CN111423937A - Aquilaria agallocha fireless aromatherapy liquid and preparation method and application thereof - Google Patents
Aquilaria agallocha fireless aromatherapy liquid and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/83—Thymelaeaceae (Mezereum family), e.g. leatherwood or false ohelo
- A61K36/835—Aquilaria
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/015—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone
- A61L9/04—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone using substances evaporated in the air without heating
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P25/00—Drugs for disorders of the nervous system
- A61P25/20—Hypnotics; Sedatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- Natural Medicines & Medicinal Plants (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention provides agilawood fire-free aromatherapy liquid and a preparation method and application thereof, and relates to the technical field of plant extraction and aromatherapy liquid. The invention relates to agilawood fireless aromatherapy liquid which comprises the following raw materials in percentage by mass: 75-89% of agilawood hydrosol, 5-10% of perfume alcohol, 0.01-0.3% of carrier oil, 0.01-0.3% of emulsifier and the balance of deionized water. The agilawood hydrolat is prepared by the methods of pretreatment, extraction, molecular cutting, distillation and the like. The agilawood fireless fragrant fumigant disclosed by the invention is low in impurity content, good in permeability, fragrant and pure in fragrance, and has the effect of helping sleep.
Description
Technical Field
The invention relates to the technical field of plant extraction and aromatherapy liquid, in particular to an agilawood fire-free aromatherapy liquid and a preparation method and application thereof.
Background
Aquilaria agallocha is a resin-containing wood produced by plants of the genus Aquilaria of the family Thymelaeaceae after being injured, and is named because it is fragrant and sinks in water. Since ancient times, eaglewood is both a precious herb and an advanced spice. Lignum Aquilariae Resinatum has effects of lowering qi, warming middle warmer, warming kidney, invigorating qi, and tranquilizing, and can be used for treating chest distress, angina pectoris, dyspepsia, etc. In ancient times, agilawood is used in many countries as a famous and precious spice special for hospitalizing visitors, and is often used as an aromatherapy. In modern times, along with the development and popularization of the incense channel culture, the agilawood incense stick and the agilawood daily chemical products are generally accepted.
The agilawood incense stick is a space incense product prepared by adding auxiliary materials such as nanmu barks into agilawood powder, has practical effects of exorcizing evil spirits, removing dirt, restoring consciousness, preserving health and the like, needs open fire in a stove or directly burns in normal use, has certain potential safety hazard to the environment, a user needs to pay attention to the burning condition of the agilawood incense stick and the cleaning of the used tool and the environment all the time, and smoke generated by burning also brings discomfort to the user.
The agilawood hydrolat is a distillation stock solution separated in the process of extracting essential oil from agilawood, contains a small amount of agilawood essential oil, is prepared into agilawood aromatherapy liquid, can be used as space incense, and has the effects of soothing the nerves and soothing the heart. However, the agilawood hydrolat adopted by the existing agilawood aromatherapy liquid has high impurity content, and the problems of sour taste, insufficient aroma and different aroma types easily occur after long-time storage, and meanwhile, certain potential safety hazards of power utilization also exist.
Disclosure of Invention
Therefore, in order to solve the above problems, a need exists for providing an agilawood fireless aromatherapy liquid, which is prepared from agilawood hydrolat with low impurity content, good permeability and pure fragrance as a raw material, does not need open fire and electricity, does not generate smoke, does not have pungent smell, and has the efficacy of helping sleep after long-term use.
The agilawood fireless aromatherapy liquid comprises the following raw materials in percentage by mass:
the agilawood hydrolat is prepared by the following method:
pretreatment: pulverizing lignum Aquilariae Resinatum, and sieving to obtain lignum Aquilariae Resinatum granule;
extraction: using supercritical CO2Extracting lignum Aquilariae Resinatum granule by method or water distillation method to obtain lignum Aquilariae Resinatum extract;
molecular cleavage: cutting the agilawood extract by using a molecular distillation device, wherein the cutting vacuum degree is 0.01-1000Pa, obtaining first-section, middle-section and tail-section products, discarding the first-section and tail-section products, and keeping the middle-section product; wherein, the first section product refers to the product from the beginning of accurate cutting for 10-30min, the last section product refers to the product from the end of accurate cutting for 90-120min, and the middle section product refers to the product between the first section and the last section;
and (3) distillation: and mixing the middle section product with water, wherein the mass ratio of the middle section product to the deionized water is 1: (1000-4000), and performing continuous distillation by gradient heating to obtain a saturated solution, namely the agilawood hydrosol.
The agilawood fire-free aromatherapy liquid adopts agilawood hydrolat which has fewer impurities than the agilawood extract on the market, and the inventor finds that the impurities are not removed when the agilawood extract is prepared by the traditional method, but are extracted or extracted indiscriminately, so that the obtained agilawood extract contains impurities such as water, acetic acid, lactic acid, resin and the like, and is easy to deteriorate in the storage process to generate sour taste to influence the fragrance type. The intermediate product mainly contains sesquiterpene, linalol, aquilaria aldehyde and other components which have pleasant fragrance and are important fragrance substances in the linaloe product, and the stepwise distillation is adopted, so that the linaloe essential oil is prevented from being independently distilled at a certain temperature, the solubility of the linaloe essential oil in water is increased, the linaloe pure water is saturated, the fragrance is more accurate, and the fragrance is more pure; therefore, the aromatherapy liquid prepared by the agilawood hydrolat also has the advantages of less impurities and pure fragrance; the agilawood hydrosol is matched with other raw materials to prepare the aromatherapy liquid, so that the aromatherapy liquid is not easy to deteriorate to generate sour, is warm and non-irritant when used, and has the effects of soothing nerves and helping sleep.
It is understood that the perfume alcohol mentioned above is deodorized alcohol, which is di-dealdehydized absolute ethyl alcohol applied to food or cosmetics, and is also called odorless ethyl alcohol.
In one embodiment, the carrier oil is selected from: one or two of sweet almond oil and fractionated coconut oil; the emulsifier is selected from: one or more of tween-20, tween-60 and tween-80. Sweet almond oil or fractionated coconut oil is used as carrier oil to perform pre-blending assistance on the sleep-assisting effect of the agalloch eaglewood fireless aromatherapy, and the obtained agalloch eaglewood fireless aromatherapy liquid has the advantages of pure fragrance, mildness, no stimulation, nerve calming and sleep assisting.
In one embodiment, the water is deionized water.
In one embodiment, in the pretreatment step, the agilawood is selected from a part of the agilawood with the age of more than 2 years, which well forms the agilawood, and the agilawood is crushed and sieved by a 20-60-mesh sieve.
In one embodiment, the density of the agilawood extract is 0.8-1.2 g/cm3。
In one embodiment, the extraction step employs supercritical CO2Extracting under 18-40MPa at 50-65 deg.C for 90-120min at 50-300L/min.
In one embodiment, the extraction step is water distillation extraction, specifically: mixing the components in a mass ratio of 1: (5-20) mixing the lignum Aquilariae Resinatum granules with water, heating to 90-100 deg.C, under 90-110kPa for 1440min, and distilling for 240-.
In one embodiment, in the molecular cutting step, the film-scraping rotation speed of the first column of the molecular distillation device is 100-. Wherein the first root column is used for separating water and small molecular impurities from the agilawood extract, and the second root column is used for separating macromolecular resin and tree wax from the agilawood extract. The above molecular cutting temperature is favorable for separating and collecting each component.
In one embodiment, in the molecular cutting step, the film scraping rotation speed of the first column of the molecular distillation device is 220r/min, the cutting temperature is 100 ℃, the collecting temperature is 35 ℃, the film scraping rotation speed of the second column is 220r/min, the cutting temperature is 135 ℃, and the collecting temperature is 15 ℃.
In one embodiment, the molecular distillation apparatus is an MDS-80 wiped film molecular distillation apparatus. The MDS-80 wiped film type molecular distillation device is small wiped film type molecular distillation device equipment produced by Hieroli Biotechnology limited, Guangzhou.
In one embodiment, the gradient heating is three-stage heating, the first stage heating is increased to 70-80 ℃ at a speed of 5-15 ℃/min, the second stage heating is increased to 90-95 ℃ at a speed of 1-5 ℃/min, and the third stage heating is increased to 97-105 ℃ at a speed of 0.5-1.5 ℃/min.
In one embodiment, the gradient heating is three-stage heating, the first stage heating is increased to 75 ℃ at a speed of 10 ℃/min, the second stage heating is increased to 95 ℃ at a speed of 3 ℃/min, and the third stage heating is increased to 100 ℃ at a speed of 1 ℃/min.
The invention also provides a preparation method of the agilawood fireless aromatherapy liquid, which comprises the following steps:
s1, uniformly mixing the carrier oil and the emulsifier to obtain water-soluble carrier oil;
s2, mixing lignum Aquilariae Resinatum hydrosol and ethanol, adding the above water soluble carrier oil, mixing, adding water, sealing, and packaging to obtain the final product.
The fire-free agilawood incense liquid prepared by the method has the advantages of pure fragrance, mildness, no stimulation, and nerve calming and sleep aiding.
In one embodiment, the step S1 specifically includes: mixing carrier oil and emulsifier, and stirring at 20-35 deg.C for 10-20min to obtain water soluble carrier oil.
In one embodiment, the step S2 specifically includes: mixing lignum Aquilariae Resinatum hydrosol and ethanol, heating to 38-42 deg.C, adding the above water soluble carrier oil under stirring, stirring for 8-12min, adding water, stirring, sealing, and packaging to obtain the final product.
Compared with the prior art, the invention has the following beneficial effects:
the agilawood pure dew adopted by the agilawood fireless fragrant liquid has fewer impurities compared with the agilawood extract on the market, and the inventor finds that the impurities are not removed but are extracted or extracted indiscriminately when the agilawood extract is prepared by the traditional method, so that the obtained agilawood extract contains impurities such as water, acetic acid, lactic acid, resin and the like, and is easy to deteriorate in the storage process, and sour taste affects the fragrance type, the agilawood pure dew in the invention adopts molecular distillation to remove the first-stage product and the last-stage product, and the detection finds that the first-stage product mainly contains water, lactic acid, acetic acid, tannin and other small molecular impurities, and the impurities can cause the agilawood essential oil to generate sour taste, bitter taste and other bad odors and affect the stability of the agilawood product, the last-stage product mainly contains resin and macromolecular impurities contained in the agilawood, and the impurities have low or no fragrance, the intermediate product mainly contains sesquiterpene, linalol, aquilaria aldehyde and other components which have pleasant fragrance and are important fragrance substances in the linaloe product, and the stepwise distillation is adopted, so that the linaloe essential oil is prevented from being independently distilled at a certain temperature, the solubility of the linaloe essential oil in water is increased, the linaloe pure water is saturated, the fragrance is more accurate, and the fragrance is more pure; therefore, the fireless fragrant liquid prepared by the agilawood hydrolat also has the advantages of less impurities and pure fragrance; the agilawood hydrosol is matched with other raw materials to prepare the agilawood fireless incense liquid, so that the agilawood fireless incense liquid is not easy to deteriorate to generate sour, is warm and non-irritant when used, and has the effects of soothing the nerves and helping sleep.
Drawings
FIG. 1 shows the radar fingerprint spectrum for evaluating the odor of Aquilaria sinensis.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the preferred embodiments. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
The agilawood hydrolat is prepared by the following preparation method:
(1) pretreatment: selecting agilawood raw materials, crushing agilawood, and sieving with a 40-mesh sieve to obtain agilawood particles.
(2) Extraction: placing lignum Aquilariae Resinatum granule in supercritical CO2In the equipment, the system pressure is set to be 28MPa, the system flow is set to be 210L/min, the extraction temperature is set to be 60 ℃, and the extraction time is set to be 120min, so that the agilawood extract is obtained.
(3) Molecular cleavage: and (3) using an MDS-80 molecular cutting machine to accurately cut the incense sections of the agilawood paste extract, wherein the cutting vacuum degree is 0.1Pa, the film scraping rotation speed of the column 1 is 200r/min, the film scraping rotation speed of the column 2 is 200r/min, the cutting temperature of the column 1 is 100 ℃, the cutting temperature of the column 2 is 135 ℃, the collecting temperature of the column 1 is 35 ℃, the collecting temperature of the column 2 is 15 ℃, the first section products and the tail section products are discarded, the middle section products are reserved, and the middle section products are the agilawood essential oil.
(4) And (3) distillation: adding 100g of the obtained agilawood essential oil and 140kg of purified water into a continuous distillation device, heating and continuously distilling in a staged manner, wherein the temperature of the first stage is increased to 75 ℃ at the speed of 10 ℃/min, the temperature of the second stage is increased to 95 ℃ at the speed of 3 ℃/min, the temperature of the third stage is increased to 100 ℃ at the speed of 1 ℃/min, keeping boiling for 60min, and collecting steam cooling liquid, namely agilawood hydrosol.
Example 2
The agilawood hydrolat is prepared by the following preparation method:
(1) pretreatment: selecting agilawood raw materials, crushing agilawood, and sieving with a 50-mesh sieve to obtain agilawood particles.
(2) Extraction: placing lignum Aquilariae Resinatum granule in supercritical CO2In the equipment, the system pressure is set to be 25MPa, the system flow is set to be 210L/min, the extraction temperature is set to be 55 ℃, the extraction time is set to be 120min, and the agilawood paste extract is obtained.
(3) Molecular cleavage: and (3) using an MDS-80 molecular cutting machine to accurately cut the incense sections of the agilawood paste extract, wherein the cutting vacuum degree is 1Pa, the film scraping rotation speed of the column 1 is 210r/min, the film scraping rotation speed of the column 2 is 210r/min, the cutting temperature of the column 1 is 90 ℃, the cutting temperature of the column 2 is 120 ℃, the collecting temperature of the column 1 is 30 ℃, the collecting temperature of the column 2 is 12 ℃, the first section product and the tail section product are discarded, the middle section product is reserved, and the middle section product is the agilawood essential oil.
(4) And (3) distillation: adding 100g of the obtained agilawood essential oil and 150kg of purified water into a continuous distillation device, heating and continuously distilling in a staged manner, wherein the temperature of the first stage is increased to 75 ℃ at the speed of 5 ℃/min, the temperature of the second stage is increased to 95 ℃ at the speed of 5 ℃/min, the temperature of the third stage is increased to 100 ℃ at the speed of 1.5 ℃/min, keeping boiling for 50min, and collecting steam cooling liquid, namely agilawood hydrosol.
Example 3
The agilawood hydrolat is prepared by the following preparation method:
(1) pretreatment: selecting agilawood raw materials, crushing agilawood, and sieving with a 60-mesh sieve to obtain agilawood particles.
(2) Extraction: placing lignum Aquilariae Resinatum granule in supercritical CO2In the equipment, the system pressure is set to be 30MPa, the system flow is set to be 210L/min, the extraction temperature is 65 ℃, and the extraction time is set to be 120min, so that the agilawood paste extract is obtained.
(3) Molecular cleavage: and (3) using an MDS-80 molecular cutting machine to accurately cut the incense sections of the agilawood paste extract, wherein the cutting vacuum degree is 10Pa, the film scraping rotation speed of the column 1 is 230r/min, the film scraping rotation speed of the column 2 is 230r/min, the cutting temperature of the column 1 is 100 ℃, the cutting temperature of the column 2 is 140 ℃, the collecting temperature of the column 1 is 40 ℃, the collecting temperature of the column 2 is 20 ℃, the first section product and the tail section product are discarded, the middle section product is reserved, and the middle section product is the agilawood essential oil.
(4) And (3) distillation: adding 100g of the obtained agilawood essential oil and 160kg of purified water into a continuous distillation device, heating and continuously distilling in a staged manner, wherein the temperature of the first stage is increased to 75 ℃ at the speed of 15 ℃/min, the temperature of the second stage is increased to 95 ℃ at the speed of 1 ℃/min, the temperature of the third stage is increased to 100 ℃ at the speed of 0.5 ℃/min, keeping boiling for 60min, and collecting steam cooling liquid, namely agilawood hydrosol.
Example 4
The agilawood hydrolat is prepared by the following preparation method:
(1) pretreatment: selecting agilawood raw materials, crushing agilawood, and sieving with a 40-mesh sieve to obtain agilawood particles.
(2) Extraction: placing agilawood particles in a water distillation device, adding deionized water under the system pressure of 90-110kPa, wherein the material-liquid ratio is 1: 20, extracting for 60min to obtain lignum Aquilariae Resinatum extract.
(3) Molecular cleavage: and (3) using an MDS-80 molecular cutting machine to accurately cut the incense sections of the agilawood extract, wherein the cutting vacuum degree is 0.1Pa, the film scraping rotation speed of the column 1 is 220r/min, the film scraping rotation speed of the column 2 is 220r/min, the cutting temperature of the column 1 is 100 ℃, the cutting temperature of the column 2 is 135 ℃, the collecting temperature of the column 1 is 35 ℃, the collecting temperature of the column 2 is 15 ℃, the first section products and the tail section products are discarded, the middle section products are reserved, and the middle section products are the agilawood essential oil.
(4) And (3) distillation: adding 100g of the obtained agilawood essential oil and 140kg of purified water into a continuous distillation device, heating and continuously distilling in a staged manner, wherein the temperature of the first stage is increased to 75 ℃ at the speed of 10 ℃/min, the temperature of the second stage is increased to 95 ℃ at the speed of 3 ℃/min, the temperature of the third stage is increased to 100 ℃ at the speed of 1 ℃/min, keeping boiling for 60min, and collecting steam cooling liquid, namely agilawood hydrosol.
Example 5
The fire-free agilawood aromatherapy liquid is prepared by the following method:
s1: weighing 1kg of sweet almond oil, pouring the sweet almond oil into a stirring container, adding 0.15kg of Tween-80 into the container, and uniformly stirring for 10-20 minutes at normal temperature to prepare water-soluble carrier oil for later use;
s2: 850g of the agalloch eaglewood hydrolat in example 1 and 80g of perfume alcohol are weighed into a stirring container, heated to 40 ℃ and kept at a constant temperature, 2g of water-soluble carrier oil is added while stirring, after stirring for 10 minutes, 68g of deionized water is added, the mixture is uniformly stirred, and the mixture is sealed and filled to obtain the agalloch eaglewood flameless incense liquid.
Example 6
An agalloch eaglewood fire-free incense liquid is different from the incense liquid of the embodiment 5 in that the step S2 is: weighing 750g of the agalloch eaglewood hydrolat in the embodiment 1 and 50g of perfume alcohol into a stirring container, heating to 40 ℃ and keeping the temperature constant, adding 1g of water-soluble carrier oil while stirring, stirring for 10 minutes, adding 199g of deionized water to constant volume, stirring uniformly, sealing and filling to obtain the agalloch eaglewood fireless fumigation solution.
Example 7
An agalloch eaglewood fire-free incense liquid is different from the incense liquid of the embodiment 5 in that the step S2 is: weighing 890g of the agalloch eaglewood hydrolat in example 1 and 100g of perfume alcohol into a stirring container, heating to 40 ℃ and keeping the temperature constant, adding 3g of water-soluble carrier oil while stirring, stirring for 10 minutes, adding 7g of deionized water, stirring uniformly, sealing and filling to obtain the agalloch eaglewood flameless incense liquid.
Comparative example 1
An Aquilaria sinensis distillate, commercially available Aquilaria sinensis distillate 1.
Comparative example 2
An Aquilaria sinensis distillate, commercially available Aquilaria sinensis distillate 2.
Comparative example 3
An Aquilaria sinensis distillate, commercially available Aquilaria sinensis distillate 3.
Comparative example 4
The difference between the agilawood hydrolat and the example 4 is that in the preparation method of the agilawood hydrolat, the step 4) is as follows: adding 100g of the obtained lignum Aquilariae Resinatum essential oil and 140kg of purified water into a distillation device, directly heating to 100 deg.C, maintaining for 60min, and collecting steam cooling liquid during the period to obtain lignum Aquilariae Resinatum hydrolat 4.
Comparative example 5
An agilawood fire-free incense liquid is different from that in example 5 in that the commercially available agilawood hydrolat 1 of comparative example 1 is adopted, and the commercially available agilawood hydrolat 1 is obtained by extracting agilawood particles through a water distillation method.
Comparative example 6
An agilawood incense liquid without fire is different from that in example 5 in that the commercially available agilawood hydrolat 2 of comparative example 2 is adopted, and the commercially available agilawood hydrolat 2 is obtained by extracting agilawood particles through a water distillation method.
Comparative example 7
An agilawood incense liquid without fire is different from that in example 5 in that the commercially available agilawood hydrolat 3 of comparative example 3 is adopted, and the commercially available agilawood hydrolat 3 is obtained by extracting agilawood particles through a water distillation method.
Experimental example 1
1. And analyzing the components of the agilawood hydrosol.
Instruments and reagents: TRACE DSQ GC-MS gas chromatography-mass spectrometer (Finnggan, USA); ethyl acetate (chromatographically pure, Tianjin City Koimeu chemical reagent Co., Ltd.)
Sample preparation: 0.5ml of the Chinese eaglewood hydrolat in the example and 0.5ml of the Chinese eaglewood hydrolat in the comparative example are taken respectively, mixed and dissolved with 0.5ml of ethyl acetate by ultrasound, and dried by anhydrous sodium sulfate to obtain colorless and clear samples.
Chromatographic conditions are as follows:
(1) column DB-5MS (30m × 0.25mm, 0.25 μm, Agilent, USA) elastic quartz capillary column:
(2) the parameters are that the temperature of a sample inlet is 270 ℃, GC carrier gas is high-purity helium (the purity is more than 99.9 percent), the carrier gas is in a constant flow mode, the volume flow is 1.0ml/min, the sample injection amount is 1 mu L, and the split ratio is 10: 1.
(3) Temperature programming: the initial temperature was 90 deg.C, held for 2min, ramped to 130 deg.C at a rate of 10 deg.C per minute, then ramped to 155 deg.C at a rate of 0.3 deg.C per minute, ramped to 180 deg.C at a rate of 5 deg.C per minute, ramped to 250 deg.C at a rate of 10 deg.C per minute, held for 20min, and ramped to 260 deg.C at a rate of 10 deg.C per minute, held for 30 min.
MS scanning range is 0.0-500.0, ionization mode E1, voltage is 70eV, ion source temperature is 250 ℃, transmission line temperature is 250 ℃, scanning speed is 500amu/s, and detection mode: positive ion mode, solvent delay time: 2min, gradient program see Table 1.
TABLE 1 GC-MS gradient temperature program
| Rate (. degree.C./min) | Temperature (. degree.C.) | Retention time (min) | |
| Stage 1 | -- | 90 | 2 |
| Stage 2 | 10.0 | 130 | 0 |
| Stage 3 | 0.3 | 155 | 0 |
| Stage 4 | 5.0 | 180 | 0 |
| Stage 5 | 10.0 | 250 | 20 |
| |
10.0 | 260 | 30 |
2. GC-MS analysis and identification of agilawood hydrolat
Analyzing the agilawood hydrolat by using a capillary chromatography method, measuring the percentage content of each component by using a normalization method, retrieving by using a computer NIST mass spectrum database, and carrying out qualitative analysis by combining with an organic compound mass spectrum fracture rule to determine the name of the compound in the agilawood hydrolat, wherein the relative percentage content of the characteristic components of the agilawood hydrolat in the embodiment and the comparative example is shown in Table 2:
TABLE 2 comparison of characteristic components of Aquilaria agallocha hydrolat
As can be seen from the above table, the contents of characteristic components of the agarwood hydrolat of the other experimental examples and comparative examples all meet the reference standard except that the longifolene content of comparative example 3 is lower than the standard. The contents of the linalool, the agarofuran and the guaiol in the example 1 are obviously higher than those of the other examples and comparative examples, and it can be presumed that the application effect of the linalool hydrolat in the example 1 in moisturizing, moisturizing and tranquilizing the skin in daily chemical products is better. Example 1 is the best process condition by combining comparative example 1, example 2 and example 3. The agilawood hydrolat of the comparative example 1, the comparative example 2 and the comparative example 3 has larger content difference of characteristic components, which indicates that the quality difference of the agilawood hydrolat products in the market is larger. The index of the agilawood hydrolat in the embodiment 4 is slightly higher than that of the agilawood hydrolat in the comparative example 4, which shows that the quality of the agilawood hydrolat is improved by stepwise heating.
Experimental example 2
And testing the in-vitro antioxidant activity of the agilawood hydrosol.
The agilawood hydrolat in the examples and the comparative examples was respectively subjected to radical scavenging ability test by the DPPH method:
the DPPH was diluted to 6.5 × 10 with absolute ethanol-5100 mu L of the agilawood hydrolat example 1 and the agilawood hydrolat at comparative example 1 and 100 mu L of the DPPH solution are respectively added into a 96-well plate, mixed evenly, measured at intervals of two minutes by an enzyme-labeling instrument to measure the light absorption value at 517nm, and the clearance rate is calculated according to the following formula:
clearance rate ═ 1- (A)1-A2)/A0]×100％
In the formula, A0Absorbance of DPPH solution 100. mu. L + distilled water 100. mu. L, A1The absorbance of DPPH solution 100 mu L + Aquilaria agallocha hydrol 100 mu L, A2The absorbance of the agilawood hydrolat 100 mu L + absolute ethyl alcohol 100 mu L is shown.
The test results are shown in table 3:
TABLE 3 test data table of the antioxidant activity of Aquilaria agallocha in vitro
From the above results, it can be seen that example 1 reached a maximum radical clearance of 24.8% and remained stable at 40 minutes, and example 4 reached a maximum radical clearance of 20.6% and remained stable at 22 minutes. While comparative example 1 reached 10.4% and remained stable at 26 minutes for the highest radical clearance, comparative example 2 reached 16.7% and remained stable at 18 minutes for the highest radical clearance, and comparative example 3 reached 6.7% and remained stable at 20 minutes for the highest radical clearance. In comprehensive comparison, the free radical scavenging ability of the example 1 is stronger than that of other experimental objects, and the agilawood hydrolat disclosed by the invention has the potential of developing natural antioxidants.
Experimental example 3
And evaluating and testing the odor of the agilawood hydrosol.
In the experiment, blind evaluation is carried out on the agilawood hydrolat of the embodiment and the comparative example according to 12 professional fragrance smellers, 8 representative fragrance descriptors are screened out, the fragrance smellers respectively score each descriptor by an integer of 0-10 for the agilawood hydrolat, wherein 0 represents that the odor is not smelled, 10 represents that the odor is strongest, the obtained scores are averaged to obtain the final score, the result is shown in table 4, and the radar fingerprint spectrum is shown in fig. 1.
TABLE 4 evaluation data of odor of Aquilaria agallocha hydrosol
From the above results, the agilawood hydrolat example 1 has the highest scores of the drug flavor, the sweet flavor, the spicy flavor, the costustoot, the bitter flavor and the cool flavor, wherein the drug flavor, the spicy flavor and the cool flavor are positive indexes for evaluating the quality of the agilawood, and the result shows that the quality of the agilawood hydrolat example 1 is the best. Meanwhile, based on the molecular distillation in the step (3) in the embodiment 1, the first-stage small molecular impurities are removed, the water boiling flavor of the agilawood hydrolat product is reduced, the tail-stage resin and other macromolecular impurities are removed, the wax flavor of the agilawood hydrolat product is reduced, and the obtained agilawood hydrolat flavor is more pure.
Experimental example 4
The agilawood fire-free aromatherapy liquid sleep-aiding effect test (CPC sleep monitoring method) comprises the following parts by weight.
The agilawood fireless aromatherapy liquid in the embodiment 5 is taken for sleep aid effect test, a cardiopulmonary coupling analysis (CPC) sleep quality evaluation analysis system is adopted in the experiment, and for 30 experimental subjects with insomnia or difficult sleep onset performance, the agilawood fireless aromatherapy liquid is used for trying to improve the sleep quality of the experimental subjects and making corresponding evaluation.
(1) Clinical data
Observing that 30 cases come from various communities in Guangzhou, all have symptoms of insomnia or difficulty in falling asleep, and voluntarily participating in the sleep improvement test, wherein 11 cases of males and 19 cases of females have the age of 19-55 years and have insomnia chief complaints, the score of a Pesburg sleep index scale (PSQI) is more than or equal to 7 points, the sleeping difficulty is taken as the main factor, and the occurrence frequency per week is more than or equal to 3 times; eliminating systemic diseases such as pain, fever, postoperative, and external environmental interference; patients with serious primary diseases such as cardiovascular diseases, lung diseases, liver diseases, kidney diseases, hemopoietic systems and the like and psychosis are excluded.
(2) Agalloch eaglewood fireless fragrant fumigation sleep-aiding liquid and equipment device
The agilawood fireless aromatherapy liquid, the reed fragrance expanding device and the CPC sleep quality evaluation analysis system.
(3) Evaluation method
Before testing, the observation cases are evaluated for the sleep quality of the conventional CPC, and the average time to fall asleep is taken as a reference value.
During testing, the agalloch eaglewood fireless aromatherapy liquid is added into the reed fragrance diffusion device, the reed fragrance diffusion device is placed at the position of about 30cm of the level of the pillow, the distance from the head is about 50cm, the user can get on the bed every night according to the daily work and rest time, the time of getting on the bed is recorded, the user can observe a case to wear the CPC sleep detector, the user can sleep when lying still, the user can feel fragrance, the user can adjust breath, and the thoughts are eliminated. And (5) recording the getting-up time after getting up the next day, and taking down the detection instrument.
(4) Evaluation results
The evaluation results are shown in table 5:
TABLE 5 Aquilaria agallocha fireless aromatherapy liquid example 5 reduction of time to sleep after treatment of insomnia
Comparison of sleep time before and after using the agilawood fire-free aromatherapy liquid of example 5: after the agilawood fireless incense liquid is used, the sleep time of the case with difficulty in falling asleep is obviously reduced compared with that before the evaluation. In 30 cases, the sleep time of 6 cases with difficult sleep is less than 30 minutes after using the agilawood fireless fragrant fumigant. The sleep time of 13 cases with difficult sleep is greatly reduced after the agilawood fireless fragrant fumigant is used, and the reduction is more than or equal to 80 percent. In 2 cases of difficult falling asleep, the falling asleep time after using the agalloch eaglewood fireless fragrant liquid was not obviously changed, and the evaluation was invalid. The average of the fall-off rates of time to sleep was 80.8%. In conclusion, the agilawood fireless fragrant liquid has definite effects of helping sleep and shortening the sleep time.
The same test of the sleeping aid effect of the agilawood fireless aromatic liquid of example 6, example 7, comparative example 5, comparative example 6 and comparative example 7 was carried out, and the results are shown in table 6:
TABLE 6 sleep-aiding effect test and comparison of lignum Aquilariae Resinatum fireless aromatherapy liquid
Wherein, the composition is obviously effective, and the time of falling asleep is less than 30 minutes or is reduced by more than 80 percent; the effect is achieved, and the time for falling asleep is reduced by over 50 percent; no effect, no obvious change in sleep time.
Therefore, the sleep-aiding effect of the agalloch eaglewood fireless aromatherapy liquids in the examples 5 to 7 of the invention is greatly improved compared with the sleep-aiding effect of the agalloch eaglewood fireless aromatherapy liquids in the comparative examples 5 to 7, wherein the agalloch eaglewood fireless aromatherapy liquid in the example 5 has the best sleep-aiding effect and is the best process condition of the agalloch eaglewood fireless aromatherapy liquid.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The agilawood fireless incense fumigating liquid is characterized by comprising the following raw materials in percentage by mass:
the agilawood hydrolat is prepared by the following method:
pretreatment: pulverizing lignum Aquilariae Resinatum, and sieving to obtain lignum Aquilariae Resinatum granule;
extraction: using supercritical CO2Extracting lignum Aquilariae Resinatum granule by method or water distillation method to obtain lignum Aquilariae Resinatum extract;
molecular cleavage: cutting the agilawood extract by using a molecular distillation device, wherein the cutting vacuum degree is 0.01-1000Pa, obtaining first-section, middle-section and tail-section products, discarding the first-section and tail-section products, and keeping the middle-section product; wherein, the first section product refers to the product from the beginning of accurate cutting for 10-30min, the last section product refers to the product from the end of accurate cutting for 90-120min, and the middle section product refers to the product between the first section and the last section;
and (3) distillation: and mixing the middle section product with water, wherein the mass ratio of the middle section product to the deionized water is 1: (1000-4000), and performing continuous distillation by gradient heating to obtain a saturated solution, namely the agilawood hydrosol.
2. The agilawood fireless incense liquid as claimed in claim 1, wherein the carrier oil is selected from the group consisting of: one or two of sweet almond oil and fractionated coconut oil; the emulsifier is selected from: one or more of tween-20, tween-60 and tween-80.
3. The fireless agilawood incense liquid as claimed in claim 1, wherein in the pretreatment step, the agilawood is selected from a good incense formation part of an aquilaria sinensis tree with the age of more than 2 years; and crushing the agilawood and sieving the crushed agilawood with a 20-60-mesh sieve.
4. The fireless agilawood incense liquid as claimed in claim 1, wherein the density of the agilawood extract is 0.8-1.2 g/cm3。
5. The fireless agilawood incense liquid as claimed in claim 1, wherein the extracting step adopts supercritical CO2Extracting under 18-40MPa at 50-65 deg.C for 90-120min at 50-300L/min.
6. The agilawood fireless incense liquid as claimed in claim 1, wherein the extraction step adopts water distillation extraction, and specifically comprises the following steps: mixing the components in a mass ratio of 1: (5-20) mixing the lignum Aquilariae Resinatum granules with water, heating to 90-100 deg.C, under 90-110kPa for 1440min, and distilling for 240-.
7. The agilawood fire-free incense liquid as claimed in any one of claims 1 to 6, wherein in the molecular cutting step, the film-scraping rotation speed of the first column of the molecular distillation device is 100-.
8. The agilawood fireless incense liquid as claimed in claim 1, wherein the gradient heating is a three-stage heating, the first stage heating is increased to 70-80 ℃ at a speed of 5-15 ℃/min, the second stage heating is increased to 90-95 ℃ at a speed of 1-5 ℃/min, and the third stage heating is increased to 97-105 ℃ at a speed of 0.5-1.5 ℃/min.
9. The preparation method of the aquilaria wood fireless aromatherapy liquid according to any one of claims 1 to 8, which is characterized by comprising the following steps:
s1, uniformly mixing the carrier oil and the emulsifier to obtain water-soluble carrier oil;
s2, mixing lignum Aquilariae Resinatum hydrosol and ethanol, adding the above water soluble carrier oil, mixing, adding water, sealing, and packaging to obtain the final product.
10. The use of the agalloch eaglewood fireless aromatherapy liquid as claimed in any one of claims 1 to 8 in the preparation of sleep-aiding products.
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Cited By (2)
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| CN111905038A (en) * | 2020-08-20 | 2020-11-10 | 海口植之素生物资源研究所有限公司 | Coconut oil-based antibacterial oil hydrogel and preparation method thereof |
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