CN114869847B - Semen katsumadai essential oil microemulsion and preparation method thereof - Google Patents

Semen katsumadai essential oil microemulsion and preparation method thereof Download PDF

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CN114869847B
CN114869847B CN202210329071.0A CN202210329071A CN114869847B CN 114869847 B CN114869847 B CN 114869847B CN 202210329071 A CN202210329071 A CN 202210329071A CN 114869847 B CN114869847 B CN 114869847B
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semen
katsumadai
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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 semen katsumadai essential oil microemulsion and a preparation method thereof, comprising the following steps: (1) Mixing sorbitan fatty acid ester with absolute ethyl alcohol to obtain a mixed surfactant A; mixing Tween 80 with absolute ethyl alcohol to obtain a mixed surfactant B; (2) Dropwise adding the surfactant A into the semen Alpiniae essential oil while vibrating and stirring to obtain a primary semen Alpiniae essential oil mixed oil phase; (3) Dropwise adding the mixed surfactant B while vibrating and stirring, and adding the mixed aqueous solution of hydrochloric acid and sodium chloride to obtain a semen Alpiniae essential oil mixed oil phase; (4) The semen alpiniae oxyphyllae essential oil mixed oil phase is added with water and mixed in a stirring state, and is sheared at a high speed until the semen alpiniae oxyphyllae essential oil mixed oil phase is clear or semitransparent to obtain semen alpiniae oxyphyllae essential oil microemulsion, and the semen alpiniae oxyphyllae essential oil microemulsion prepared by the method has excellent oxidation resistance and is used for DPPH free radical and ABTS + The scavenging ability of free radicals is high, meanwhile, the stability of the catalyst is obviously improved, the particle size distribution is uniform, and the dispersibility is good.

Description

Semen katsumadai essential oil microemulsion and preparation method thereof
Technical Field
The invention relates to the technical field of plant essential oil processing, in particular to a semen katsumadai essential oil microemulsion and a preparation method thereof.
Background
Microemulsions (ME) are thermodynamically stable, transparent dispersion systems formed automatically from surfactants, oil, water (or brine) and cosurfactants. The dispersed phase particles in such dispersions are much smaller than those of conventional emulsions, typically between 10-100nm, and are largely classified into three categories: oil-in-water (O/W), bicontinuous, and water-in-oil (W/O). The excellent performance of the microemulsion can lead the microemulsion to be widely applied in the fields of food, chemical industry, medicine and the like, for example, the microemulsion can improve the solubility of substances such as indissolvable nutrient substances, flavor enhancers and the like in the food field, and can lead unstable components to resist the influence of external environment such as oxygen, light, heat, acid and alkali and the like, and prevent the quality of the food from deteriorating in the processing and preserving 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 have been few studies on plant essential oils in microemulsion systems. With the continuous and intensive 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 (Km value) of the surfactant to the cosurfactant, the ratio (S/O value) of the surfactant to the essential oil, the parameter conditions of the mixing process and the like have important influences on the final uniformity and stability of the microemulsion system, and the efficacy performance of the microemulsions are greatly different. At present, the research on the semen katsumadai essential oil microemulsion is not reported, and the invention provides a preparation process of the microemulsion liquid aiming at semen katsumadai essential oil, thereby providing a technical foundation for the application of semen katsumadai essential oil microemulsion.
Disclosure of Invention
In view of the above, the invention provides a semen katsumadai essential oil microemulsion and a preparation method thereof, and the semen katsumadai 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 semen katsumadai essential oil microemulsion, which comprises the following steps:
step 1: mixing sorbitan fatty acid ester and absolute ethyl alcohol according to a mass ratio of 1-2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to a mass ratio of 2-4:1 to obtain a mixed surfactant B for standby;
step 2: adding semen Alpiniae essential oil into a vortex oscillator, carrying out oscillation treatment, and dropwise adding a mixed surfactant A while stirring under oscillation to obtain a primary semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 2-4:1;
step 3: dropwise adding the mixed surfactant B into the primary semen Alpiniae essential oil mixed oil phase while vibrating and stirring again, and simultaneously adding a mixed aqueous solution of hydrochloric acid and sodium chloride to obtain a semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the semen katsumadai essential oil is 12-14:1;
step 4: according to the mass ratio of 2:8, adding water into the katsumadai seed essential oil mixed oil phase under a stirring state, mixing to obtain katsumadai seed essential oil colostrum, and shearing at a high speed until the solution becomes clear or semitransparent from turbidity, thus obtaining 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 semen katsumadai essential oil is 3:1.
Further, in the step 2, after the semen katsumadai essential oil is heated to 35-38 ℃, a vortex oscillator is added, the stirring speed of the vortex oscillator is 300-500rpm, and the dripping speed of the mixed surfactant A is 20-30ml/min.
Further, in the step 2, after the dripping 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 semen katsumadai essential oil is 12:1, and the mass ratio of the tween 80 to the absolute ethyl alcohol is 3:1.
Further, in the step 3, the stirring speed of the shaking is 600-800rpm, and the dripping speed of the mixed surfactant B is 10-20ml/min.
Further illustratively, in step 3, the aqueous solution of hydrochloric acid and sodium chloride mixture is added to the primary katsumadai seed essential oil mixture phase at a rate of 0.5-1 ml/min.
Further, the mass concentration of the mixed aqueous solution of the hydrochloric acid and the sodium chloride is 0.15-0.2%, wherein the mass ratio of the hydrochloric acid to the sodium chloride is 1:1-2; the mass ratio of the hydrochloric acid and sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 4-6:1.
Further illustratively, in step 4, the high speed shear speed is in the range of 1200-1500rpm.
The semen Alpiniae essential oil microemulsion prepared by the preparation method of the semen Alpiniae essential oil microemulsion.
Compared with the prior art, the invention has the beneficial effects that:
the semen alpiniae oxyphyllae essential oil microemulsion prepared by the invention has excellent oxidation resistance, and when 0.7700mg/mL of semen alpiniae oxyphyllae essential oil microemulsion is used for treating DPPH free radical and ABTS + The free radical scavenging rate can be above 85%, and the method is suitable for DPPH free radical and ABTS + Radical scavenging IC 50 The content of the semen Alpiniae essential oil microemulsion can reach 0.083mg/mL and 0.203mg/mL, and meanwhile, the semen Alpiniae essential oil microemulsion has good stability, uniform particle size distribution and good dispersibility.
The invention adopts a small amount of surfactant A compounded by sorbitan fatty acid ester and cosurfactant absolute ethanol to perform moderate-temperature preliminary emulsification and short-time high-speed magnetic stirring on the semen Alpiniae essential oil water mixed solution so as to form a certain oil-water interfacial film mobile phase; and then, the mixed surfactant B formed by combining tween 80 and absolute ethyl alcohol is used for secondary emulsification treatment, and low-concentration hydrochloric acid and sodium chloride mixed aqueous solution are slowly added at a low speed in combination to form a slightly acidic microemulsion mixed system, so that the microemulsion forming capability of the mixed surfactant is enhanced, the particle size and the polydisperse index PDI of the microemulsion are obviously reduced, and therefore, more stable O/W type microemulsion is formed, the oxidation resistance of the semen katsumadai essential oil can be effectively improved, the performance of the semen katsumadai microemulsion is obviously improved, and the centrifugal stability, the thermal stability and the low-temperature stability of the semen katsumadai essential oil microemulsion are enhanced, so that the microemulsion effect of the semen katsumadai essential oil by independently using tween 80 or sorbitan fatty acid ester is better.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1
A preparation method of semen Alpiniae essential oil microemulsion comprises the following steps:
(1) Mixing sorbitan fatty acid ester (span-80) and absolute ethyl alcohol according to a mass ratio of 1:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to a mass ratio of 2:1 to obtain a mixed surfactant B for standby;
(2) Heating semen Alpiniae essential oil to 35 ℃, adding a vortex oscillator for oscillation treatment, dropwise adding a surfactant A while stirring in an oscillating way, wherein the dripping speed is 20ml/min, the stirring speed is 300rpm, and after the dripping is completed, converting into high-speed magnetic stirring at 800rpm for 60s to obtain a primary semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 4:1;
(3) Adding dropwise the mixed surfactant B into the primary semen Alpiniae essential oil mixed oil phase while stirring at 600rpm at a dropwise speed of 10ml/min, and simultaneously adding 0.2% hydrochloric acid and sodium chloride mixed aqueous solution at a speed of 0.5ml/min to obtain the semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the semen 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 hydrochloric acid to the sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 4:1;
(4) Adding water into the mixed oil phase of the semen Alpiniae essential oil according to the mass ratio of 2:8 under the stirring state of 600rpm to obtain semen Alpiniae essential oil colostrum, and shearing at a high speed of 1200rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the semen Alpiniae essential oil microemulsion.
Example 2
A preparation method of semen Alpiniae essential oil microemulsion comprises the following steps:
(1) Mixing sorbitan fatty acid ester (span-80) and absolute ethyl alcohol according to a mass ratio of 2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to a mass ratio of 3:1 to obtain a mixed surfactant B for standby;
(2) Heating semen Alpiniae essential oil to 38deg.C, adding vortex oscillator for oscillation treatment, dropwise adding surfactant A while stirring at 30ml/min, stirring at 500rpm, and stirring at 900rpm for 50 s; the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 3:1;
(3) Adding the primary semen Alpiniae essential oil mixed oil phase into the mixed surfactant B dropwise while stirring at 800rpm at a dropwise speed of 20ml/min, and simultaneously adding a mixed aqueous solution of hydrochloric acid with a mass concentration of 0.15% and sodium chloride at a speed of 1ml/min to obtain the semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the semen 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 hydrochloric acid to the sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 6:1;
(4) Adding water into the mixed oil phase of the semen Alpiniae essential oil according to the mass ratio of 2:8 under the stirring state of 600rpm to obtain semen Alpiniae essential oil colostrum, and shearing at a high speed of 1500rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the semen Alpiniae essential oil microemulsion.
Example 3
A preparation method of semen Alpiniae essential oil microemulsion comprises the following steps:
(1) Mixing sorbitan fatty acid ester (span-80) and absolute ethyl alcohol according to a mass ratio of 1:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to a mass ratio of 3:1 to obtain a mixed surfactant B for standby;
(2) Heating the semen Alpiniae essential oil water mixed solution to 36 ℃, adding a vortex oscillator for oscillation treatment, dropwise adding a surfactant A while stirring in an oscillating way, wherein the dripping speed is 25ml/min, the stirring speed is 400rpm, and after the dripping is completed, converting into high-speed magnetic stirring at 850rpm for 60s to obtain a primary semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 3:1;
(3) Adding dropwise the mixed surfactant B into the primary semen Alpiniae essential oil mixed oil phase while stirring at 700rpm, wherein the dripping speed is 15ml/min, and simultaneously adding 0.15% hydrochloric acid and sodium chloride mixed aqueous solution at the speed of 0.5ml/min to obtain the semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the semen 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 hydrochloric acid to the sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 6:1;
(4) Adding water into the mixed oil phase of the semen Alpiniae essential oil according to the mass ratio of 2:8 under the stirring state of 600rpm to obtain semen Alpiniae essential oil colostrum, and shearing at a high speed of 1300rpm until the solution becomes clear or semitransparent from turbidity, thus obtaining the semen Alpiniae essential oil microemulsion.
Example 4
The preparation method of the semen katsumadai essential oil microemulsion of the embodiment 3 is characterized in that the semen katsumadai essential oil microemulsion is preliminarily emulsified at normal temperature and is not subjected to high-speed magnetic stirring; the method comprises the following steps:
in the step 3, adding the semen Alpiniae essential oil water mixture into a vortex oscillator at normal temperature for oscillation treatment, dropwise adding the surfactant A while stirring, and obtaining a primary semen Alpiniae essential oil mixed oil phase after the dropwise adding is completed; the procedure of example 3 was followed except that the mixed surfactant B was continuously added dropwise while stirring at 700 rpm.
Example 5
The preparation method of the semen Alpiniae essential oil microemulsion of the embodiment 3 is characterized in that in the step 4, a mixed aqueous solution of hydrochloric acid with the mass concentration of 0.5ml/min of 5% and sodium chloride is added; the mass ratio of the hydrochloric acid to the sodium chloride is 1:2; the mass ratio of the hydrochloric acid and sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 6:1.
Comparative example 1
The preparation method of the semen katsumadai essential oil microemulsion of the embodiment 3 is different in that the addition sequence of the mixed surfactants A and B is changed, specifically:
in the step 2, the mixed surfactant A is replaced by the mixed surfactant B, and the mass ratio of the mixed surfactant B to the semen katsumadai essential oil is 12:1;
in the step 3, the mixed surfactant B is replaced by a mixed surfactant A, wherein the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 3:1; the remaining parameters were the same as in example 3.
Comparative example 2
The preparation method of the semen katsumadai essential oil microemulsion of the embodiment 3 is characterized in that no step-by-step secondary emulsification treatment is performed, specifically:
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 the mixed surfactant C for standby;
in the mixing step 2-3, adding semen Alpiniae essential oil into a vortex oscillator for oscillation treatment, dropwise adding a mixed surfactant C while stirring at 700rpm, wherein the dropwise adding speed is 15ml/min, and simultaneously, adding a mixed aqueous solution of hydrochloric acid with the mass concentration of 0.15% and sodium chloride at the speed of 0.5ml/min to obtain a semen Alpiniae essential oil mixed oil phase; the mass ratio of the hydrochloric acid to the sodium chloride is 1:2; the mass ratio of the hydrochloric acid to the sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 6:1; the other parameters were the same as in example 3.
Example 6
The katsumadai seed essential oil microemulsion prepared by the above examples and comparative examples was subjected to performance measurement and analysis, including particle size, polydispersity index (PDI) and stability analysis of the microemulsion.
Test material: semen Alpiniae essential oil is obtained by supercritical extraction of semen Alpiniae, and purchased from Jiangxi Hailin perfume Limited company.
The measuring method comprises the following steps:
1. microemulsion particle size and polydispersity index (PDI): the particle sizes and polydispersity index (PDI) of the above-described different semen Alpiniae essential oil microemulsions were measured using a Markov laser particle size analyzer at 25℃and a scattering angle of 90 ℃.
2. Centrifugal stability analysis: taking a proper amount of prepared semen Alpiniae essential oil microemulsion, centrifuging for 30min at 6000 and 8000r/min, observing whether layering exists, and if not, taking deionized water as a blank control, measuring absorbance at 315nm before and after centrifugation, wherein the light transmittance is calculated according to a formula (1):
wherein: t, light transmittance; a is that 0 Absorbance of the microemulsion prior to centrifugation; a is that 1 And (3) the absorbance of the microemulsion after centrifugation.
3. Thermal stability analysis: the appropriate amount of microemulsion was heated in a constant temperature water bath at 70 and 90℃for 30min, respectively. The stability of the microemulsion was evaluated by visual observation (phase separation) and light transmittance. Deionized water is used as a blank control, an ultraviolet spectrophotometer is used for measuring absorbance of the microemulsion before and after heating at the wavelength of 315nm, and the light transmittance is calculated according to the formula (2):
wherein: a is that 0 Absorbance of the microemulsion prior to heating; a is that 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 light transmittance. The light transmittance of the day 14 microemulsion was measured at 315nm wavelength using an ultraviolet spectrophotometer with deionized water as a blank.
The light transmittance is calculated according to formula (3):
wherein: a is that 0 Absorbance of the microemulsion prior to low temperature storage; a is that 1 Absorbance of the microemulsion at day n after low temperature storage. The measurement results and analysis are shown in Table 1 below:
TABLE 1
As can be seen from the table, the particle size of the semen alpiniae oxyphyllae essential oil microemulsion prepared in the embodiment 1-5 is less than 15nm, the polydispersity index PDI is less than 0.3, the particle size distribution is uniform, the dispersibility is good, stable O/W type microemulsion is formed, the semen alpiniae oxyphyllae essential oil microemulsion has good centrifugal stability, thermal stability and low-temperature stability under certain conditions, layering and turbidity phenomena are not generated in the centrifugation, water bath heating and low-temperature storage for 14d under 6000 and 8000r/min respectively, the light transmittance is kept to 100%, and clear, transparent and uniform liquid is shown.
From comparison of example 3 with comparative examples 1 to 2, it can be seen that the emulsions of comparative examples 1 and 2 have significantly increased particle diameters, have increased polydispersity index PD, and at the same time, have significantly decreased stability. Wherein, example 3 compares with example 4-5, demonstrate in the course of preliminary emulsification, through the high-speed magnetic stirring of moderate temperature, is favorable to further reducing emulsion particle diameter and PDI, when the hydrochloric acid of too high concentration is mixed with sodium chloride mixed aqueous solution in example 5, although kept certain particle diameter, the polydisperse index PDI is in the trend of rising.
Example 7
The katsumadai seed essential oil microemulsions prepared in the above examples 3-5 and comparative examples 1-2 were subjected to an antioxidant capacity analysis,
(1) Scavenging ability to DPPH free radical
With reference to the method of Xu Zongyun et al (2004), the ability of katsumadai microemulsion to scavenge DPPH free radicals was measured, and the ability of microemulsion to scavenge DPPH free radicals was quantified by measuring absorbance at 517nm with a spectrophotometer.
Weighing 0.0256g DPPH in 100mL volumetric flask, and shaking with absolute ethanol to give stock solution (6.5X10) -4 mol/L) is stored in a refrigerator at 4 ℃ and diluted step by step when in use.
In the measurement, 10mL of DPPH stock solution was taken up, and the solution was shaken up in a 100mL volumetric flask to give a working solution (6.5X10) -5 mol/L). Absorbing a certain amount of semen Alpiniae essential oil and microemulsion, respectively preparing into 0.77mg/mL solution with absolute ethanol, absorbing 2mL of the semen Alpiniae essential oil and microemulsion diluent, and adding 2mL of DPPH working solution (6.5X10) - 5 mol/L), mixing uniformly at room temperature, reacting for 30min in dark, and measuring absorbance value A at 517nm i The method comprises the steps of carrying out a first treatment on the surface of the The absorbance value of 2mL of absolute ethyl alcohol added to 2mL of sample solution with corresponding concentration is taken as background value A j The method comprises the steps of carrying out a first treatment on the surface of the The absorbance of 2mL absolute ethanol plus 2mL DPPH solution was used as initial value A k . With vitamin C as positive control, the experiment was repeated 3 times and the clearance of DPPH free radical was calculated according to formula (1):
simultaneously using GraphPad Prism 5.0 software to calculate IC of semen Alpiniae essential oil microemulsion 50 Value, IC 50 The value is the essential oil amount required for half of DPPH removal, IC 50 Smaller values indicate greater DPPH scavenging capacity.
(2) Scavenging ability to ABTS free radical
Referring to the GUO et al (2018) method, first 0.4mL of 7.4mmol/L ABTS solution (3 mg of ABTS is dissolved in 0.735mL of distilled water) and 1.43mL of 2.6mmol/L K are taken 2 S 2 O 3 Solution (1 mg K) 2 S 2 O 3 Dissolving in 1.43mL distilled water), mixing, standing in dark for 12 hr, and diluting with anhydrous ethanol 45 times to absorbance at 734nm of about 0.7 to obtain ABTS + The free radical working solution is then taken up in 4mM LABSS + Adding semen Alpiniae essential oil and microemulsion with mass concentration of 0.77mg/mL prepared from absolute ethanol into free radical working solution, respectively, shaking for 10s, mixing thoroughly, reacting at room temperature in dark for 10min, and measuring absorbance value A at 734nm 1 The method comprises the steps of carrying out a first treatment on the surface of the Blank was equal amount of absolute ethanol (A 0 ). With vitamin C as positive control, the experiment was repeated 3 times, and the clearance of ABTS cationic free radical was calculated according to the formula(2) And (3) calculating:
simultaneously using GraphPad Prism 5.0 software to calculate IC of semen Alpiniae essential oil microemulsion 50 Value, IC 50 The value is the amount of essential oil needed to clear half of ABTS, IC 50 Smaller values indicate greater cleanup capacity for ABTS.
The results are shown in Table 2 below:
TABLE 2
From the above table, the semen Alpiniae essential oil microemulsion prepared by the invention has the clearance rate of DPPH free radical and ABTS + Radical scavenging rates are all significantly higher than essential oils (P<0.05 Especially the ABTS clearance/% of the semen Alpiniae essential oil microemulsion prepared in example 3 is close to vitamin C, and IC for scavenging DPPH free radical 50 And ABTS + Radical scavenging IC 50 Can reach 0.083mg/mL and 0.211mg/mL respectively. Compared with the preparation method in example 3, the antioxidant capacity of comparative examples 1-2 is poorer, which shows that under the preparation process of the invention, the prepared semen alpiniae zerumbet essential oil microemulsion not only has obviously improved emulsion performance, but also has obviously enhanced centrifugal stability, thermal stability and low-temperature stability, and can effectively ensure the antioxidant capacity of semen alpiniae zerumbet essential oil.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (9)

1. A preparation method of semen 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 a mass ratio of 1-2:1 to obtain a mixed surfactant A; mixing Tween 80 and absolute ethyl alcohol according to a mass ratio of 2-4:1 to obtain a mixed surfactant B for standby;
step 2: adding semen Alpiniae essential oil into a vortex oscillator, carrying out oscillation treatment, and dropwise adding a mixed surfactant A while stirring under oscillation to obtain a primary semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant A to the semen katsumadai essential oil is 2-4:1;
step 3: dropwise adding the mixed surfactant B into the primary semen Alpiniae essential oil mixed oil phase while vibrating and stirring again, and simultaneously adding a mixed aqueous solution of hydrochloric acid and sodium chloride to obtain a semen Alpiniae essential oil mixed oil phase; the mass ratio of the mixed surfactant B to the semen katsumadai essential oil is 12-14:1, the mass concentration of the hydrochloric acid is 0.15% -0.2%, the mass ratio of the hydrochloric acid to the sodium chloride is 1:1-2, and the mass ratio of the hydrochloric acid to the sodium chloride mixed aqueous solution to the semen katsumadai essential oil is 4-6:1;
step 4: according to the mass ratio of 2:8, adding water into the katsumadai seed essential oil mixed oil phase under the stirring state for mixing to obtain katsumadai seed essential oil colostrum, and shearing at high speed until the solution becomes clear or semitransparent from turbidity to obtain the katsumadai seed essential oil microemulsion.
2. The method for preparing the semen katsumadai essential oil microemulsion according to claim 1, which is characterized in that: the mass ratio of the mixed surfactant A to the semen 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 semen katsumadai essential oil microemulsion as claimed in claim 2, wherein the method comprises the following steps: in the step 2, after the semen katsumadai essential oil is heated to 35-38 ℃, adding a vortex oscillator for oscillation treatment; the shaking stirring speed is 300-500rpm, and the dripping speed of the mixed surfactant A is 20-30ml/min.
4. A method for preparing a semen katsumadai essential oil microemulsion according to claim 3, wherein: in the step 2, after the dripping 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.
5. The method for preparing the semen katsumadai essential oil microemulsion according to claim 1, which is characterized in that: in the step 3, the mass ratio of the mixed surfactant B to the semen katsumadai 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 semen katsumadai essential oil microemulsion according to claim 5, which is characterized in that: in the step 3, the stirring speed of the shaking is 600-800rpm, and the dripping speed of the mixed surfactant B is 10-20ml/min.
7. The method for preparing the semen katsumadai essential oil microemulsion according to claim 6, which is characterized in that: in the step 3, the mixed aqueous solution of hydrochloric acid and sodium chloride is added into the primary semen Alpiniae essential oil mixed oil phase at a rate of 0.5-1 ml/min.
8. The method for preparing the semen katsumadai essential oil microemulsion according to claim 1, which is characterized in that: in step 4, the high speed shear speed is 1200-1500rpm.
9. A katsumadai seed essential oil microemulsion prepared by the method for preparing a katsumadai seed essential oil microemulsion according to any one of claims 1 to 8.
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CN113908082A (en) * 2021-10-14 2022-01-11 上海应用技术大学 Preparation method of soybean oil microemulsion capable of being infinitely diluted

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