.
The technology of described supercritical carbon dioxide extraction method is: get the Lignum Aquilariae Resinatum raw material after the pulverizing, add 95% ethanol submergence medical material, place and carry out supercritical extraction after 24 hours, extraction conditions is: extraction column 26~28Mpa, and temperature is 30~35 ℃; Detached dowel 6~7Mpa, temperature is 55~60 ℃, CO 2Flow is 18~20L/h, and the extraction time is 1.5~2.5h, and resulting Lignum Aquilariae Resinatum extractum reuse organic solvent extraction obtains linaloe oil.
Result of the test shows that the Ligaloes perfumes of the inventive method preparation has tangible sedative-hypnotic effect.
The present invention has initiated the method for preparing perfume with Lignum Aquilariae Resinatum, and preparation technology is simple.The Ligaloes perfumes prescription that obtains is simple, and fragrant product are graceful, not only kept the original peculiar fragrance of Lignum Aquilariae Resinatum, the effect that also has tranquillizing and allaying excitement simultaneously, can play the effect of alleviating operating pressure, minding at rest quickly and easily to user, the scope of application is extensive, has the good prospect of marketing.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1, employing the inventive method prepare Ligaloes perfumes
Get Lignum Aquilariae Resinatum raw material 1.6Kg, put among the steam distillation device after it is pulverized, utilize steam distillation to extract, obtain extract linaloe oil 4.0g.After testing, mainly contain sesquiterpene compositions such as Lignum Aquilariae Resinatum spiral alcohol, α-agarofuran, baimuxinic acid, baimuxinal in the linaloe oil, and benzylacetone, to aromatic components such as methoxybenzyl benzylacetones, the sesquiterpene composition is the aroma component of linaloe oil.
The 4.0g linaloe oil is dissolved in concentration is 95%, weight is in the ethanol of 100g; Alcoholic solution is filtered, remove the insoluble matter in the solution, then gained filtrate is refrigerated to 5 ℃ and places 12h, more refrigerated alcoholic solution is filtered, the filtrate behind the secondary filter is returned to room temperature, promptly obtain Ligaloes perfumes, bottling promptly can be sold.
Embodiment 2, employing the inventive method prepare Ligaloes perfumes
Get Lignum Aquilariae Resinatum raw material 708g, it is pulverized the back add extremely just submergence medical material of low boiling petroleum ether (the boiling range temperature of petroleum ether is 30~60 ℃), adopt the water-bath reflow method to extract then, extract altogether 3 times, each 1~3h (present embodiment extracts 2h at every turn) that extracts obtains linaloe oil 8.5g with extracting solution again behind reclaim under reduced pressure petroleum ether solvent under the water-bath.After testing, mainly contain sesquiterpene compositions such as Lignum Aquilariae Resinatum spiral alcohol, α-agarofuran, baimuxinic acid, baimuxinal in the linaloe oil, and benzylacetone, to aromatic components such as methoxybenzyl benzylacetones, the sesquiterpene composition is the aroma component of linaloe oil.
The 8.5g linaloe oil is dissolved in concentration is 90%, weight is in the ethanol of 105g; Alcoholic solution is filtered, remove the insoluble matter in the solution, then gained filtrate is refrigerated to 5 ℃ and placed 12 hours, more refrigerated alcoholic solution is filtered, the filtrate behind the secondary filter is returned to room temperature, bottling promptly obtains Ligaloes perfumes.
Embodiment 3, employing the inventive method prepare Ligaloes perfumes
Get Lignum Aquilariae Resinatum raw material 500g, it is pulverized the back add extremely just submergence medical material of low boiling petroleum ether (the boiling range temperature of petroleum ether is 30~60 ℃), adopt cold-maceration to extract then, extract altogether 3 times, each 5~7d that extracts obtains linaloe oil 5.5g with extracting solution again behind reclaim under reduced pressure organic solvent under the water-bath.After testing, mainly contain sesquiterpene compositions such as Lignum Aquilariae Resinatum spiral alcohol, α-agarofuran, baimuxinic acid, baimuxinal in the linaloe oil, and benzylacetone, to aromatic components such as methoxybenzyl benzylacetones, the sesquiterpene composition is the aroma component of linaloe oil.
The 5.5g linaloe oil is dissolved in concentration is 90%, weight is in the ethanol of 96g; Alcoholic solution is filtered, remove the insoluble matter in the solution, then gained filtrate is refrigerated to 5 ℃ and placed 12 hours, more refrigerated alcoholic solution is filtered, the filtrate behind the secondary filter is returned to room temperature, bottling promptly obtains Ligaloes perfumes.
Embodiment 4, employing the inventive method prepare Ligaloes perfumes
Get the Lignum Aquilariae Resinatum raw material 643g after the pulverizing, add 95% ethanol submergence medical material, carry out supercritical extraction after placing 24h.Extraction conditions is: extraction column 28Mpa, and temperature is 33 ℃; Detached dowel 6.3Mpa, temperature is 55 ℃, CO 2Flow is 20L/h, and the extraction time is 2h.Lignum Aquilariae Resinatum extractum reuse low boiling petroleum ether (the boiling range temperature is 30~60 ℃) extraction that said method obtains obtains linaloe oil 2.5g.Through the GC/MS analyzing and testing, mainly contain sesquiterpene compositions such as Lignum Aquilariae Resinatum spiral alcohol, α-agarofuran, baimuxinic acid, baimuxinal in the linaloe oil, and benzylacetone, to aromatic components such as methoxybenzyl benzylacetones, the sesquiterpene composition is the aroma component of linaloe oil.
The 2.5g linaloe oil is dissolved in concentration is 100%, weight is in the ethanol of 95g; Alcoholic solution is filtered, remove the insoluble matter in the solution, then gained filtrate is refrigerated to 5 ℃ and places 12h, more refrigerated alcoholic solution is filtered, the filtrate behind the secondary filter is returned to room temperature, bottling promptly obtains Ligaloes perfumes.
Embodiment 5, Ligaloes perfumes are to the test of mice sedative-hypnotic effect
Adopt the Ligaloes perfumes (being designated as 1,2,3 respectively) of embodiment 1~3 preparation respectively mice to be carried out the test that pentobarbital sodium sub-threshold lull dosage influences, concrete process of the test is as follows:
Get totally 40 of Kunming mouses, be male, body weight is respectively 18~22g/ only; With the mice random packet, 10 every group, totally four groups, each is organized in the constant temperature box of packing into respectively (31 ± 0.5 ℃).With concentration be 95% ethanol in contrast, the Ligaloes perfumes of embodiment 1~3 preparation is respectively charged in the perfume vial of 10mL band sprayer unit with contrast ethanol, then it is sprayed into respectively and be equipped with in the constant temperature box of respectively organizing mice, straying quatity is a 0.1mL/10g mice body weight.Behind the 5min, each group mice is carried out lumbar injection pentobarbital sodium solution 30mg/kg.Observe then, reaching the above person of 1min with mice righting reflex loss in the 30min is sleeping index, observes sleeping number of animals.The result is as shown in table 1.The result shows: the Ligaloes perfumes of embodiment 1~3 preparation has the effect to the mice tranquilizing soporific.
Table 1 Ligaloes perfumes is to the result of the test of mice pentobarbital sodium sub-threshold lull dosage influence
Group The contrast of 95% ethanol Ligaloes perfumes 1 Ligaloes perfumes 2 Ligaloes perfumes 3
Dosage (mL/10g) 0.1 0.1 0.1 0.1
Test Mus number (only) 10 10 10 10
Sleep Mus number (only) 3 8 * 7 * 7 *
Annotate: compare with matched group, *P<0.05, i.e. significant difference.
Embodiment 6, Ligaloes perfumes are to the test of mice sedative-hypnotic effect
The Ligaloes perfumes (being designated as 1,2,3 respectively) that adopts embodiment 1~3 to prepare carries out the test of the pentobarbital sodium influence length of one's sleep respectively to mice, concrete process of the test is as follows:
Get totally 40 of Kunming mouses, be male, body weight is respectively 18~22g/ only; With the mice random packet, 10 every group, totally four groups, each is organized in the constant temperature box of packing into respectively (31 ± 0.5 ℃).With concentration be 95% ethanol in contrast, the Ligaloes perfumes of embodiment 1~3 preparation is respectively charged in the perfume vial of 10mL band sprayer unit with contrast ethanol, then it is sprayed into respectively and be equipped with in the constant temperature box of respectively organizing mice, straying quatity is a 0.1mL/10g mice body weight.After 5 minutes, each group mice is carried out lumbar injection pentobarbital sodium solution 45mg/kg, record mice righting reflex loss to righting reflex recovers required time, i.e. the length of one's sleep.The meansigma methods of result of the test of each group mice is carried out the score of t primary system analyse, the result is as shown in table 2.The result shows: the Ligaloes perfumes of embodiment 1~3 preparation has the effect to the mice tranquilizing soporific.
Table 2 Ligaloes perfumes is to the result of the test of mice pentobarbital sodium dosage sleep period influence above threshold (x ± s)
Group The contrast of 95% ethanol Ligaloes perfumes 1 Ligaloes perfumes 2 Ligaloes perfumes 3
Dosage (mL/10g) 0.1 0.1 0.1 0.1
Test Mus number (only) 10 10 10 10
The length of one's sleep (min) 30.67+10.27 42.51+11.52* * 46.78+15.32** 45.31+12.47**
Annotate: compare with matched group, * * P<0.01, promptly difference is extremely remarkable.
The result of the test of comprehensive the foregoing description 5,6 shows that the Ligaloes perfumes that the inventive method prepares has tangible sedative-hypnotic effect.

Claims (10)

1. Ligaloes perfumes, it is that the ethanol that 2.5~8.5 parts linaloe oil and parts by weight are 95~105 parts is formed by parts by weight.
2. Ligaloes perfumes as claimed in claim 1 is characterized in that: described Ligaloes perfumes is that the ethanol that 4 parts linaloe oil and parts by weight are 100 parts is formed by parts by weight.
3. Ligaloes perfumes as claimed in claim 1 or 2 is characterized in that: the concentration of described ethanol is 90%~100%.
4. method for preparing Ligaloes perfumes, it may further comprise the steps:
1) getting parts by weight is 2.5~8.5 parts linaloe oil, is dissolved in parts by weight and is in 95~105 parts the ethanol;
2) alcoholic solution with step 1 filters, and gained filtrate is Ligaloes perfumes.
5. method as claimed in claim 4 is characterized in that: the concentration of described ethanol is 90%~100%.
6. as claim 4 or 5 described methods, it is characterized in that: the extracting method of described linaloe oil is steam distillation, organic solvent extraction method or supercritical carbon dioxide extraction method.
7. method as claimed in claim 6 is characterized in that: the technology of described steam distillation is: get the Lignum Aquilariae Resinatum raw material after the pulverizing, put it among the steam distillation device, utilize steam distillation to extract, the extract that obtains is linaloe oil.
8. method as claimed in claim 6, it is characterized in that: the technology of described organic solvent extraction method is selected from one of the following: A, get the Lignum Aquilariae Resinatum raw material after the pulverizing, add extremely just submergence medical material of organic solvent, adopt the water-bath reflow method to extract then, extract altogether 3 times, each 1~3h that extracts is obtaining linaloe oil behind the reclaim under reduced pressure organic solvent with extracting solution under the water-bath again; B, get the Lignum Aquilariae Resinatum raw material after the pulverizing, add organic solvent, adopt cold-maceration to extract then, extract altogether 3 times, extract 5~7d at every turn, again extracting solution is being obtained linaloe oil behind the reclaim under reduced pressure organic solvent under the water-bath to submergence medical material just.
9. method as claimed in claim 8 is characterized in that: the organic solvent in the described organic solvent extraction method is: petroleum ether, normal hexane, chloroform, ether or ethyl acetate.
10. method as claimed in claim 6, it is characterized in that: the technology of described supercritical carbon dioxide extraction method is: get the Lignum Aquilariae Resinatum raw material after the pulverizing, the ethanol submergence medical material of adding 95%, place and carry out supercritical extraction after 24 hours, extraction conditions is: extraction column 26~28Mpa, and temperature is 30~35 ℃; Detached dowel 6~7Mpa, temperature is 55~60 ℃, CO 2Flow is 18~20L/h, and the extraction time is 1.5~2.5h, and resulting Lignum Aquilariae Resinatum extractum reuse organic solvent extraction obtains linaloe oil.
CN 200710121128 2007-08-30 2007-08-30 Ligaloes perfumes and method of producing the same Active CN101129316B (en)

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CN101829245A (en) * 2010-05-17 2010-09-15 中国医学科学院药用植物研究所海南分所 Compound agilawood essential oil
CN101991715A (en) * 2010-10-28 2011-03-30 广东省微生物研究所 Aquilaria sinensis fruit skin extract and preparation method and application thereof
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