CN113430050A - Preparation method of antioxidant essential oil of angelica dahurica - Google Patents
Preparation method of antioxidant essential oil of angelica dahurica Download PDFInfo
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Abstract
The invention provides a preparation method of antioxidant essential oil of angelica dahurica, which adopts absolute ethyl alcohol as an extraction solvent, prepares the essential oil of angelica dahurica by an ultrasonic extractor, designs a single-factor experiment from three factors of material-liquid ratio, ultrasonic extraction temperature and ultrasonic extraction time so as to design an orthogonal experiment to optimize extraction conditions, performs gas phase-gas quality analysis on the extracted essential oil, and preliminarily judges the components of the essential oil. The invention analyzes the DPPH free radical clearance rate of the extracted essential oil through experiments, and then preliminarily judges the antioxidant activity of the extracted essential oil. The result shows that when the feed-liquid ratio is 1:4, the extraction rate of the essential oil is 0.91% when the temperature is set to 40 ℃ and the time is set to 40 min. Analyzing the components and the antioxidant activity of the obtained essential oil of the angelica dahurica, and preliminarily determining that the essential oil of the angelica dahurica consists of fatty acid, ketone and alcohol; the result of measuring the clearance rate of the essential oil of the angelica dahurica on DPPH free radicals shows that the essential oil of the angelica dahurica has the potential of becoming a natural anticaking agent.
Description
Technical Field
The invention relates to a preparation method of antioxidant radix angelicae essential oil, and an experimental method for analyzing components and detecting antioxidant capacity of the antioxidant radix angelicae essential oil, in particular to a preparation method, a component analysis method and an antioxidant detection method of the antioxidant radix angelicae essential oil.
Background
Angelica dahurica (Angelica dahurica Benth) belongs to a dry root plant, and is a plant of Angelica of Umbelliferae. Radix angelicae dahuricae is a perennial plant, and is a woody plant of Quashan. The fruits of dahurian angelica root are mostly oval, while the color of the fruits of dahurian angelica root is yellowish-brown, sometimes it may have purple color, its length is 4-7mm, and width is about 4-6mm, the surface of the fruit has no hair, the back is flat, the fruit is thick, and its texture is like sponge. Radix Angelicae Dahuricae basically blooms in 7-8 months and fruits in Bayueny. In the forest, the edges of the forest, the sides of creeks, mountain ditches and bushes usually see more angelica dahurica, because the angelica dahurica likes sufficient illumination and mild and humid climate, in most northern areas of China, the angelica dahurica has good medicinal value, so that more angelica dahurica is planted, and the angelica dahurica has stronger cold resistance. The angelica dahurica serving as a traditional Chinese herbal medicine has good medicinal value, has obvious effects on whitening and skin care, and has high utilization value in the aspects of bacteriostasis and oxidation resistance.
At present, the common essential oil extraction methods mainly comprise a steam distillation method, a solvent extraction method and supercritical CO2The extraction method adopts ultrasonic assisted absolute ethyl alcohol extraction method to extract the essential oil of the angelica dahurica, and the principle of the ultrasonic extraction method is that strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, stirring effect and other effects are generated by ultrasonic radiation pressure, the motion frequency and speed of macromolecules are increased, the fusion of a solvent and the wanted components is accelerated, and the extraction efficiency of the essential oil is improved. The method has high efficiency in dispersing, atomizing and homogenizing processes, and no loss of essential oil due to excessive temperature. The obtained essential oil has high extraction rate, high extraction speed and high efficiency, is the greatest advantage of ultrasonic extraction, can be extracted at room temperature, does not need heating, can save energy, and can be used for extracting natural products and biological activity by ultrasonic wavesThe composition is advantageous.
The radix angelicae essential oil extracted by the ultrasonic extraction method is a tawny essential oil with strong Chinese herbal medicine taste, has a certain antioxidant capacity, and has the potential of being used as a natural antioxidant. At present, the reports of the essential oil of the angelica dahurica are less than related researches, and the researches on the components of the essential oil of the angelica dahurica and the related researches on the oxidation resistance are less. And the obtained essential oil is subjected to gas phase-gas quality analysis to detect the main components of the essential oil of the angelica dahurica, so that the composition of the essential oil of the angelica dahurica is preliminarily judged, and the antioxidant activity of the essential oil of the angelica dahurica is preliminarily judged by detecting the removal rate of DPPH free radicals by the essential oil of the angelica dahurica, thereby laying a certain scientific foundation for further research, development and utilization of the extract of the angelica dahurica.
Disclosure of Invention
Aiming at a series of problems in the existing essential oil extraction technology, the invention adopts the technology of an ultrasonic-assisted absolute ethyl alcohol extraction method, and carries out preliminary analysis and research on the components and the antioxidant activity of the extracted essential oil of angelica dahurica through the experiment, and the technology can effectively overcome the problems of low extraction efficiency of essential oil and toxic organic solvent residue, and can well control the extraction conditions, thereby belonging to the technology of energy conservation and environmental protection. On the basis of experimental design and analysis of single factors (material-liquid ratio, ultrasonic extraction time and ultrasonic extraction temperature), the influence of the material-liquid ratio, the ultrasonic extraction temperature and the ultrasonic extraction time on the extraction rate is respectively analyzed, an orthogonal experiment is further designed on the basis, the extraction conditions of the angelica essential oil are further optimized, and the experiment is designed to detect components and antioxidant activity.
In order to achieve the purpose, the technical scheme of the invention is as follows, the extraction process of the angelica essential oil by the ultrasonic assisted absolute ethanol extraction method is characterized by comprising the following steps:
preparation method of antioxidant essential oil of angelica dahurica
Step 1), preparing radix angelicae powder;
step 2), ultrasonic extraction;
step 3), suction filtration;
step 4), rotary evaporation;
step 5), centrifuging;
and 6) weighing and calculating.
As an improvement of the invention, in the step 1) of preparing the radix angelicae powder, the dried radix angelicae blocks are crushed into powder by a crusher and placed in a dry plastic bottle for storage.
As an improvement of the invention, for the ultrasonic extraction in the step 2), 30g of the crushed angelica dahurica powder is weighed by an electronic balance and put into a 250mL conical flask, the extraction solvent absolute ethyl alcohol is added, and the conical flask is sealed by a silica gel plug matched with an ultrasonic extraction device, so that the volatilization of the absolute ethyl alcohol and the volatile oil is prevented. And (3) placing the sealed conical flask in an ultrasonic extraction device, inserting an amplitude transformer, and adjusting the height to keep the depth of the amplitude transformer penetrating into the liquid level to be 1 cm. Starting the ultrasonic wave, adjusting the proportional parameters and starting extraction.
As an improvement of the present invention, in the step 3), the liquid after ultrasonic extraction is subjected to suction filtration by a vacuum suction filtration pump to obtain a filtrate.
As an improvement of the invention, for the rotary evaporation in the step 4), the filtrate obtained after the suction filtration in the step is poured into a round-bottom flask, a rotary evaporator is correctly installed according to the instruction, the airtightness of the device is checked, the rotary evaporation operation is carried out, the temperature (the temperature is set to be 40-50 ℃, the temperature is prevented from being too high, so that the essential oil volatilizes, and the measurement result is inaccurate) and the rotating speed are set, and the angelica essential oil is obtained.
As an improvement of the invention, for the centrifugation in the step 5), specifically, the angelica essential oil obtained after the rotary evaporation is filled into a proper centrifugal tube for balancing, and is placed in an ultracentrifuge for centrifugation twice at 10000r/s for 10 minutes, and then the precipitate is removed, and the supernatant is reserved.
As a modification of the invention, for step 6) weighing and calculating, specifically, as follows, weighing and recording the supernatant after centrifugation, and storing in a brown bottle.
As an improvement of the invention, in the step 2), the material-liquid ratio is 1:4, the ultrasonic temperature is set to be 40 ℃, the ultrasonic time is set to be 40min, and the extraction rate under the extraction condition can reach 0.91 percent at most.
(II) analysis of Components
(1) Gas phase experiment
Gas chromatography conditions:
column type: DB-5 capillary chromatographic column
The gasification temperature: 280 deg.C
Column temperature: 50 ℃ (1min) - -10 ℃/min-240 ℃ (15min)
Carrier gas: helium gas
Flow rate of carrier gas: 2.0mL/min
The split ratio is as follows: 30:1
Sample introduction amount: 0.5. mu.L
(2) Mass Spectrometry experiment
Mass spectrum conditions:
an ionization mode: EI (El)
Ionization energy: 70ev
Scanning range: 20-500amu
Ion source temperature: 230 deg.C
A spectrum library: NIST spectral library
(III) measurement of Oxidation resistance
Step 1), preparing a sample solution for removing DPPH (dehydroepiandrosterone) free radicals from radix angelicae essential oil;
step 2) preparing a DPPH-absolute ethyl alcohol reagent;
step 3) preparing a vitamin C sample solution (serving as a control group);
step 4), blank liquid;
step 5), sample adding;
step 6), measuring an absorbance value by using a spectrophotometer;
step 7), calculating the sample clearance rate of the oxidation resistance calculation method;
step 8) the antioxidant capacity of the test sample is analyzed by the experimental method.
As an improvement of the invention, for the preparation of the sample solution for removing DPPH from the angelica essential oil in the step 1), 0mg,5mg,10mg,15mg,20mg and 25mg of the angelica essential oil are respectively weighed, and absolute ethyl alcohol is added to the weighed volume of 10mL to obtain the essential oil diluent of 0mg/mL,0.5mg/mL,1mg/mL,1.5mg/mL,2mg/mL and 2.5 mg/mL.
As an improvement of the invention, for the preparation of the DPPH-absolute ethyl alcohol reagent in the step 2), 0.004g of DPPH solid is weighed by an analytical balance and placed in a beaker, absolute ethyl alcohol is added, stirring is carried out to enable the DPPH solid to be fully dissolved, then a 50mL volumetric flask is used for constant volume, the prepared solution is bottled, a layer of tinfoil is wrapped outside the flask, and then the solution is placed in a refrigerator at 4 ℃ for storage. (follow-up and use)
As an improvement of the invention, in step 3), the vitamin C sample solution (as a control group) is prepared by respectively weighing 0mg,5mg,10mg,15mg,20mg and 25mg of ascorbic acid, and then using absolute ethyl alcohol to respectively fix the volume to 10mL to obtain solutions of 0mg/mL,0.5mg/mL,1mg/mL,1.5mg/mL,2mg/mL and 2.5 mg/mL.
As an improvement of the invention, the blank liquid in the step 4) is prepared by taking absolute ethyl alcohol
As an improvement of the present invention, for the sample addition in step 5), the liquid obtained in the above step is added according to the following table, and is protected from light for 30 min.
TABLE 1 sample loading table (/ mL) for determining antioxidant capacity of sample by DPPH method
As an improvement of the invention, in step 6), the absorbance value is measured by a spectrophotometer, specifically, as follows, 517nm is the wavelength set by the experiment, the absorbance value is adjusted to zero, and then the absorbance value of different samples is measured and recorded.
As a modification of the present invention, the method for calculating the oxidation resistance in step 7) is a method for calculating the sample clearance, specifically, as follows, the clearance (%) ═ a0-(A1-A2)]/A0X 100% (wherein A)0Is the absorbance of DPPH solution, A1Is the light absorption value of the DPPH solution removed by sample solutions with different concentrations, A2Repeat 3 times for absorbance values of sample solutions of different concentrations. The control method is the same. )
As a modification of the present invention, the antioxidant ability of the essential oil of angelica dahurica and ascorbic acid is analyzed by the experimental method for step 8), and the measurement result of the antioxidant ability shows that the essential oil of angelica dahurica and ascorbic acid have good antioxidant ability and the antioxidant effect of the essential oil of angelica dahurica and ascorbic acid is better along with the increase of the respective concentrations in the respective proper concentration ranges.
Compared with the prior art, the invention has the following advantages that 1) the raw material of the technical scheme is angelica dahurica, the selected extraction process is an ultrasonic assisted absolute ethyl alcohol extraction method, and the principle of the method is that the principle of ultrasonic extraction of essential oil is strong cavitation effect, mechanical vibration, disturbance effect, high acceleration, stirring effect and other effects generated by ultrasonic radiation pressure, the motion frequency and speed of macromolecules are increased, the fusion of a solvent and the wanted components is accelerated, and the extraction efficiency of the essential oil is improved. The method has high efficiency in dispersing, atomizing and homogenizing processes, and no loss of essential oil due to excessive temperature. The obtained essential oil has the advantages of high extraction rate, high extraction speed and high efficiency, is the greatest advantage of ultrasonic extraction, can be extracted at room temperature, does not need heating, can save energy, and has great advantages when extracting natural products and bioactive components by ultrasonic waves. 2) The extraction solvent used in the process is absolute ethyl alcohol, the materials are easy to obtain, and the cost is low. 3) The optimal condition extracted by the scheme is determined by optimizing on the basis of a single-factor experiment and an orthogonal experiment: the material-liquid ratio is 1:4, the ultrasonic extraction time is 40min, and the highest extraction rate can reach 0.91% under the condition when the ultrasonic extraction temperature is 40 ℃. 4) Through analysis of the antioxidant activity of the essential oil, the determination result shows that the essential oil of angelica dahurica and the ascorbic acid both have better antioxidant activity.
Drawings
Fig. 1 is a graph showing the effect of feed liquid ratio on the extraction rate of essential oil from radix angelicae dahuricae.
Figure 2 is a graph of the effect of temperature on the extraction rate of angelica essential oil.
FIG. 3 is a graph showing the effect of time on the extraction rate of essential oil from radix Angelicae Dahuricae.
Fig. 4 is a picture of essential oil of angelica dahurica.
Fig. 5 is a total ion flow chromatogram of radix angelicae essential oil.
Fig. 6 is a graph comparing the removal rate of DPPH by essential oil of dahurian angelica root and ascorbic acid.
Detailed Description
For the purpose of enhancing an understanding of the present invention, the present embodiment will be described in detail below with reference to the accompanying drawings.
The invention relates to a process for extracting essential oil by an ultrasonic-assisted absolute ethyl alcohol extraction technology, and detecting the components and antioxidant activity of the essential oil, which comprises the following steps:
preparation method of antioxidant essential oil of angelica dahurica
Step 1), preparing radix angelicae powder;
step 2), ultrasonic extraction;
step 3), suction filtration;
step 4), rotary evaporation;
step 5), centrifuging;
and 6) weighing and calculating.
In this example, for the preparation of the radix angelicae powder in step 1), the dried radix angelicae blocks are pulverized into powder by a blender and stored in a dry plastic bottle as follows.
In this embodiment, for the ultrasonic extraction in step 2), specifically, 30g of the crushed angelica dahurica powder is weighed by an electronic balance and placed in a 250mL conical flask, the extraction solvent absolute ethyl alcohol is added, and the conical flask is sealed by a silica gel plug matched with the ultrasonic extraction device, so as to prevent the evaporation of the absolute ethyl alcohol and the volatile oil. And (3) placing the sealed conical flask in an ultrasonic extraction device, inserting an amplitude transformer, and adjusting the height to keep the depth of the amplitude transformer penetrating into the liquid level to be 1 cm. Starting the ultrasonic wave, adjusting the proportional parameters and starting extraction.
In this example, as for the suction filtration in step 3), specifically, the liquid after the ultrasonic extraction was suction-filtered by a vacuum suction pump to obtain a filtrate.
In this embodiment, for the rotary evaporation in step 4), specifically, the filtrate obtained in the step is poured into a round-bottom flask after suction filtration, a rotary evaporator is correctly installed according to the instruction, the airtightness of the device is checked, the rotary evaporation operation is performed, and the temperature (set at 40-50 ℃ to avoid over-high temperature, so that the essential oil volatilizes, and the measurement result is inaccurate) and the rotation speed are set, so as to obtain the essential oil of angelica dahurica.
In this embodiment, as for the centrifugation in step 5), specifically, the angelica essential oil obtained after the rotary evaporation is filled into a proper centrifugal tube for balancing, and is placed in an ultracentrifuge for centrifugation twice, the rotation speed is 10000r/s, the setting time is 10 minutes, the precipitate is removed, and the supernatant is retained.
In this example, for step 6) weighing and calculation, specifically as follows, the supernatant after centrifugation was weighed and recorded, and stored in a brown bottle.
In this example, the extraction rate under the extraction conditions was as high as 0.91% for the step 2) at a feed-to-liquid ratio of 1:4, an ultrasonic temperature of 40 ℃ and an ultrasonic time of 40 min.
(II) analysis of Components
(1) Gas phase experiment
Gas chromatography conditions:
column type: DB-5 capillary chromatographic column
The gasification temperature: 280 deg.C
Column temperature: 50 ℃ (1min) - -10 ℃/min-240 ℃ (15min)
Carrier gas: helium gas
Flow rate of carrier gas: 2.0mL/min
The split ratio is as follows: 30:1
Sample introduction amount: 0.5. mu.L
(2) Mass Spectrometry experiment
Mass spectrum conditions:
an ionization mode: EI (El)
Ionization energy: 70ev
Scanning range: 20-500amu
Ion source temperature: 230 deg.C
A spectrum library: NIST spectral library
(III) measurement of Oxidation resistance
Step 1), preparing a sample solution for removing DPPH (dehydroepiandrosterone) free radicals from radix angelicae essential oil;
step 2) preparing a DPPH-absolute ethyl alcohol reagent;
step 3) preparing a vitamin C sample solution (serving as a control group);
step 4), blank liquid;
step 5), sample adding;
step 6), measuring an absorbance value by using a spectrophotometer;
and 7) calculating the sample clearance rate of the oxidation resistance calculation method.
In this embodiment, for the preparation of the sample solution for removing DPPH from the angelica essential oil in step 1), 0mg,5mg,10mg,15mg,20mg, and 25mg of the angelica essential oil are weighed respectively, and absolute ethyl alcohol is added to a constant volume of 10mL, so as to obtain 0mg/mL,0.5mg/mL,1mg/mL,1.5mg/mL,2mg/mL, and 2.5mg/mL of the essential oil diluent.
In this embodiment, for the preparation of DPPH-absolute ethanol reagent in step 2), specifically, 0.004g of DPPH solid is weighed by an analytical balance and placed in a beaker, absolute ethanol is added, stirring is performed to fully dissolve the DPPH solid, then a 50mL volumetric flask is used for constant volume, the prepared DPPH solid is bottled, a layer of tinfoil is wrapped outside the volumetric flask, and the DPPH-absolute ethanol reagent is placed in a refrigerator at 4 ℃ for storage. (follow-up and use)
In this example, in step 3), ascorbic acid was weighed as 0mg,5mg,10mg,15mg,20mg, and 25mg, respectively, and the volume was adjusted to 10mL with absolute ethanol to obtain solutions of 0mg/mL,0.5mg/mL,1mg/mL,1.5mg/mL,2mg/mL, and 2.5mg/mL, respectively, for the preparation of the vitamin C sample solution (as a control group).
In this embodiment, as for the blank liquid in the step 4), the anhydrous ethanol is taken as follows
In this example, the liquid obtained in the above step was added in the following manner, specifically, according to table 1, and the sample was kept in the dark for 30 min.
TABLE 1 sample loading table (/ mL) for determining antioxidant capacity of sample by DPPH method
In this example, for step 6), absorbance was measured spectrophotometrically, specifically as follows, 517nm is the experimentally set wavelength, zeroed, and absorbance was measured and recorded for different samples.
In the present example, the method sample clearance was calculated for the oxidation resistance at step 7), specifically as follows, clearance (%) ═ a0-(A1-A2)]/A0X 100% (wherein A)0Is the absorbance of DPPH solution, A1Is the light absorption value of the DPPH solution removed by sample solutions with different concentrations, A2Repeat 3 times for absorbance values of sample solutions of different concentrations. The control method is the same. )
The technical process of the invention is mainly optimized by the following technical scheme:
single factor experimental method and results and analysis
Single factor experimental method:
(1) ultrasonic extraction of essential oil from radix angelicae dahuricae at different material-liquid ratios
Accurately weighing 30g of radix angelicae powder, respectively placing 3 parts of the radix angelicae powder in 250mL conical flasks, respectively adding different milliliters of absolute ethyl alcohol into each flask according to different material-liquid ratios to ensure that the material-liquid ratios are 1:4,1:6 and 1:8 respectively, stirring, placing at 50% ultrasonic frequency, setting the temperature at 40 ℃, and performing ultrasonic extraction for 40 minutes. And testing and calculating the extraction rate of the essential oil. Repeat three times, take the average value.
(2) Ultrasonic extraction of essential oil of angelica dahurica at different temperatures
Accurately weighing 30g of radix angelicae powder, respectively placing 3 parts of the radix angelicae powder in 250mL conical flasks, respectively adding 180mL of absolute ethyl alcohol into each flask according to different temperatures to ensure that the material-liquid ratio is 1:6, stirring, placing at 50% ultrasonic frequency, respectively setting the temperature at 30 ℃, 40 ℃ and 50 ℃, and performing ultrasonic extraction for 40 minutes. And testing and calculating the extraction rate of the essential oil. Repeat three times, take the average value.
(3) Ultrasonic extraction of essential oil of angelica dahurica at different times
Accurately weighing 30g of radix angelicae powder, respectively placing 3 parts of the radix angelicae powder in 250mL conical flasks, respectively adding 180mL of absolute ethyl alcohol into each flask according to different temperatures to ensure that the material-liquid ratio is 1:6, stirring, placing at 50% ultrasonic frequency, setting the temperature at 40 ℃, and respectively setting the ultrasonic extraction at 30, 40 and 50 minutes. And testing and calculating the extraction rate of the essential oil. Repeat three times, take the average value. Single factor experimental results and analysis:
(1) influence of different feed liquid ratios on extraction rate of essential oil from radix Angelicae Dahuricae
Analyzing the figure 1, controlling the temperature and the time to be unchanged, and discussing the influence of different material liquid ratios on the extraction rate of the angelica essential oil. When the ratio of the material to the liquid is 1:4, the first measurement is 0.3%, the second measurement is 0.33%, the third measurement is 0.4%, and the average of the three measurements is 0.34%; when the material-liquid ratio is 1:6, the extraction rate of the angelica essential oil is 0.6 percent for the first time, 0.7 percent for the second time and 0.68 percent for the third time, and the average of the three times is 0.66 percent; when the material-liquid ratio is 1:8, the extraction rate of the angelica essential oil is 0.07 percent when the material-liquid ratio is measured for the first time. The second time is 0.07%, the third time is 0.09%, and the average of the three times is 0.08%. Finally, the deviation of the three groups of data calculated by an Excel table is 0.041,0.043 and 0.009 respectively. The radix angelicae essential oil is increased along with the increase of the material-liquid ratio, the extraction rate of the radix angelicae essential oil is the largest at the material-liquid ratio of 1:6, and the extraction rate is reduced after 1: 6. In the material-liquid ratio of 1: the analysis of the curve between 4 and 1:6 may be that the more absolute ethyl alcohol, the more complete the mixing with the angelica dahurica powder, so that more essential oil can be extracted from the angelica dahurica powder, and the extraction rate shows a rising trend. In the ratio of material to liquid of 1:6 to 1:8, the extraction rate of the essential oil is rather reduced as the ratio of material to liquid increases, and the reason for analyzing the high ratio of material to liquid is that the essential oil part of angelica dahurica is dissolved in absolute ethyl alcohol and can dilute certain components of the essential oil, so that the extraction rate becomes low. Therefore, the feed-liquid ratio of 1:6 is optimal.
(2) Influence of different temperatures on extraction rate of angelica essential oil
According to the figure 2, under the condition that other conditions are not changed, the influence of different temperatures on the extraction rate of the essential oil of the angelica dahurica extracted by ultrasonic waves can be seen. When the temperature is 30 ℃, the extraction rate of the angelica essential oil is 0.37 percent in the first measurement, 0.4 percent in the second measurement and 0.38 percent in the third measurement, and the average value is 0.38 percent; when the temperature is 40 ℃, the extraction rate of the angelica essential oil is 0.6 percent when being measured for the first time, the extraction rate of the angelica essential oil is 0.7 percent when being measured for the second time, the extraction rate of the angelica essential oil is 0.68 percent when being measured for the third time, and the average of the extraction rate of the angelica essential oil for the third time is 0.66 percent; when the temperature is 50 ℃, the extraction rate of the angelica essential oil is 0.43 percent for the first time, the extraction rate of the angelica essential oil is 0.53 percent for the second time, the extraction rate of the angelica essential oil is 0.49 percent for the third time, and the average value of the three times is 0.48 percent. Finally, the deviation of the three groups of data calculated by an Excel table is 0.012,0.043 and 0.041 respectively. The extraction rate of the angelica essential oil is increased and then reduced along with the increase of the ultrasonic temperature, when the temperature is 40 ℃, the extraction rate of the angelica essential oil is the highest, and after the temperature is 40 ℃, the extraction rate of the angelica essential oil is in a descending trend, which shows that the extracted angelica essential oil can volatilize at the temperature of more than 40 ℃, so that the extraction rate of the angelica essential oil obtained by controlling the ultrasonic extraction temperature to be 40 ℃ is the highest.
(3) Influence of different ultrasonic extraction time on angelica essential oil extraction rate
According to fig. 3, it can be seen that, under the condition of keeping other conditions unchanged, the influence of different ultrasonic extraction time on the extraction rate of the essential oil of angelica dahurica by ultrasonic extraction is avoided. When the time is 30min, the extraction rate of the radix angelicae essential oil is 0.27% in the first measurement, the extraction rate of the radix angelicae essential oil is 0.37% in the second measurement, the extraction rate of the radix angelicae essential oil is 0.34% in the third measurement, and the average value of the values of the three measurements is 0.33%; when the time is 40min, the extraction rate of the radix angelicae essential oil is 0.6% in the first measurement, the extraction rate of the radix angelicae essential oil is 0.7% in the second measurement, the extraction rate of the radix angelicae essential oil is 0.68% in the third measurement, and the average value of the three times is 0.66%; when the time is 50min, the extraction rate of the radix angelicae essential oil is 0.33% measured for the first time, the extraction rate of the radix angelicae essential oil is 0.23% measured for the second time, the extraction rate of the radix angelicae essential oil is 0.26% measured for the third time, and the average value of the three times is 0.27%. Finally, the deviation of the three groups of data calculated by an Excel table is 0.041,0.043 and 0.041 respectively. The extraction rate of the radix angelicae essential oil is increased and then reduced along with the increase of time. The extraction rate of the angelica essential oil is in a rising trend from 30min to 40min, which shows that the longer the time is, the more beneficial the extraction of the essential oil is; after 40min, the extraction rate of the radix angelicae essential oil is low, which shows that the soaking of the absolute ethyl alcohol only has the function of water dispersion on the radix angelicae powder, and after 40min, the effect is not achieved even if the time is prolonged, and the extraction rate is optimal at 40 min.
Orthogonal test design and result analysis
TABLE 2 orthogonal experimental design table for essential oil of dahurian angelica
Taking the extraction rate of the angelica essential oil as an evaluation index, carrying out data analysis on the three-factor three-level orthogonal test design, and making an angelica essential oil orthogonal test design table (table 2). The extraction rate of each experiment was measured for 9 experiments in sequence according to the running order (table 3).
TABLE 3 analysis of orthogonal test results
The radix angelicae essential oil extracted by the ultrasonic extraction method has the advantages that the raw material is absolute ethyl alcohol, the absolute ethyl alcohol is simple and easy to obtain, the extraction efficiency is high, the extraction rate of the obtained radix angelicae essential oil is high, and harmful gas cannot be generated. As can be seen from the analysis of the results of the orthogonal test in Table 3, R(B)>R(C)>R(A)Therefore, the influence of the temperature on the extraction rate of the essential oil of the angelica dahurica is greater than the influence of the ultrasonic extraction time which is greater than the material-liquid ratio, so that the influence of the temperature on the extraction rate of the essential oil of the angelica dahurica is most obvious, and the effect of the material-liquid ratio is least obvious, so that the optimal level of the temperature is selected to be 40 ℃, the optimal level of the time is preferably 40min, and the optimal level of the material-liquid ratio is 1:4, and the extraction rate of the obtained white paper essential oil is optimal. The results of the orthogonal test are combined to show that when the temperature is 40 ℃ and the ultrasonic extraction time is 40min, the measured essential oil is 0.272g, namely the extraction rate is 0.91 percent and is higher than the maximum 0.8 percent, so the optimal extraction rate obtained by the orthogonal test is reliable.
Sensory evaluation results of essential oils
The essential oil is yellow brown, has low transparency, is obviously oily when being dipped on a small amount of hands, and has a strong herbal medicine taste.
Analysis results of essential oil components
TABLE 4 ingredient results of essential oils of Angelica dahurica
According to the detection report of the angelica essential oil by the modern analysis center of Nanjing university (Table 4), the essential oil contains ten components, namely about 2.98 percent of 5-hydroxymethyl furfural, about 5.44 percent of palmitic acid, about 11.71 percent of xanthotoxol, about 16.16 percent of linoleic acid and elaidic acid, about 3.19 percent of falcarinone, about 9.99 percent of phellandrin, about 4.86 percent of monolinolein 3 glyceride, about 3.98 percent of stigmasterol and about 3.34 percent of gamma-sitosterol, which are detected and reported by the Nanjing university. Furthermore, it can be seen from FIG. 5 that the peaks corresponding to the four components linoleic and elaidic acid, palmitic acid, and sickle-leaf celery ketone are highest. Therefore, the essential oil of the angelica dahurica is preliminarily determined to be mainly composed of ketones, alcohols and fatty acids. 5-hydroxymethylfurfural contained in the essential oil of the angelica dahurica can reduce blood fat and blood pressure and soften blood vessels, can prevent and treat cardiovascular diseases and has a prevention effect on atherosclerosis; the linoleic acid is used as the fatty acid necessary for human beings, and has good utilization value.
Results of oxidation resistance analysis
Tests show that the clearance of the essential oil of angelica dahurica and the ascorbic acid to DPPH free radicals under the condition of the same concentration is in a comparative relation, and the clearance of the ascorbic acid is obviously higher than that of the essential oil of angelica dahurica. At a concentration of 0.5mg/ml, the clearance of ascorbic acid is 57.80%, the clearance of DPPH free radicals is stronger and stronger with the increase of the concentration of ascorbic acid, and the clearance of DPPH free radicals is up to 100% after 2.0 mg/ml. In the concentration range, the removal rate of DPPH free radicals of the angelica essential oil is 32.1% at 0.5mg/ml, 34.6% at 1mg/ml, 41.5% at 1.5mg/ml, 47.5% at 2.0mg/ml and 52.1% at 2.5mg/ml, so that the ratio of DPPH free radicals removed shows a rising trend along with the increase of the concentration. According to the figure, the clearance rate of ascorbic acid on DPPH free radicals is obviously higher than that of the radix angelicae essential oil, but the clearance rate of the radix angelicae essential oil on DPPH free radicals in the experiment can reach as high as 52.1%, so the radix angelicae essential oil has the potential of being used as an antioxidant.
Conclusion
The essential oil of angelica dahurica extracted by the ultrasonic wave assisted absolute ethanol extraction method is a liquid which is brownish yellow and has poor transparency and strong traditional Chinese medicine taste. Through a single-factor experiment design orthogonal test, the extraction condition of the radix angelicae essential oil is optimized, and the highest extraction rate of the radix angelicae essential oil is 0.91% when the material-liquid ratio is 1:4, the ultrasonic temperature is 40 ℃ and the ultrasonic extraction time is 40 min. And the modern analysis center of Nanjing university can obtain that the essential oil of radix Angelicae Dahuricae is mainly composed of fatty acid, ketone and alcohol. The obtained essential oil is further subjected to oxidation resistance analysis, the DPPH free radical clearance rate is measured, and the maximum clearance rate in the set concentration gradient can reach 52.1%, so that the essential oil of the angelica dahurica has the potential of being used as a natural antioxidant.
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (8)
1. The preparation method of the antioxidant essential oil of the angelica dahurica is characterized by comprising the following steps:
step 1), preparing radix angelicae powder;
step 2), ultrasonic extraction;
step 3), suction filtration;
step 4), rotary evaporation;
step 5), centrifuging;
and 6) weighing and calculating.
2. The preparation method of the antioxidant radix angelicae essential oil as claimed in claim 1, wherein the radix angelicae powder is prepared in step 1), and specifically, dried radix angelicae blocks are crushed into powder by a blender and placed in a dry plastic bottle for storage.
3. The preparation method of the antioxidant essential oil of radix angelicae dahuricae according to claim 1, wherein the step 2) comprises the steps of carrying out ultrasonic extraction, specifically, weighing 30g of the crushed radix angelicae dahuricae powder in a 250mL conical flask by using an electronic balance, adding an extraction solvent, namely absolute ethyl alcohol, and sealing the conical flask by using a silica gel plug matched with an ultrasonic extraction device to prevent the absolute ethyl alcohol and volatile oil from volatilizing; placing the sealed conical flask in an ultrasonic extraction device, inserting an amplitude transformer, and adjusting the height to keep the depth of the amplitude transformer penetrating into the liquid level at 1 cm; starting the ultrasonic wave, adjusting the proportional parameters and starting extraction.
4. The preparation method of the antioxidant essential oil of radix angelicae dahuricae according to claim 1, wherein the step 3) comprises suction filtration, specifically, the liquid after ultrasonic extraction is subjected to suction filtration by a vacuum suction filtration pump, and a filtrate is obtained.
5. The method for preparing antioxidant radix angelicae essential oil according to claim 1, wherein the step 4) of rotary evaporation comprises pouring the filtered filtrate into a round-bottomed flask, correctly installing a rotary evaporator according to the instruction, checking the airtightness of the device, performing rotary evaporation operation, and setting the temperature and the rotation speed to obtain the radix angelicae essential oil, wherein the set temperature is 40-50 ℃.
6. The preparation method of the antioxidant radix angelicae essential oil as claimed in claim 1, wherein the step 5) of centrifugation comprises the steps of filling the radix angelicae essential oil obtained after the rotary evaporation into a proper centrifuge tube, balancing, placing the centrifuge tube in an ultracentrifuge for centrifugation twice, rotating at 10000r/s for 10 minutes, removing the precipitate, and keeping the supernatant.
7. The preparation method of antioxidant essential oil of radix angelicae dahuricae as claimed in claim 1, wherein the step 6) is weighing and calculating, and specifically, the following steps are carried out, weighing and recording of clear liquid after centrifugation, and storing in a brown bottle.
8. The preparation method of anti-oxidation radix angelicae essential oil according to claim 3, wherein the material-liquid ratio in the step 2) is 1:4, the ultrasonic temperature is set to 40 ℃, and the ultrasonic time is set to 40 min.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854275A (en) * | 2005-04-26 | 2006-11-01 | 天津唐朝食品工业有限公司 | Supercritical CO extraction of Angelica dehurical oil resin |
| CN101380109A (en) * | 2008-09-23 | 2009-03-11 | 江南大学 | Extraction method of Angelica Dahurica extract and use thereof as natural antioxidant |
| JP2011174021A (en) * | 2010-02-25 | 2011-09-08 | Japan Aroma Laboratory Co Ltd | Aromatic composition and fragrant using the same, deodorant, and antibacterial agent |
| CN108125874A (en) * | 2017-11-06 | 2018-06-08 | 朱浩奇 | A kind of Chinese medicine composition cosmetics of the essential oil containing Swertia patens and preparation method thereof |
| CN108159179A (en) * | 2018-02-09 | 2018-06-15 | 陈桂芳 | A kind of Qarnet cream containing the root of Dahurain angelica and preparation method thereof |
| CN110218612A (en) * | 2019-06-18 | 2019-09-10 | 江苏第二师范学院（江苏省教育科学研究院） | A kind of Ultrasound-assisted ethyl alcohol extraction process of butterfly Tofu pudding essential oil |
| CN112481032A (en) * | 2020-11-09 | 2021-03-12 | 江苏第二师范学院（江苏省教育科学研究院） | Extraction process of Holland chrysanthemum essential oil and Holland chrysanthemum essential oil |
-
2021
- 2021-06-16 CN CN202110668507.4A patent/CN113430050A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1854275A (en) * | 2005-04-26 | 2006-11-01 | 天津唐朝食品工业有限公司 | Supercritical CO extraction of Angelica dehurical oil resin |
| CN101380109A (en) * | 2008-09-23 | 2009-03-11 | 江南大学 | Extraction method of Angelica Dahurica extract and use thereof as natural antioxidant |
| JP2011174021A (en) * | 2010-02-25 | 2011-09-08 | Japan Aroma Laboratory Co Ltd | Aromatic composition and fragrant using the same, deodorant, and antibacterial agent |
| CN108125874A (en) * | 2017-11-06 | 2018-06-08 | 朱浩奇 | A kind of Chinese medicine composition cosmetics of the essential oil containing Swertia patens and preparation method thereof |
| CN108159179A (en) * | 2018-02-09 | 2018-06-15 | 陈桂芳 | A kind of Qarnet cream containing the root of Dahurain angelica and preparation method thereof |
| CN110218612A (en) * | 2019-06-18 | 2019-09-10 | 江苏第二师范学院（江苏省教育科学研究院） | A kind of Ultrasound-assisted ethyl alcohol extraction process of butterfly Tofu pudding essential oil |
| CN112481032A (en) * | 2020-11-09 | 2021-03-12 | 江苏第二师范学院（江苏省教育科学研究院） | Extraction process of Holland chrysanthemum essential oil and Holland chrysanthemum essential oil |
Non-Patent Citations (1)
| Title |
|---|
| 郭耀杰等: "川白芷不同品种（系）挥发油成分GC-MS分析" * |
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