CN111481483A - Aquilaria sinensis hydrolat and preparation method thereof - Google Patents
Aquilaria sinensis hydrolat and preparation method thereof Download PDFInfo
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- CN111481483A CN111481483A CN202010424697.0A CN202010424697A CN111481483A CN 111481483 A CN111481483 A CN 111481483A CN 202010424697 A CN202010424697 A CN 202010424697A CN 111481483 A CN111481483 A CN 111481483A
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- agilawood
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- hydrolat
- water
- distillation
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- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- Fats And Perfumes (AREA)
Abstract
The invention provides a preparation method of agilawood hydrolat, and relates to the technical field of plant extraction. The preparation method comprises the following steps: 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 lignum Aquilariae Resinatum extract with molecular distillation device at vacuum degree of 0.01-1000Pa to obtain first, middle and tail products, and discarding the first productProducts of the section and the tail section, and a product of the middle section is reserved; and (3) distillation: and mixing the middle-stage product with water, wherein the mass ratio of the middle-stage product to the water is 1: (1000-4000), and carrying out continuous distillation by adopting staged heating to obtain a saturated solution, namely the agilawood hydrosol. The agilawood hydrolat obtained by the method disclosed by the invention is low in impurity content, good in permeability and pure in fragrance.
Description
Technical Field
The invention relates to the technical field of plant extraction, and in particular relates to agilawood hydrolat and a preparation method 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. The lignum Aquilariae Resinatum has effects of lowering qi, warming middle warmer, warming kidney and invigorating qi, 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 incense channel culture, the agilawood function is developed more comprehensively, agilawood is mostly applied to the aspects of daily chemical skin care, aromatic health preservation and the like, and a plurality of agilawood products are successively appeared and pursued by the public.
The agilawood hydrolat generally refers to a distillation stock solution separated in the process of extracting essential oil from agilawood, contains a small amount of agilawood essential oil, has a good skin care effect, and can also be used as space incense. The agilawood hydrolat obtained by the traditional preparation method has high impurity content, is easy to have the problems of sour taste, insufficient aroma and different hydrolat odor types of different batches, and can not establish a product standard.
Disclosure of Invention
Therefore, the preparation method of the agilawood hydrolat is needed to solve the problems, and the obtained agilawood hydrolat has the advantages of low impurity content, good permeability and pure fragrance.
A preparation method of agilawood hydrolat comprises the following steps:
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 paste 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-stage product with deionized water, wherein the mass ratio of the middle-stage product to water is 1: (1000-4000), and performing continuous distillation by gradient heating to obtain a saturated solution, namely the agilawood hydrosol.
The inventor finds that extraction or extraction by using a traditional method can obtain an agilawood extract containing impurities, such as moisture, acetic acid, lactic acid, resin and the like, which are easy to deteriorate and generate sour and astringent taste influence odor type in the later storage process of the product without further purification treatment. The byproduct water solution obtained in the extraction process, namely the common agilawood hydrolat is easy to deteriorate, sour and astringent and the like. According to the purification method, molecular distillation is adopted to remove the first-stage and last-stage products, detection shows that the first-stage products mainly comprise water and small molecular impurities such as lactic acid, acetic acid and tannin, the impurities can cause the agilawood essential oil to generate bad smells such as sour taste and bitter taste and influence the stability of the agilawood products, the last-stage products mainly comprise resin and macromolecular impurities contained in the agilawood, the smells of the impurities are low or non-fragrant, the middle-stage products mainly comprise components such as sesquiterpene, agaric spironol and aquilaria sinensis aldehyde, and the components have pleasant fragrance and are not only important fragrant substances in the agilawood products but also effective components for medicinal effect of the agilawood; in addition, the gradient heating distillation is adopted, so that the agilawood essential oil is prevented from being independently distilled at a certain temperature, the agilawood hydrolat is more stable in saturation, more accurate in fragrance and purer in fragrance, and the phenomenon that the quality of hydrolat produced by the traditional distillation process is unstable is reduced.
In one embodiment, in the step of preprocessing, the agilawood is selected from a part of the agilawood with the age of more than 2 years, which is a good part of the agilawood. The lignum Aquilariae Resinatum material has the advantages of high oil content, and mellow and sweet fragrance.
In one embodiment, in the pretreatment step, the agilawood is crushed and then sieved by a 20-60-mesh sieve. Preferably, the agilawood is crushed and sieved by a 40-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 to obtain lignum Aquilariae Resinatum extract.
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 97-100 ℃ at a speed of 0.5-1.5 ℃/min. The first stage of heating makes the temperature of the deionized water gradually reach the condition of dissolving the agilawood essential oil, the second stage of heating makes the agilawood essential oil uniformly dissolved in the water and kept stable, and the third stage of heating makes the saturated agilawood hydrolat solution formed by the agilawood essential oil and the water reach and keep boiling, and the solution is continuously taken out of the distillation container in a steam form.
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 the agilawood hydrolat on one hand, wherein the agilawood hydrolat is prepared by the method. The agilawood hydrolat has the advantages of low impurity content, good permeability, stable property, long storage time, accurate fragrance and pure fragrance, can be applied to daily chemical products, and has the effects of fresh fragrance, lasting fragrance, sleep aiding, nerve calming and the like.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method, molecular distillation is adopted to remove the first-stage and the last-stage products, detection shows that the first-stage products mainly comprise water and small molecular impurities such as lactic acid, acetic acid and tannin, the impurities can cause the agilawood essential oil to generate bad smells such as sour taste and bitter taste and influence the stability of the agilawood products, the last-stage products mainly comprise resin and macromolecular impurities contained in the agilawood, the impurities have low or no fragrance, the middle-stage products mainly comprise components such as sesquiterpene, agaric spirol and aquilaria aldehyde, and the components have pleasant fragrance and are important fragrance substances in the agilawood products; moreover, the invention adopts gradient distillation, which avoids the agilawood essential oil from being independently distilled out under a certain temperature condition, so that the agilawood hydrolat saturation degree is more stable, the fragrance type is more accurate, and the fragrance is more pure.
The fragrant hydrolat disclosed by the invention has the advantages of low impurity content, good permeability, stable property, long storage time, accurate fragrance and pure fragrance, can be applied to daily chemical products, and has the effects of fresh fragrance, lasting fragrance, sleep aiding, nerve calming and the like.
Drawings
FIG. 1 is a radar fingerprint spectrum for evaluating the odor of Chinese eaglewood hydrolat;
fig. 2 is a schematic diagram of a test point of the agilawood mask.
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: the agilawood particles are placed in a water distillation device, the system pressure is normal pressure, deionized water is added, and the material-liquid ratio is 1: and 5, extracting for 60min to obtain the agilawood 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.
Comparative example 1
Aquilaria sinensis hydrolat 1 is commercially available and is obtained by extracting Aquilaria sinensis granules by a water distillation method.
Comparative example 2
Aquilaria sinensis hydrolat 2 is commercially available, and is obtained by extracting Aquilaria sinensis granules by a water distillation method.
Comparative example 3
Aquilaria sinensis hydrolat 3 is commercially available, and is obtained by extracting Aquilaria sinensis granules by a water distillation method.
Comparative example 4
An agilawood hydrolat is different from the agilawood hydrolat in example 4 in that 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, keeping boiling for 60min, and collecting steam cooling liquid to obtain lignum Aquilariae Resinatum hydrosol.
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 agilawood hydrolat the example and 0.5ml of the agilawood hydrolat at 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
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 in the agilawood hydrolat of the examples and the comparative examples 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 example 4 is higher than that of the agilawood hydrolat in comparative example 4, which indicates that the quality of the agilawood hydrolat is improved to a certain extent by step-type heating.
Experimental example 2
And testing the in-vitro antioxidant activity of the agilawood hydrosol.
The agilawood hydrolat of examples and comparative examples was subjected to radical scavenging ability test by DPPH method:
the DPPH was diluted to 6.5 × 10 with absolute ethanol-5And (3) mol/L, namely a DPPH solution, 100 mu L of the agilawood hydrolat in the example 1 and the comparative example 1 and 100 mu L of the DPPH solution are respectively added into a 96-well plate, uniformly mixed, and the absorbance at 517nm is measured by a microplate reader every two minutes, 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 words are carried out on the agilawood hydrolat obtained in the embodiment 1 and the comparative example 2 according to 12 professional fragrance smellers, 8 representative fragrance descriptors are screened out, the fragrance smellers respectively score each descriptor by using an integer of 0-10 for the agilawood hydrolat obtained pure dew, 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
| Fragrance type | Example 1 | Example 4 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Medicine incense | 5 | 4 | 3 | 3 | 2 |
| |
8 | 5 | 6 | 5 | 5 |
| |
6 | 5 | 3 | 4 | 3 |
| Wax incense | 3 | 6 | 6 | 5 | 5 |
| |
8 | 6 | 6 | 5 | 4 |
| Boiled flavor | 1 | 3 | 5 | 2 | 5 |
| Bitter incense | 3 | 3 | 0 | 2 | 0 |
| Cool feeling | 4 | 4 | 2 | 3 | 2 |
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
And testing the agilawood mask, wherein the following parts are parts by weight.
The agilawood hydrolat in example 1 is prepared into agilawood masks called example masks respectively, and the preparation method of the agilawood masks is as follows:
(1) weighing 30 parts of agilawood hydrolat, 1 part of yellow collagen, 0.3 part of vitamin E, 15 parts of glycerol, 5 parts of 1, 3-butanediol, 1 part of betaine, 0.3 part of sodium hyaluronate, 2 parts of β -glucan and 45.4 parts of deionized water;
(2) adding deionized water, lignum Aquilariae Resinatum hydrosol, xanthan gum, betaine, sodium hyaluronate and β -dextran into water phase container, heating to 78 deg.C, stirring for 25min, and cooling to 40 deg.C to obtain water phase solution;
(3) adding glycerol, 1, 3-butanediol and vitamin E into an emulsifying container, and stirring for 15min to obtain an oil phase solution for later use;
(4) adding the water phase solution into the oil phase solution, keeping the temperature at 40 deg.C, stirring for 15min, adding appropriate amount of L-lactic acid while stirring to adjust pH to 5.8-6.5 to obtain facial mask stock solution, dripping 40g facial mask stock solution into elastic facial mask base cloth, sealing and packaging.
The above facial masks were taken, and three commercially available eaglewood facial masks (commercially available facial mask 1, commercially available facial mask 2, and commercially available facial mask 3) were taken from 40 volunteer subjects, respectively, as follows:
(1) clinical data
40 volunteers were from communities of Guangzhou with symptoms of dry, rough, tense facial skin, 16 men and 24 women.
(2) Test method
Cleaning the face with warm water of 38 ℃ at night every day, applying the agilawood mask, taking down the agilawood mask after 15-20 minutes, gently massaging the face for 3 minutes to help absorption, and finally cleaning the face with clear water; after each use, the subject records evaluation of each index of the mask, and the score is divided into 10 points, wherein 0 point is the worst and 10 points are the best;
(3) evaluation index and test result
The evaluation indexes of the facial mask comprise moisturizing effect, fitting degree, relieving effect and fragrance evaluation, the average value of the scores of all indexes of the facial mask of a subject is counted, and the test result is finally obtained as follows:
TABLE 5 Aquilaria sinensis mask test results
| Item | Water replenishing effect | Degree of adhesion | Soothing effect | Evaluation of fragrance |
| EXAMPLES mask | 9.8 | 9.5 | 9.1 | 9.6 |
| Commercial mask 1 | 9.0 | 8.2 | 8.2 | 7.7 |
| Commercial mask 2 | 8.8 | 8.0 | 7.8 | 8.1 |
| Commercial mask 3 | 8.2 | 7.2 | 7.4 | 6.8 |
Therefore, compared with three commercially available facial masks, the facial mask of the embodiment has better moisturizing effect, fitting degree, relieving effect and fragrance evaluation.
Experimental example 5
Agilawood mask moisturizing test, the example mask and three commercially available agilawood masks (commercially available mask 1, commercially available mask 2, commercially available mask 3) were used by 30 volunteers, respectively, as follows:
(1) clinical data
30 volunteers were from communities of Guangzhou with no wounds, inflammation or skin-borne diseases on the face, 12 men and 18 women.
(2) Test method
The subject was placed in a relatively closed space at 25 deg.C and 60% air humidity and left in this space for 1 hour to eliminate the effect of environmental factors on the experiment. Measuring the moisture content of stratum corneum of facial mask by using skin detector, and measuring point 1 on forehead and point 2, point 3, point 4 and point 5 on cheek respectively, and averaging and recording as shown in FIG. 2;
using distilled water as a blank test, respectively applying the blank test, example 1, comparative example 2 and comparative example 3 to the face positions of point 1, point 2, point 3, point 4 and point 5, cutting the application mask to a size of 3cm by 3cm, removing the application mask after 20 minutes, respectively measuring the water content of the skin stratum corneum after 0 minute, 30 minutes and 120 minutes after the application mask is removed by using a skin detector, and recording the water content;
(3) skin moisture measurement data and calculations
TABLE 6 Water supplement test results
Calculating formula and defining: water supplement value (skin water content after application-skin water content before application)/skin water content before application is 100%; the mean hydration value is the mean of the hydration values of 30 subjects.
The average hydration values of the example mask, the commercial mask 1, the commercial mask 2, and the commercial mask 3 were calculated from the data as follows:
TABLE 7 average water supplement value obtained by calculation
According to the table, the low-sensitivity moisturizing agilawood mask prepared by using the agilawood hydrolat of the embodiment 1 of the invention as a raw material has an excellent moisturizing effect, and can effectively supplement skin moisture and keep the skin moisture. The moisturizing effect of the commercially available mask 1 was not maintained for a long time. Neither the moisturizing effect nor the maintenance effect of the commercially available mask 2 nor the commercially available mask 3 was satisfactory.
Experimental example 6
The agilawood mask skin irritation test was carried out by using 30 volunteers to respectively test the skin reactions of the patients by using the masks of example 1, the commercially available mask 2 and the commercially available mask 3 according to a method specified in the human body skin patch test of the second section of the seventh chapter of the human body safety test method of the cosmetic safety technical specification 2015 edition, and the results were recorded according to the skin reaction grading standard.
The experiment is specifically operated as follows: selecting skin area of 30mm2The nutrient solution of the mask in the mask of the embodiment is respectively put into a small chamber of the spot tester, the dosage is about 0.020m L, a control hole is a blank control (no substance is put), the spot tester added with the tested object is pasted on the curved side of the forearm of the tested object by using a hypoallergenic adhesive tape, the patch tester is lightly pressed by hands and is evenly pasted on the skin for 24h, the skin reaction is observed according to the standard of a table 8 after 30min (after the indentation disappears), 24h and 48h after the spot tester of the tested object is removed, and the observation result is recorded.
TABLE 8 skin Patch test skin response grading Standard
TABLE 9 skin irritation test integral record table
From the above table it can be derived: the accumulated integral of the commercially available facial mask 1 is 2, and 1 case of erythema occurs; the accumulated integral of the commercially available mask 2 is 1, and 1 case of weak erythema occurs; indicating that the mask 1 and the mask 2 have certain irritation to the skin. The cumulative integration of the mask of the examples and the mask 3 sold on the market is 0, which indicates that the low-sensitivity agilawood moisturizing mask obtained by using the agilawood hydrolat has no irritation to the skin.
Experimental example 7
And (3) testing the sleep-aiding effect of the agilawood fire-free aromatherapy liquid (CPC sleep monitoring method).
The agilawood hydrolat in example 1 is prepared into agilawood fire-free aromatherapy liquid, and the preparation method comprises the following steps:
(1) 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;
(2) putting 850g of the agalloch eaglewood hydrolat in example 1 and 80g of perfume alcohol into a stirring container, heating to 40 ℃ and keeping the temperature constant, adding 2g of water-soluble carrier oil while stirring, stirring for 10 minutes, adding 68g of deionized water, stirring uniformly, sealing and filling to obtain the agalloch eaglewood flameless incense liquid. Wherein the perfume alcohol is dehydrated alcohol without aldehyde.
The agilawood fireless aromatherapy liquid is taken to carry out sleep aiding effect test, a cardio-pulmonary coupling analysis (CPC) sleep quality evaluation analysis system is adopted in the experiment, and for 30 experimental subjects with insomnia or difficult sleep 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 the following table:
TABLE 10 situation of shortened sleep time after treatment of insomnia with lignum Aquilariae Resinatum fire-free aromatherapy liquid
Comparing the sleep time before and after using the agilawood fireless aromatherapy liquid: 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 method is adopted to respectively test the sleep-aiding effect of the agalloch eaglewood fireless aromatherapy liquid prepared by the agalloch eaglewood hydrolat of the comparative examples 1 to 3 to the comparative aromatherapy liquid 1 to 3, and the results are shown in the following table:
TABLE 11 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 agilawood fireless aromatherapy liquid prepared by the embodiment 1 of the invention has a sleep-aiding effect which is greatly improved compared with the comparative aromatherapy liquids 1-3.
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 preparation method of the agilawood hydrolat is characterized by comprising the following steps:
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 preparation method according to claim 1, wherein in the pretreatment step, the agilawood is selected from a part of the aquilaria sinensis tree with the age of more than 2 years.
3. The preparation method according to claim 1, wherein in the pretreatment step, the agilawood is crushed and then sieved by a 20-60-mesh sieve.
4. The preparation method according to claim 1, wherein the agilawood extract has a density of 0.8-1.2 g/cm3。
5. The method of claim 1, wherein the extracting step uses supercritical CO2Extracting under 18-40MPa at 50-65 deg.C for 90-120min at 50-300L/min.
6. The preparation method according to claim 1, wherein the extraction step is carried out by water distillation, 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 method as claimed in any one of claims 1 to 6, wherein in the step of molecular cutting, the first column of the molecular distillation device has a film-scraping rotation speed of 100-.
8. The method of claim 7, wherein the molecular distillation apparatus is an MDS-80 wiped film molecular distillation apparatus.
9. The method according to claim 1, wherein the gradient heating is a three-stage heating, the first stage heating is increased to 70-80 ℃ at a rate of 5-15 ℃/min, the second stage heating is increased to 90-95 ℃ at a rate of 1-5 ℃/min, and the third stage heating is increased to 97-100 ℃ at a rate of 0.5-1.5 ℃/min.
10. An agilawood hydrolat obtained by the preparation method of any one of claims 1-9.
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