CN114149864A - Method for improving extraction rate of essential oil of citrus unshiu by using ultrasonic-assisted micro-cutting auxiliary agent and application - Google Patents
Method for improving extraction rate of essential oil of citrus unshiu by using ultrasonic-assisted micro-cutting auxiliary agent and application 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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a method for improving the extraction rate of citrus aurtantium essential oil by using an ultrasonic-assisted micro-cutting auxiliary agent, which comprises the following steps: adding distilled water and a NaCl aqueous solution with the mass concentration of 1-2% into the citrus unshiu powder; stirring for 20-30 min at the temperature of 40-50 ℃, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15-20 min, and obtaining an extract mixture of emperor orange peel powder; and (3) carrying out steam distillation on the extracted mixture of the emperor orange powder, and collecting fractions to obtain the emperor orange essential oil. The mandarin orange essential oil has antibacterial effect on Staphylococcus aureus.
Description
Technical Field
The invention relates to the technical field of essential oil extraction, in particular to a method for improving the extraction rate of citrus aurtantium essential oil by using an ultrasonic-assisted micro-cutting auxiliary agent and application of the method for inhibiting staphylococcus aureus.
Background
The citrus fruits are subtropical fruits with the largest yield and the widest distribution in southern areas in China, are sweet and full in taste, rich in nutrient substances, rich in various vitamins and trace elements, fresh and pleasant in aroma and bright in color and luster, and are deeply favored by consumers. The pharmacological activity and physiological activity, low toxicity and economic feasibility of the citrus components cause great enthusiasm for plant research in academia. In recent years, the processing of oranges and the deep utilization of byproducts are increasing day by day, and oranges and byproducts thereof have certain effects of protecting heart, preventing cardiovascular and cerebrovascular diseases, resisting inflammation, resisting tumor and cancer.
The citrus plant belongs to citrus plants of the genus emperor, also called tribute citrus, belongs to tropical and subtropical fruits, is a hybrid variety of citrus and orange, is rich in nutrition, and is rich in various vitamins, trace elements, mineral substances, organic acids and the like. The essential oil of emperor orange is an aromatic compound which is abundantly present in oil sacs or oil glands of the pericarp, is mainly distributed in the outer skin of the pericarp, can be dissolved in alcohol, ether and natural oil, but is not dissolved in water. The specific content and composition of a complex mixture of approximately 400 compounds of citrus essential oil depends on the species of citrus. Essential oil extracted from the pericarp of citrus unshiu, which is insoluble in water and has an aromatic odor. The citrus peel essential oil has the effects of promoting gastrointestinal tract digestion, relieving cough, reducing sputum, dissolving gallstone, diminishing inflammation, inhibiting bacteria, resisting oxidation and the like, can be used as a flavoring agent of beverages, cake and fruit foods, can also be used as a flavoring agent of daily necessities such as perfume, cleaning agent and the like, is natural and environment-friendly, and saves cost.
Disclosure of Invention
The invention aims to provide a method for improving the extraction rate of citrus aurtantium essential oil by using an ultrasonic-assisted micro-cutting auxiliary agent and application of the method in inhibiting staphylococcus aureus.
In order to solve the technical problem, the invention provides a method for improving the extraction rate of essential oil of citrus unshiu by using an ultrasonic-assisted micro-cutting auxiliary agent, which comprises the following steps:
step 1: preparing citrus peel of citrus of emperor into citrus powder of emperor;
step 2: adding distilled water and a NaCl aqueous solution with the mass concentration of 1-2% into the citrus unshiu powder; stirring for 20-30 min at 40-50 ℃ under heat preservation, adding zeolite, performing ice bath ultrasonic auxiliary treatment for 15-20 min to obtain an extract mixture (suspension) of emperor orange peel powder;
the citrus emperor powder comprises the following components: distilled water is in a mass ratio of 1: 18-22;
the dosage of the emperor orange peel powder, the NaCl aqueous solution and the zeolite is as follows: (10-20) mL (200-400) and (1-3) g;
and step 3: and (3) distilling the mixture obtained by leaching the emperor orange powder in the step (2) by using water vapor at the temperature of 200-220 ℃ for 2-3 h, and collecting fractions at the temperature of 100 +/-0.5 ℃ to obtain the emperor orange essential oil.
The improvement of the method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent comprises the following steps:
in the step 2: the ultrasonic power is 400-500 w.
The method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent is further improved as follows:
the step 1 is as follows: citrus aurantium peel (obtained by peeling fresh Citrus aurantium) with 0.05% CaCl2And (4) cleaning the water solution, drying in the shade, and then crushing (sieving by a sieve of 40-80 meshes) to obtain the citrus emperor powder.
The method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent is further improved as follows:
the pulverization in the step 1 is to pulverize to pass through a 60-mesh sieve (pulverize with a pulverizer).
The method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent is further improved as follows:
the step 2 is as follows: adding distilled water and a NaCl aqueous solution with the mass concentration of 1.5% into the citrus unshiu powder; keeping the temperature at 45 ℃, magnetically stirring for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, wherein the ultrasonic power is 450w, and obtaining an extraction mixture (suspension) of emperor orange peel powder;
the citrus emperor powder comprises the following components: distilled water 1: 20 in mass ratio;
the dosage of the emperor orange peel powder, the NaCl aqueous solution and the zeolite is as follows: (10-20) mL (200-400) and (1-3) g.
The method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent is further improved as follows:
and step 3: the steam distillation temperature is 220 ℃, and the steam distillation time is 2 h.
The invention also provides the application of the citrus emperor essential oil prepared by the method, which comprises the following steps: inhibiting Staphylococcus aureus.
Compared with the traditional method for extracting the citrus essential oil of the emperor citrus, the method provided by the invention has the advantages that the extraction rate and the extraction efficiency of the citrus essential oil of the emperor citrus extracted by the ultrasonic-assisted micro-cutting auxiliary agent are obviously improved.
The invention takes staphylococcus aureus as an indicator bacterium, and verifies that the emperor orange essential oil has relatively high in-vitro bacteriostatic effect.
In the present invention, the ice bath ultrasound-assisted treatment after zeolite addition is to prevent bumping, since high temperatures can cause thermal decomposition or oxidation of essential oils.
The invention has the technical advantages that:
1. according to the method for improving the extraction rate of the citrus unshiu essential oil by using the ultrasonic-assisted micro-cutting auxiliary agent, under the extraction condition, the extraction rate of the citrus unshiu essential oil is 8.92% when the citrus unshiu essential oil is subjected to steam distillation for 2 hours, the extraction rate of the citrus unshiu essential oil is 4.46% when the citrus unshiu essential oil is subjected to a traditional steam distillation method for 3 hours, and the main chemical components and the relative content of the citrus unshiu essential oil are measured to show that the main components of the citrus unshiu essential oil are between 5 and 60 minutes through GC-MS gas chromatography-mass spectrometry combined technology (figure 8).
2. The citrus essential oil of the emperor orange has a certain bacteriostatic action on staphylococcus aureus, and the minimum bacteriostatic concentration MIC of the citrus essential oil of the emperor orange is 4mg/mL, and the minimum bactericidal concentration MBC of the citrus essential oil of the emperor orange is 8 mg/mL.
In conclusion, the difference of chemical active ingredients of the plant essential oil is large under different extraction processes, the key point of research and development of the citrus essential oil of the emperor citrus lies in the investigation and optimization of different extraction process conditions, and by optimizing the extraction process of the citrus essential oil of the emperor citrus, important theoretical basis and technical basis are provided for the application of the citrus essential oil of the emperor citrus in the aspects of deep development of external natural bacteriostatic products and the like.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a graph of the results of experiments conducted in accordance with the present invention to determine the effect of varying particle sizes on the extraction yield of citrus essential oil from an emperor citrus;
FIG. 2 is a graph of the results of experiments conducted with different ratios of feed to solution on the effect of the extraction rate of citrus essential oil from an emperor citrus;
FIG. 3 is a graph of the results of experiments conducted with different ultrasonic powers on the effect of the extraction rate of citrus essential oil from an emperor citrus according to the present invention;
FIG. 4 is a graph of the results of experiments conducted with different ultrasound times of the present invention on the effect of citrus essential oil extraction from the emperor citrus;
FIG. 5 is a graph of the results of experiments conducted to determine the effect of different distillation temperatures on the extraction yield of citrus essential oil from an citrus unshiu of the emperor citrus in accordance with the present invention;
FIG. 6 is a graph of the results of tests of the effect of different distillation times on the extraction rate of citrus essential oil from an emperor citrus in accordance with the practice of the present invention;
FIG. 7 is a graph of the results of experiments conducted in accordance with the present invention to determine the effect of different NaCl concentrations on the extraction yield of citrus essential oil from an emperor citrus;
FIG. 8 is a graph showing the results of tests on the effect of different distillation times of steam distillation and ultrasonic-assisted micro-cutting aids on the extraction rate of citrus essential oil from the emperor citrus;
FIG. 9 is a GC-MS total ion flux plot of an optimized citrus unshiu essential oil of the present invention.
Detailed Description
The invention will now be further described with reference to specific examples, which are provided for the purpose of illustration.
The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the examples of the present invention are commercially available unless otherwise specified.
Peeling fresh Citrus Auranthi to obtain Citrus Auranthi peel, and adding 0.05% CaCl2Cleaning with water solution, and drying in the shade; the orange peel of the emperor orange after being cleaned and dried in the shade is obtained; orange peel of emperor orange and 0.05% of CaCl2The dosage ratio of the aqueous solution is as follows: 1 kg/6-8L; the drying in the shade is naturally drying in the shade to constant weight for about 72 hours.
The ultrasonic frequency is conventional 20 KHZ.
The extraction rate (%) of the citrus essential oil of the emperor citrus is equal to the volume (g) of the essential oil/the mass (g) of the citrus powder of the emperor citrus multiplied by 100%.
Example 1, a method for improving an extraction rate of an essential oil of citrus unshiu by using an ultrasonic-assisted micro-cutting auxiliary agent, sequentially performing the following steps:
(1) processing the orange peel of the emperor oranges after being cleaned and dried in the shade by a tissue crusher and then sieving the orange peel with a 40-mesh sieve to obtain emperor orange powder;
(2) adding 20 times of distilled water by mass into 10g of emperor orange powder, adding a NaCl solution with the mass concentration of 3%, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, and obtaining an extraction mixture of emperor orange peel powder, wherein the ultrasonic power is 450 w.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 200mL, 3 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus unshiu powder in the step (2) at 220 ℃ for 2h, and collecting fractions at 100 ℃ to obtain 0.782g of unshiu essential oil.
(1) after being cleaned and dried in the shade, the citrus peel of the citrus emperor is processed by a tissue crusher and then is sieved by a 60-mesh sieve, so as to obtain citrus emperor powder;
(2) adding 18 times of distilled water by mass into 10g of emperor orange powder, adding a NaCl solution with the mass concentration of 1%, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 20min, and carrying out ultrasonic power at 500w to obtain an extraction mixture of emperor orange peel powder.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 180mL, 3 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus powder of the emperor citrus in the step (2) at 200 ℃ for 3h, and collecting fractions at 100 ℃ to obtain 0.825g of emperor citrus essential oil.
Embodiment 3, a method for improving the extraction rate of citrus aurtantium essential oil by using an ultrasonic-assisted micro-cutting auxiliary agent, which sequentially comprises the following steps:
(1) processing the orange peel of the emperor orange after being cleaned and dried in the shade by a tissue crusher, and sieving by a sieve of 80 meshes to obtain emperor orange powder;
(2) adding 18 times of distilled water by mass into 10g of emperor orange powder, adding 2% NaCl solution with mass concentration, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 20min, and obtaining an extraction mixture of emperor orange peel powder, wherein the ultrasonic power is 400 w.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 180mL, 2 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus powder of the emperor citrus in the step (2) at 200 ℃ for 2h, and collecting fractions at 100 ℃ to obtain 0.838g of emperor citrus essential oil.
Embodiment 4, a method for improving the extraction rate of citrus aurtantium essential oil by using an ultrasonic-assisted micro-cutting auxiliary agent, which sequentially comprises the following steps:
(1) processing the orange peel of the emperor oranges after being cleaned and dried in the shade by a tissue crusher and then sieving the orange peel with a 60-mesh sieve to obtain emperor orange powder;
(2) adding 20 times of distilled water by mass into 10g of emperor orange powder, adding a NaCl solution with the mass concentration of 2%, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, and obtaining an extraction mixture of emperor orange peel powder, wherein the ultrasonic power is 450 w.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 200mL, 3 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus unshiu powder in the step (2) at 220 ℃ for 2h, and collecting fractions at 100 ℃ to obtain 0.746g of unshiu essential oil.
Example 5, a method for improving an extraction rate of an essential oil of citrus unshiu by using an ultrasonic-assisted micro-cutting aid, sequentially performing the following steps:
(1) processing the orange peel of the emperor oranges after being cleaned and dried in the shade by a tissue crusher and then sieving the orange peel with a 60-mesh sieve to obtain emperor orange powder;
(2) adding 20 times of distilled water by mass into 10g of emperor orange powder, adding a NaCl solution with the mass concentration of 1.5%, heating to 40-50 ℃, keeping the temperature for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, and carrying out ultrasonic power at 450w to obtain an extraction mixture of emperor orange peel powder.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 200mL, 2 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus unshiu powder in the step (2) at 220 ℃ for 2h, and collecting fractions at 100 ℃ to obtain 0.892g of unshiu essential oil.
Example 6, a method for improving an extraction rate of an essential oil of citrus unshiu by using an ultrasonic-assisted micro-cutting aid, sequentially comprising the following steps:
(1) processing the orange peel of the emperor oranges after being cleaned and dried in the shade by a tissue crusher and then sieving the orange peel with a 40-mesh sieve to obtain emperor orange powder;
(2) adding 22 times of distilled water by mass into 10g of emperor orange powder, adding a NaCl solution with the mass concentration of 3%, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, and obtaining an extraction mixture of emperor orange peel powder, wherein the ultrasonic power is 400 w.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 220mL and 2 g.
(3) And (3) extracting the mixture of the citrus unshiu powder prepared in the step (2), performing steam distillation at 240 ℃ for 1h, and collecting fractions at 100 ℃ to obtain 0.724g of the citrus unshiu essential oil.
Example 7, a method for improving an extraction rate of an essential oil of citrus unshiu with an ultrasonic-assisted micro-cutting aid, sequentially comprising the following steps:
(1) processing the orange peel of the emperor orange after being cleaned and dried in the shade by a tissue crusher, and sieving by a sieve of 80 meshes to obtain emperor orange powder;
(2) adding 22 times of distilled water by mass into 10g of emperor orange powder, adding 1% NaCl solution with mass concentration, heating to 40-50 ℃, preserving heat for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 25min, and obtaining an extraction mixture of emperor orange peel powder, wherein the ultrasonic power is 500 w.
The material-liquid ratio of the citrus unshiu powder to the NaCl solution to the zeolite is as follows: 10g, 220mL and 3 g.
(3) And (3) carrying out steam distillation on the mixture obtained by leaching the citrus powder of the emperor citrus in the step (2) at 180 ℃ for 1h, and collecting fractions at 100 ℃ to obtain 0.738g of emperor citrus essential oil.
In the invention process, in order to fully consider the influence of extraction conditions of different factors on the extraction rate of the citrus essential oil of the emperor citrus, the following experiments are carried out:
setting 10g of emperor orange powder, a NaCl aqueous solution with the mass concentration of 1.5%, and the dosage of the emperor orange peel powder, the NaCl aqueous solution and the zeolite is 10g, 200mL and 2 g;
(1) and (3) experimental design:
different crushing degrees: taking washed and dried citrus peel of the emperor orange, cutting and crushing, and respectively crushing the orange peel and sieving the crushed orange peel with 20, 40, 60, 80 and 100 meshes to obtain samples with different particle sizes. Respectively weighing 10g of citrus unshiu powder with different sizes, adding 20 times of distilled water, soaking with 1.5% NaCl, adding zeolite, performing ultrasonic auxiliary treatment in ice bath, performing steam distillation at 220 ℃ for 2h, repeating the test for 3 times, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening out the optimal particle size for extraction.
② different feed-liquid ratios: respectively weighing 10g of emperor orange powder sieved by a 60-mesh sieve, respectively adding 16, 18, 20, 22, 24 and 26 times of distilled water, soaking by using NaCl with the concentration of 1.5%, then adding zeolite, carrying out ice-bath ultrasonic auxiliary treatment, carrying out steam distillation at 220 ℃ for 2h, repeating the test for 3 times, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening out the optimal material-liquid ratio of extraction.
③ different ultrasonic powers: respectively weighing 10g of emperor orange powder sieved by a 60-mesh sieve, adding 20 times of distilled water, soaking by using 1.5% NaCl, adding zeolite ice bath for ultrasonic auxiliary treatment, respectively measuring the ultrasonic power of 350w, 400w, 450w, 500w and 550w, distilling for 2h by using steam at 220 ℃, repeating the test for 3 times, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening out the optimal ultrasonic power for extraction.
Fourthly, different ultrasonic time: respectively weighing 10g of citrus unshiu powder which is sieved by a 60-mesh sieve, adding 20 times of distilled water, soaking by using NaCl with the concentration of 1.5%, adding zeolite, carrying out ice bath and ultrasonic auxiliary treatment, carrying out ultrasonic power of 450w, carrying out ultrasonic time of 5min, 10min, 15min, 20min, 25min and 30min, carrying out steam distillation at 220 ℃ for 2h, repeating 3 times of test each time, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening the optimal ultrasonic time for extraction.
Different distillation temperatures: respectively weighing 10g of emperor orange powder which is sieved by a 60-mesh sieve, adding 20 times of distilled water, soaking by using 1.5% NaCl, adding zeolite ice bath for ultrasonic auxiliary treatment, wherein the ultrasonic power is 450w, the ultrasonic time is 15min, carrying out steam distillation for 2h at the distillation temperatures of 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃ and 220 ℃, repeating the test for 3 times each time, collecting and measuring the weight of essential oil, and calculating the extraction rate, so as to screen out the optimal distillation temperature for extraction.
Sixthly, different distillation time: respectively weighing 10g of citrus unshiu powder which is sieved by a 60-mesh sieve, adding 20 times of distilled water, soaking by using NaCl with the concentration of 1.5%, adding zeolite ice bath for ultrasonic auxiliary treatment, performing ultrasonic power of 450w for 15min, performing steam distillation for 1h, 2h, 3h, 4h, 5h and 6h at the distillation temperature of 220 ℃, repeating the test for 3 times, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening out the optimal distillation time for extraction.
Different NaCl concentrations: respectively weighing 10g of citrus unshiu powder which is sieved by a 60-mesh sieve, adding 20 times of distilled water, soaking in NaCl concentration of 0.5%, 1%, 1.5%, 2% and 2.5%, respectively, adding zeolite ice bath ultrasonic wave auxiliary treatment, carrying out ultrasonic power of 450w, carrying out ultrasonic treatment for 15min, carrying out steam distillation at the distillation temperature of 220 ℃ for 2h, repeating 3 times of tests each time, collecting and measuring the weight of essential oil, and calculating the extraction rate, thereby screening out the optimal NaCl concentration for extraction.
The results of the extraction rate of the citrus unshiu essential oil of emperor orange are shown in fig. 1-7.
As shown in fig. 1, when the citrus size particles were reduced from 60 mesh to 100 mesh, the extraction yield of the citrus essential oil from the emperor citrus decreased dramatically, probably because the citrus powder particle size was too small and most of the volatile material was lost during the tissue disruption process;
as shown in fig. 2, when the feed liquor ratio is 20 times, the extraction rate of the citrus essential oil of the emperor citrus is high;
as shown in fig. 3, when the ultrasonic power is greater than 450w, the extraction rate of the citrus unshiu essential oil tends to decrease, which is probably because the cavitation of ultrasonic disruption sufficiently breaks the citrus peel, and at the same time, the cavitation causes the local temperature to increase and part of volatile substances to escape;
as shown in fig. 4, the extraction rate of the citrus unshiu essential oil decreases sharply with the increase of the ultrasonic time, which is probably because the temperature rises sharply due to the cavitation over time and volatile substances escape;
as shown in fig. 5, when the distillation temperature was 220 ℃, the extraction rate of the citrus aurtantium essential oil was gradually decreased, which is probably because the high temperature causes oxidation of the heat-sensitive essential oil component, resulting in the decrease of the extraction rate;
as shown in FIG. 6, the extraction rate of the essential oil of the emperor orange also shows a slow increase after 2h of distillation time.
As shown in fig. 7, as the NaCl concentration increased from 1.5% to 2.5%, the extraction rate of the citrus unshiu essential oil showed a tendency to decrease, probably due to the adhesion of the essential oil to the surface layer of the citrus peel caused by the NaCl hydration.
As can be seen from fig. 1 to 7, different crushing particle sizes, material-liquid ratios, ultrasonic powers, ultrasonic times, distillation temperatures, distillation times, and NaCl concentrations all have significant effects on the extraction rate of citrus essential oil from citrus emperor.
Comparative example 1: a steam distillation process comprising the steps of:
(1) processing the orange peel of the emperor oranges after being cleaned and dried in the shade by a tissue crusher and then sieving the orange peel with a 60-mesh sieve to obtain emperor orange powder;
(2) adding 20 times of distilled water by mass into 10g of citrus unshiu powder, and leaching at 40-50 ℃ for 1h to obtain an infusion mixture (suspension) of citrus unshiu powder;
(3) and (3) carrying out steam distillation on the extract mixture of the citrus unshiu powder obtained in the step (2) at 220 ℃ for different time (specifically shown in figure 8), and collecting fractions at 100 ℃ to obtain the citrus unshiu essential oil.
The corresponding relationship between the distillation time and the extraction rate of the citrus essential oil of the citrus unshiu is shown in the steam distillation method of fig. 8.
The corresponding relationship between the distillation time and the extraction rate of the citrus essential oil of the emperor citrus is shown in the ultrasonic-assisted micro-cutting auxiliary agent method in figure 8.
As shown in fig. 8, the conventional steam distillation method and the ultrasonic-assisted micro-cutting auxiliary agent method show an increasing trend along with the increase of the extraction time, the extraction rate of the citrus aurea essential oil is increased rapidly and then slowly along with the extension of the extraction time, and the extraction rate of the ultrasonic-assisted micro-cutting auxiliary agent method is significantly higher than that of the conventional steam distillation method.
As can be seen from FIG. 8, the extraction rate of the essential oil of the emperor orange extracted by the ultrasonic-assisted micro-cutting auxiliary agent method is significantly higher than that of the conventional steam distillation method.
The results of measuring the composition and relative content of the citrus essential oil of emperor citrus obtained by the present invention by GC-MS are shown in fig. 9. A-E in FIG. 9 represent the main 5 components of the citrus essential oil of emperor citrus; alpha-pinene, beta-pinene, myrcene, limonene and linalool.
The emperor orange essential oil prepared by the extraction method of the emperor orange essential oil of the embodiments 1 to 7 performs a bacteriostatic test on staphylococcus aureus.
(1) Test strains: staphylococcus aureus (Staphylococcus aureus ATCC43300) was purchased from Beijing Biodepositary.
(2) Determining the bacteriostatic circle: adopting filter paper sheet agar plate diffusion method, using pipette to transfer 20. mu.L of citrus unshiu essential oil drop onto sterilized filter paper (d ═ 6mm), after the filter paper sheet is fully absorbed, placing on culture medium plate (bacterial liquid concentration is 10) coated with staphylococcus aureus7cfu/mL, 100. mu.L) in each group, and sterile water was used as a negative control and streptomycin was used as a positive control (concentration 5. mu.g/mL) and incubated in a 37 ℃ incubator for 24 h. Observing and recording the existence and the diameter of the bacteriostatic circle as the standard for judging the bacteriostatic action, measuring the diameter of the bacteriostatic circle by adopting a cross method, and taking the average value as a measurement result. The diameter of the inhibition zone is more than 20mm, the sensitivity is high, the diameter of the inhibition zone is 15-20 mm, the sensitivity is medium, the diameter of the inhibition zone is 10-15 mm, and the sensitivity is low, wherein the diameter of the inhibition zone is less than 10 mm.
(3) 3-5 staphylococcus aureus with similar morphology are picked by using an inoculating loop, inoculated in 4-5ml of TSB broth and incubated for 2-6h at 37 ℃. The logarithmic phase bacterial liquid after enrichment is corrected to 0.5 McLeod's turbidimetric standard by normal saline or TSB broth culture medium, and the concentration is about 1-2 × 108CFU/mL. The bacterial suspension was diluted 1: 100 with TSB broth for use. Note that the prepared inoculum should be inoculated within 15 minutes and an aliquot taken for subculture on non-selective agar plates to check inoculum purity.
Taking 13 sterile test tubes (13X 100mm), arranging in a row, adding 1mL of TSB broth into each tube except 1.6mL of TSB broth into the 1 st tube, adding 0.4mL of citrus essential oil of the citrus unshiu into the 1 st tube, uniformly mixing, sucking 1mL to the 2 nd tube, uniformly mixing, sucking 1mL to the 3 rd tube, diluting to the 11 th tube in a multiple ratio manner continuously, sucking 1mL from the 11 th tube, discarding, taking the 12 th tube as a growth control without a medicament, and taking the 13 th tube as a positive control. At this time, the drug concentration in each tube was 256, 128, 64, 32, 16, 8, 4, 2, 1, 0.5, and 0.25mg/mL in this order. Then, 1mL of each of the prepared inocula was added to each tube to give a final bacterial liquid concentration of about 5X 105CFU/mL. The drug concentrations of the 1 st tube to the 11 th tube are respectively 128, 64, 32, 16, 8, 4, 2, 1, 0.5, 0.25 and 0.125 mug/ml.
(4) Minimum Inhibitory Concentration (MIC): and (3) carrying out MIC test by using a 10mL test tube by adopting a two-fold dilution method, fully and uniformly mixing according to the operation (3), repeating the operation for three times each time, placing the test tube in a constant-temperature incubator at 37 ℃ for 24h, observing whether the test tube is turbid, and marking the test tube as Minimum Inhibitory Concentration (MIC) of the emperor orange essential oil on the staphylococcus aureus by using a tube without turbidity.
(5) Determination of Minimum Bactericidal Concentration (MBC): and (3) uniformly coating the solution corresponding to the MIC value of each sample in the step (4) in a TSA culture medium by adopting an agar medium plate method, and performing inverted culture in a constant-temperature incubator at 37 ℃ for 24 hours. The medium was observed for growth of Staphylococcus aureus and plates without growing colonies were recorded as the lowest bactericidal concentration (MBC).
The results of the measurement were as follows:
TABLE 1
As can be seen from the above table 1, the Kingy citrus essential oil obtained by the extraction method of the Kingy citrus essential oil has a certain bacteriostatic action on Staphylococcus aureus, and both MIC and MBC are below 16 mg/mL. Wherein the citrus essential oil of emperor orange obtained in example 5 has the best bacteriostatic effect. According to the invention, the citrus essential oil of the emperor citrus is extracted by combining ultrasonic-assisted extraction and a steam distillation method, so that the extraction time of the essential oil is effectively shortened, the efficiency is improved, and meanwhile, the bacteriostatic activity of the citrus essential oil of the emperor citrus on staphylococcus aureus is remarkably improved.
According to the change of the extraction rate of the citrus essential oil of the emperor citrus in the embodiments 1 to 7, the sodium salt ion micro-cutting auxiliary agent and the ultrasonic-assisted steam distillation method are combined, so that the extraction rate of the citrus essential oil of the emperor citrus is improved.
Comparative example 2, elimination of "zeolite addition" in step 2) of example 5, and corresponding elimination of "ice bath ultrasound-assisted treatment", the rest being identical to example 5.
Comparative example 3, only the "zeolite addition" of step 2) of example 5 was omitted, namely, the ice bath ultrasonic wave-assisted treatment was directly carried out after the heat preservation for 25min, and the rest was identical to example 5.
Comparative example 4, only the 'NaCl solution' added in the step 2) of the example 5 is omitted, namely, distilled water is added into the citrus powder of the emperor orange, then the citrus powder is directly heated to 40-50 ℃ and is kept warm for 25min, then zeolite is added, ice bath is carried out, ultrasonic wave auxiliary treatment is carried out, and the rest is the same as that of the example 5.
Comparative example 5-1, the "2% NaCl aqueous solution" was changed to "2% KCl aqueous solution", and the remainder was the same as in example 5.
Comparative example 5-2, 2% CaCl instead of "2% NaCl solution2Aqueous solution ", the rest is identical to example 5.
Comparative examples 5 to 3, changing "2% NaCl solution" to "2% Na2CO3Aqueous solution ", the rest is identical to example 5.
The product obtained in the above comparative example was subjected to the above bacteriostatic test, and the results are shown in table 2 below.
TABLE 2
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (7)
1. The method for improving the extraction rate of the essential oil of the citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent is characterized by comprising the following steps of:
step 1: preparing citrus peel of citrus of emperor into citrus powder of emperor;
step 2: adding distilled water and a NaCl aqueous solution with the mass concentration of 1-2% into the citrus unshiu powder; stirring for 20-30 min at the temperature of 40-50 ℃, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15-20 min, and obtaining an extract mixture of emperor orange peel powder;
the citrus emperor powder comprises the following components: distilled water 1: 18-22 mass ratio;
the dosage of the emperor orange peel powder, the NaCl aqueous solution and the zeolite is as follows: (10-20) mL (200-400) and (1-3) g;
and step 3: and (3) distilling the mixture obtained by leaching the emperor orange powder in the step (2) by using water vapor at the temperature of 200-220 ℃ for 2-3 h, and collecting fractions at the temperature of 100 +/-0.5 ℃ to obtain the emperor orange essential oil.
2. The method for improving the extraction rate of the essential oil of citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent according to claim 1, wherein the ultrasonic-assisted micro-cutting auxiliary agent comprises the following steps:
in the step 2: the ultrasonic power is 400-500 w.
3. The method for improving the extraction rate of the essential oil of citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent according to claim 1 or 2, is characterized in that:
the step 1 is as follows: 0.05% CaCl is used for orange peel of emperor orange2Cleaning with water solution, drying in the shade, and pulverizing to obtain mandarin orange powder.
4. The method for improving the extraction rate of the essential oil of citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent according to claim 3, wherein the ultrasonic-assisted micro-cutting auxiliary agent is used for improving the extraction rate of the essential oil of citrus unshiu, and is characterized in that:
the crushing in the step 1 is to crush and pass through a 60-mesh sieve.
5. The method for improving the extraction rate of the essential oil of citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent according to claim 4, wherein the ultrasonic-assisted micro-cutting auxiliary agent comprises the following steps:
the step 2 is as follows: adding distilled water and a NaCl aqueous solution with the mass concentration of 1.5% into the citrus unshiu powder; keeping the temperature at 45 ℃, magnetically stirring for 25min, adding zeolite, carrying out ice bath ultrasonic auxiliary treatment for 15min, wherein the ultrasonic power is 450w, and obtaining an extract mixture of emperor orange peel powder;
the citrus emperor powder comprises the following components: distilled water 1: 20 in mass ratio;
the dosage of the emperor orange peel powder, the NaCl aqueous solution and the zeolite is as follows: (10-20) mL (200-400) and (1-3) g.
6. The method for improving the extraction rate of the essential oil of citrus unshiu by using the ultrasonic-assisted micro-cutting auxiliary agent according to claim 5, wherein the ultrasonic-assisted micro-cutting auxiliary agent is used for improving the extraction rate of the essential oil of citrus unshiu, and is characterized in that:
and step 3: the steam distillation temperature is 220 ℃, and the steam distillation time is 2 h.
7. Use of an essential oil of citrus unshiu, obtained by the process according to any one of claims 1 to 6: inhibiting Staphylococcus aureus.
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