CN114869847A - Amomum katsumadai essential oil microemulsion and preparation method thereof - Google Patents

Amomum katsumadai essential oil microemulsion and preparation method thereof Download PDF

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CN114869847A
CN114869847A CN202210329071.0A CN202210329071A CN114869847A CN 114869847 A CN114869847 A CN 114869847A CN 202210329071 A CN202210329071 A CN 202210329071A CN 114869847 A CN114869847 A CN 114869847A
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郇志博
褚祚晨
薛书敏
罗金辉
徐志
王明月
段云
韩丙军
吕岱竹
马晨
张群
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Analysis & Testing Center Chinese Academy Of Tropical Agricultural Sciences
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Abstract

The invention provides alpinia katsumadai essential oil microemulsion and a preparation method thereof, and the preparation method comprises the following steps: (1) mixing sorbitan fatty acid ester with absolute ethyl alcohol to obtain a mixed surfactant A; mixing tween 80 and absolute ethyl alcohol to obtain a mixed surfactant B; (2) dripping surfactant A into the katsumadai seed essential oil while shaking and stirring to obtain a primary katsumadai seed essential oil mixed oil phase; (3) dripping the mixed surfactant B while shaking and stirring, and adding a mixed aqueous solution of hydrochloric acid and sodium chloride to obtain a katsumadai seed essential oil mixed oil phase; (4) mixing the semen Alpiniae essential oil mixed oil phase with water under stirring, and high-speed shearing to obtainClarifying or semitransparent to obtain the katsumadai seed essential oil microemulsion, and the katsumadai seed essential oil microemulsion prepared by the invention has excellent oxidation resistance and can resist DPPH free radicals and ABTS + The free radical has high cleaning capacity, obviously improved stability, uniform particle size distribution and good dispersibility.

Description

Amomum katsumadai essential oil microemulsion and preparation method thereof
Technical Field
The invention relates to the technical field of plant essential oil processing, and particularly relates to alpinia katsumadai essential oil microemulsion and a preparation method thereof.
Background
Microemulsions (MEs) are thermodynamically stable, transparent dispersion systems formed spontaneously from surfactants, oil, water (or brine) and cosurfactants. The dispersed phase particles in the dispersion system are much smaller than those of common emulsion, generally between 10 and 100nm, and are mainly divided into three types: oil-in-water (O/W), bicontinuous, and water-in-oil (W/O). The microemulsion has the advantages that the microemulsion can be widely applied to the fields of food, chemical engineering, medicines and the like, for example, in the field of food, the microemulsion can improve the solubility of substances such as insoluble nutrient substances, flavor enhancers and the like in food, can resist the influence of unstable ingredients on external environment such as oxygen, light, heat, acid and alkali and the like, and can prevent the quality of the food from being deteriorated in the processing and preservation processes.
In recent years, many essential oils extracted from plants have been found to have antioxidant, antimicrobial, anti-inflammatory, free radical scavenging, antitumor and cytoprotective effects, but there are still few studies on plant essential oils in microemulsion systems. With the continuous and deep research of different microemulsion systems, the method has important practical significance for expanding the application range of the microemulsion in various fields. For the design of the microemulsion formula, the selection of the surfactant, the ratio of the surfactant to the cosurfactant (Km value), the ratio of the surfactant to the essential oil (S/O value), the parameter conditions of the mixing process and the like all have important influences on the final uniformity and stability of the microemulsion system, and the efficacy and performance of the microemulsion are greatly different. At present, the study on the alpinia katsumadai essential oil microemulsion is not reported, and the invention provides a preparation process of microemulsion for alpinia katsumadai essential oil and provides a technical basis for the application of the alpinia katsumadai essential oil microemulsion.
Disclosure of Invention
In view of the above, the invention provides the alpinia katsumadai seed essential oil microemulsion and the preparation method thereof, and the alpinia katsumadai seed essential oil microemulsion with high oxidation resistance and high stability is prepared.
The technical scheme of the invention is realized as follows:
the invention provides a preparation method of alpinia katsumadai essential oil microemulsion, which comprises the following steps:
step 1: mixing sorbitan fatty acid ester and absolute ethyl alcohol according to the mass ratio of 1-2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to the mass ratio of 2-4:1 to obtain a mixed surfactant B for later use;
step 2: adding the katsumadai seed essential oil into a vortex oscillator, carrying out oscillation treatment, and dripping the mixed surfactant A while carrying out oscillation stirring to obtain a primary katsumadai seed essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 2-4: 1;
and step 3: the primary alpinia katsumadai essential oil mixed oil phase is vibrated and stirred again, the mixed surfactant B is dripped, and meanwhile, the hydrochloric acid and sodium chloride mixed aqueous solution is added to obtain the alpinia katsumadai essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12-14: 1;
and 4, step 4: according to the mass ratio of 2: and 8, adding water into the katsumadai seed essential oil mixed oil phase under the stirring state for mixing to obtain katsumadai seed essential oil primary emulsion, and carrying out high-speed shearing until the solution is clear or semitransparent from turbidity to obtain the katsumadai seed essential oil microemulsion.
Further, the mass ratio of the sorbitan fatty acid ester to the absolute ethyl alcohol is 1.5:1, and the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 3: 1.
Further, in the step 2, the alpinia katsumadai essential oil is heated to 35-38 ℃, and then is added into a vortex oscillator, the speed of the vortex oscillator is 300-500rpm, and the dropping speed of the mixed surfactant A is 20-30 ml/min.
Further, in the step 2, after the dropwise addition of the mixed surfactant A is completed, the high-speed magnetic stirring is performed, wherein the speed of the high-speed magnetic stirring is 800-900rpm, and the magnetic stirring time is 50-60 s.
Further, in the step 3, the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12:1, and the mass ratio of the Tween 80 to the absolute ethyl alcohol is 3: 1.
Further, in step 3, the speed of the shaking and stirring is 600-800rpm, and the dropping speed of the mixed surfactant B is 10-20 ml/min.
Further, in step 3, the mixed aqueous solution of hydrochloric acid and sodium chloride is added into the primary alpinia katsumadai essential oil mixed oil phase at a rate of 0.5-1 ml/min.
Further explaining, the mass concentration of the mixed aqueous solution of hydrochloric acid and sodium chloride is 0.15-0.2%, wherein the mass ratio of hydrochloric acid to sodium chloride is 1: 1-2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the alpinia katsumadai essential oil is 4-6: 1.
Further, in step 4, the speed of the high-speed shearing machine is 1200-1500 rpm.
The katsumadai seed essential oil microemulsion prepared by the preparation method is provided.
Compared with the prior art, the invention has the beneficial effects that:
the katsumadai seed essential oil microemulsion prepared by the invention has excellent oxidation resistance, and can be used for treating DPPH free radical and ABTS when the katsumadai seed essential oil microemulsion is 0.7700mg/mL + Free radical scavenging rate of 85% or more for DPPH free radicals and ABTS + Free radical scavengerIC removing device 50 Can reach 0.083mg/mL and 0.203mg/mL, and simultaneously, the katsumadai seed essential oil microemulsion has good stability, uniform particle size distribution and good dispersibility.
The method comprises the following steps of preparing a katsumadai seed essential oil-water mixed solution, and carrying out medium-temperature preliminary emulsification and short-time high-speed magnetic stirring on the katsumadai seed essential oil-water mixed solution by adopting a small amount of surfactant A compounded by sorbitan fatty acid ester and cosurfactant absolute ethyl alcohol to form a certain oil-water interfacial film mobile phase; and then, carrying out secondary emulsification treatment by using a mixed surfactant B formed by combining Tween 80 and absolute ethyl alcohol, and slowly adding a low-concentration hydrochloric acid and sodium chloride mixed aqueous solution at a low speed in a combined manner to form a weakly acidic microemulsion mixed system, so that the microemulsion forming capability of the mixed surfactant is enhanced, and the microemulsion particle size and the polydispersity index PDI are obviously reduced, thereby forming a more stable O/W type microemulsion, effectively improving the oxidation resistance of the Alpinia katsumadai Hayata essential oil, remarkably improving the performance of the Alpinia katsumadai Hayata microemulsion, and enhancing the centrifugal stability, the thermal stability and the low-temperature stability of the Alpinia katsumadai Hayata microemulsion, and being superior to the microemulsifying effect of the Alpinia katsumadai Hayata essential oil by singly using Tween 80 or sorbitan fatty acid ester.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
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 can be obtained commercially without specific description.
Example 1
A preparation method of alpinia katsumadai essential oil microemulsion comprises the following steps:
(1) taking sorbitan fatty acid ester (span-80) and absolute ethyl alcohol, and mixing according to the mass ratio of 1:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to the mass ratio of 2:1 to obtain a mixed surfactant B for later use;
(2) heating the katsumadai seed essential oil to 35 ℃, adding a vortex oscillator for oscillation treatment, dropwise adding the surfactant A while oscillating and stirring, wherein the dropwise adding speed is 20ml/min, the oscillating and stirring speed is 300rpm, and after the dropwise adding is finished, converting to high-speed magnetic stirring at 800rpm for 60s to obtain a primary katsumadai seed essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 4: 1;
(3) the primary alpinia katsumadai essential oil mixed oil phase is added with the mixed surfactant B again at 600rpm while shaking and stirring, the dropping speed is 10ml/min, and meanwhile, the mixed aqueous solution of hydrochloric acid with the mass concentration of 0.2 percent and sodium chloride is added at the speed of 0.5ml/min to obtain the alpinia katsumadai essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 14: 1; the mass ratio of the hydrochloric acid to the sodium chloride is 1: 1; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the katsumadai seed essential oil is 4: 1;
(4) adding water into the katsumadai seed essential oil mixed oil phase in a stirring state of 600rpm according to a mass ratio of 2:8, mixing to obtain katsumadai seed essential oil primary emulsion, and carrying out high-speed shearing at a speed of 1200rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the katsumadai seed essential oil microemulsion.
Example 2
A preparation method of alpinia katsumadai essential oil microemulsion comprises the following steps:
(1) taking sorbitan fatty acid ester (span-80) and absolute ethyl alcohol, and mixing according to the mass ratio of 2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to the mass ratio of 3:1 to obtain a mixed surfactant B for later use;
(2) heating the katsumadai seed essential oil to 38 ℃, adding a vortex oscillator for oscillation treatment, dropwise adding the surfactant A while oscillating and stirring, wherein the dropwise adding speed is 30ml/min, the oscillating and stirring speed is 500rpm, after the dropwise adding is finished, converting to high-speed magnetic stirring of 900rpm for 50s, and mixing the primary katsumadai seed essential oil with an oil phase; the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 3: 1;
(3) dripping the mixed surfactant B into the primary alpinia katsumadai essential oil mixed oil phase while shaking and stirring at 800rpm at the dripping speed of 20ml/min, and simultaneously adding a mixed aqueous solution of hydrochloric acid and sodium chloride with the mass concentration of 0.15% at the speed of 1ml/min to obtain the alpinia katsumadai essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12: 1; the mass ratio of the hydrochloric acid to the sodium chloride is 1: 2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the katsumadai seed essential oil is 6: 1;
(4) adding water into the katsumadai seed essential oil mixed oil phase in a stirring state of 600rpm according to a mass ratio of 2:8, mixing to obtain katsumadai seed essential oil primary emulsion, and carrying out high-speed shearing at a speed of 1500rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the katsumadai seed essential oil microemulsion.
Example 3
A preparation method of alpinia katsumadai essential oil microemulsion comprises the following steps:
(1) taking sorbitan fatty acid ester (span-80) and absolute ethyl alcohol, and mixing according to the mass ratio of 1:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to the mass ratio of 3:1 to obtain a mixed surfactant B for later use;
(2) heating the katsumadai seed essential oil-water mixed solution to 36 ℃, adding a vortex oscillator for oscillation treatment, dropwise adding a surfactant A while carrying out oscillation stirring, wherein the dropwise adding speed is 25ml/min, the oscillation stirring speed is 400rpm, and after the dropwise adding is finished, converting to 850rpm and carrying out high-speed magnetic stirring for 60s to obtain a primary katsumadai seed essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 3: 1;
(3) dropwise adding a mixed surfactant B into the primary alpinia katsumadai essential oil mixed oil phase while shaking and stirring at 700rpm, wherein the dropwise adding speed is 15ml/min, and simultaneously adding a mixed aqueous solution of hydrochloric acid and sodium chloride with the mass concentration of 0.15% at the speed of 0.5ml/min to obtain the alpinia katsumadai essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12: 1; the mass ratio of the hydrochloric acid to the sodium chloride is 1: 2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the katsumadai seed essential oil is 6: 1;
(4) adding water into the katsumadai seed essential oil mixed oil phase in a stirring state of 600rpm according to the mass ratio of 2:8, mixing to obtain katsumadai seed essential oil primary emulsion, and carrying out high-speed shearing at the speed of 1300rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the katsumadai seed essential oil microemulsion.
Example 4
The preparation method of the alpinia katsumadai essential oil microemulsion as in example 3 is characterized in that the preparation method comprises the steps of initially emulsifying at normal temperature and not carrying out high-speed magnetic stirring; the method specifically comprises the following steps:
step 3, adding the katsumadai seed essential oil-water mixed solution into a vortex oscillator at normal temperature for oscillation treatment, dripping the surfactant A while oscillating and stirring, and obtaining a primary katsumadai seed essential oil mixed oil phase after finishing dripping; the mixed surfactant B was continuously added dropwise while shaking and stirring at 700rpm, and the remaining steps were the same as in example 3.
Example 5
The Alpinia katsumadai essential oil microemulsion preparation method as in example 3, except that in step 4, a 5% hydrochloric acid and sodium chloride mixed aqueous solution at a mass concentration of 0.5ml/min is added; the mass ratio of the hydrochloric acid to the sodium chloride is 1: 2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the alpinia katsumadai essential oil is 6: 1.
Comparative example 1
The preparation method of alpinia katsumadai essential oil microemulsion as in example 3 is different in that the adding sequence of the mixed surfactants A and B is changed, and specifically comprises the following steps:
in the step 2, replacing the mixed surfactant A with a mixed surfactant B, wherein the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12: 1;
in the step 3, replacing the mixed surfactant B with a mixed surfactant A, wherein the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 3: 1; the other parameter conditions were the same as in example 3.
Comparative example 2
The preparation method of the alpinia katsumadai essential oil microemulsion as in example 3 is different in that step-by-step secondary emulsification treatment is not carried out, and specifically comprises the following steps:
in the step 1, the mixed surfactant A and the mixed surfactant B with the same dosage as that of the embodiment 3 are directly mixed to be used as a mixed surfactant C for standby;
in the mixing step 2-3, adding the alpinia katsumadai essential oil into a vortex oscillator for oscillation treatment, dropwise adding the mixed surfactant C at the speed of 700rpm while oscillating and stirring, wherein the dropwise adding speed is 15ml/min, and simultaneously, adding a mixed aqueous solution of hydrochloric acid and sodium chloride with the mass concentration of 0.15% at the speed of 0.5ml/min to obtain an alpinia katsumadai essential oil mixed oil phase; the mass ratio of the hydrochloric acid to the sodium chloride is 1: 2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the katsumadai seed essential oil is 6: 1; the other parameters were the same as in example 3.
Example 6
The microemulsion properties of Alpinia katsumadai Hayata essential oil prepared in the above examples and comparative examples were measured and analyzed, including particle size, polydispersity index (PDI) and stability analysis of the microemulsion.
Test materials: alpinia katsumadai Hayata essential oil extracted by supercritical extraction is purchased from Jiangxi Hai Lin spice Co.
The determination method comprises the following steps:
1. microemulsion particle size and polydispersity index (PDI): and (3) measuring the particle size and the polydispersity index (PDI) of the different katsumadai seed essential oil microemulsions by using a Malvern laser particle size analyzer, wherein the measuring temperature is 25 ℃ and the scattering angle is 90 ℃.
2. And (3) centrifugal stability analysis: taking a proper amount of prepared katsumadai seed essential oil microemulsion, centrifuging for 30min at 6000 and 8000r/min, observing whether layering exists, if no layering exists, taking deionized water as a blank control, measuring the absorbance at 315nm before and after centrifugation, and calculating the light transmittance according to a formula (1):
Figure RE-GDA0003740862160000071
in the formula: t, light transmittance; a. the 0 Absorbance of the microemulsion before centrifugation; a. the 1 Absorbance of the microemulsion after centrifugation.
3. Thermal stability analysis: heating appropriate amount of microemulsion in constant temperature water bath at 70 and 90 deg.C for 30 min. The stability of the microemulsions was evaluated by visual observation (phase separation) and light transmittance. Taking deionized water as a blank control, measuring the absorbance of the microemulsion before and after heating at the wavelength of 315nm by using an ultraviolet spectrophotometer, and calculating the light transmittance according to the formula (2):
Figure RE-GDA0003740862160000072
in the formula: a. the 0 Absorbance of the microemulsion before heating; a. the 1 Absorbance of the microemulsion after heating.
4. Low temperature stability analysis: the microemulsion was stored in a low temperature environment of 4 ℃ and the stability of the microemulsion was evaluated by visual observation (phase separation) and transmittance. The light transmittance of the microemulsion on day 14 was measured using an ultraviolet spectrophotometer at a wavelength of 315nm, using deionized water as a blank.
The light transmittance is calculated according to formula (3):
Figure RE-GDA0003740862160000073
in the formula: a. the 0 Absorbance of the microemulsion before low temperature storage; a. the 1 Absorbance of microemulsion on day n after low temperature storage. The measurement results and analysis are shown in the following table 1:
TABLE 1
Figure RE-GDA0003740862160000074
Figure RE-GDA0003740862160000081
As can be seen from the above table, the Alpinia katsumadai essential oil microemulsion prepared in the embodiments 1-5 of the invention has a particle size of less than 15nm, a polydispersity index PDI of less than 0.3, uniform particle size distribution, good dispersibility, and forms a stable O/W type microemulsion, and the Alpinia katsumadai essential oil microemulsion has good centrifugal stability, thermal stability and low temperature stability under certain conditions, respectively, has no delamination and turbidity phenomena in centrifugation, water bath heating and low temperature storage at 6000 r/min and 8000r/min for 14d, has a light transmittance of 100%, and presents a clear, transparent and uniform liquid.
From the comparison of example 3 with comparative examples 1-2, it can be seen that the particle size of the emulsions of comparative examples 1 and 2 is significantly increased, the polydispersity index PD thereof is increased, and at the same time, the stability thereof is significantly reduced. In example 3, compared with examples 4 to 5, it is shown that the particle size and PDI of the emulsion can be further reduced by high-speed magnetic stirring at medium temperature during the preliminary emulsification, and the polydispersity index PDI tends to increase although a certain particle size is maintained when hydrochloric acid with an excessively high concentration is mixed with the mixed aqueous solution of sodium chloride in example 5.
Example 7
The Alpinia katsumadai essential oil microemulsions prepared in the above examples 3-5 and comparative examples 1-2 were analyzed for their antioxidant ability,
(1) scavenging ability for DPPH free radical
Referring to the method of Schlumberger et al (2004), the DPPH radical scavenging ability of Alpinia katsumadai microemulsion was measured, and the DPPH radical scavenging ability of microemulsion was quantified by measuring the absorbance value at 517nm with a spectrophotometer.
Weighing 0.0256g DPPH in 100mL volumetric flask, adding absolute ethanol to constant volume, shaking up to obtain stock solution (6.5X 10) -4 mol/L) are stored in a refrigerator at 4 ℃ and are diluted step by step when in use.
During the measurement, 10mL of DPPH stock solution was aspirated, and the solution was shaken up to a constant volume in a 100mL volumetric flask as a working solution (6.5X 10) -5 mol/L). Sucking a certain amount of semen Alpiniae extract oil and microemulsion, respectively preparing into solution with mass concentration of 0.77mg/mL with anhydrous ethanol, sucking 2mL of the above semen Alpiniae extract oil and microemulsion diluent, and adding 2mL of DPPH working solution (6.5 × 10) - 5 mol/L) are mixed evenly at room temperature, the mixture is reacted for 30min in a dark place, and the absorbance value A at 517nm is measured i (ii) a The absorbance value of 2mL of sample solution with corresponding concentration and 2mL of absolute ethyl alcohol is taken as a background value A j (ii) a The light absorption value of 2mL absolute ethyl alcohol and 2mL DPPH solution is taken as an initial value A k . The experiment was repeated 3 times with vitamin C as a positive control, and the DPPH radical clearance was calculated according to formula (1):
Figure RE-GDA0003740862160000091
simultaneous use of GraphPad Prism 5.0 software, calculating the IC of the Alpinia katsumadai essential oil microemulsion 50 Value, IC 50 The value is the amount of essential oil, IC, required to clear half of DPPH 50 Smaller values indicate greater clearance of DPPH.
(2) Scavenging ability for ABTS free radical
Referring to the GUO et al (2018) procedure, first 0.4mL of a 7.4mmol/L ABTS solution (3 mg ABTS dissolved in 0.735mL distilled water) and 1.43mL of 2.6mmol/L K 2 S 2 O 3 Solution (1 mg K) 2 S 2 O 3 Dissolving in 1.43mL of distilled water), mixing, standing in dark for 12h, diluting with anhydrous ethanol 45 times to make its absorbance value at 734nm be about 0.7 to obtain ABTS + Free radical working solution, and then 4mLABTS + Adding 0.4mL of semen Alpiniae extract oil with mass concentration of 0.77mg/mL and microemulsion prepared with anhydrous ethanol into the free radical working solution, shaking for 10s, mixing, reacting at room temperature in dark for 10min, and measuring absorbance A at 734nm 1 (ii) a The blank is equal amount of absolute ethyl alcohol (A) 0 ). The experiment was repeated 3 times with vitamin C as a positive control and the clearance of ABTS cationic radicals was calculated according to equation (2):
Figure RE-GDA0003740862160000092
simultaneously, the IC of the katsumadai seed essential oil microemulsion is calculated by using GraphPad Prism 5.0 software 50 Value, IC 50 The value is the amount of essential oil, IC, required to clear half of the ABTS 50 Smaller values indicate greater ability to clear ABTS.
The results are given in table 2 below:
TABLE 2
Figure RE-GDA0003740862160000093
As can be seen from the above table, the Alpinia katsumadai essential oil microemulsion prepared by the invention has the DPPH free radical clearance rate and ABTS + The clearance rate of free radicals is obviously higher than that of essential oil (P)<0.05) In particular, the microemulsion of Alpinia katsumadai essential oil prepared in example 3 exhibited an ABTS clearance/% similar to that of vitamin C, and at the same time, exhibited an IC for DPPH radical scavenging 50 And ABTS + Free radical scavenging IC 50 Respectively reach 0.083mg/mL and 0.211 mg/mL. The oxidation resistance of the comparative examples 1-2 is relatively poor compared with that of the example 3, which shows that the prepared alpinia katsumadai seed essential oil microemulsion has the advantages that the performance of the emulsion is remarkably improved, the centrifugal stability, the thermal stability and the low-temperature stability are remarkably enhanced, and the oxidation resistance of the alpinia katsumadai seed essential oil can be effectively ensured.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A preparation method of alpinia katsumadai essential oil microemulsion is characterized by comprising the following steps: the method comprises the following steps:
step 1: mixing sorbitan fatty acid ester and absolute ethyl alcohol according to the mass ratio of 1-2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to the mass ratio of 2-4:1 to obtain a mixed surfactant B for later use;
step 2: adding the katsumadai seed essential oil into a vortex oscillator, carrying out oscillation treatment, and dripping the mixed surfactant A while carrying out oscillation stirring to obtain a primary katsumadai seed essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 2-4: 1;
and step 3: the primary alpinia katsumadai essential oil mixed oil phase is vibrated and stirred again, the mixed surfactant B is dripped, and meanwhile, the hydrochloric acid and sodium chloride mixed aqueous solution is added to obtain the alpinia katsumadai essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the alpinia katsumadai essential oil is 12-14: 1;
and 4, step 4: according to the mass ratio of 2: and 8, adding water into the katsumadai seed essential oil mixed oil phase under the stirring state for mixing to obtain katsumadai seed essential oil primary emulsion, and carrying out high-speed shearing until the solution is clear or semitransparent from turbidity to obtain the katsumadai seed essential oil microemulsion.
2. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 1, wherein the method comprises the following steps: the mass ratio of the mixed surfactant A to the alpinia katsumadai essential oil is 3:1, and the mass ratio of the sorbitan fatty acid ester to the absolute ethyl alcohol is 1: 1.
3. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 2, wherein the method comprises the following steps: in the step 2, the katsumadai seed essential oil is heated to 35-38 ℃, and then added into a vortex oscillator for oscillation treatment; the shaking and stirring speed is 300-500rpm, and the dropping speed of the mixed surfactant A is 20-30 ml/min.
4. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 3, wherein the method comprises the following steps: in the step 2, after the dropwise addition of the mixed surfactant A is completed, high-speed magnetic stirring is carried out, wherein the speed of the high-speed magnetic stirring is 800-900rpm, and the magnetic stirring time is 50-60 s.
5. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 1, wherein the method comprises the following steps: in the step 3, the mass ratio of the mixed surfactant B to the katsumadai seed essential oil is 12:1, and the mass ratio of the Tween 80 to the absolute ethyl alcohol is 3: 1.
6. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 5, wherein the method comprises the following steps: in the step 3, the speed of the shaking and stirring is 600-800rpm, and the dropping speed of the mixed surfactant B is 10-20 ml/min.
7. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 6, wherein the method comprises the following steps: in step 3, the mixed aqueous solution of hydrochloric acid and sodium chloride is added into the primary katsumadai seed essential oil mixed oil phase at the speed of 0.5-1 ml/min.
8. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 7, wherein the method comprises the following steps: the mass concentration of the mixed aqueous solution of hydrochloric acid and sodium chloride is 0.15-0.2%, wherein the mass ratio of hydrochloric acid to sodium chloride is 1: 1-2; the mass ratio of the mixed aqueous solution of hydrochloric acid and sodium chloride to the alpinia katsumadai essential oil is 4-6: 1.
9. The method for preparing the alpinia katsumadai essential oil microemulsion of claim 1, wherein the method comprises the following steps: in step 4, the speed of the high-speed shearing machine is 1200 and 1500 rpm.
10. A Alpinia katsumadai essential oil microemulsion according to any one of claims 1 to 9, which is prepared by the method.
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