CN110074456B - A kind of peppermint oil gel beads and preparation method thereof - Google Patents

Abstract

The invention discloses peppermint oil gel beads and a preparation method thereof, belonging to the technical field of microcapsule technology. By optimizing and adjusting the form and proportion of the peppermint oil core material, the method prepares a peppermint oil gel beads that can maintain a good shape during drying and storage. The method adopts the following steps: preparing a peppermint oil cyclodextrin inclusion compound, mixing it with a peppermint oil emulsion in a certain proportion, and then adding it dropwise to a sodium alginate solution to form peppermint oil gel beads immediately, and then respectively in chlorine. The calcium chloride solution and the chitosan acetic acid solution are solidified and then taken out, and the finished product is obtained by vacuum drying. The gel beads prepared by the invention are well formed in the drying process, have low collapse rate and strong stability in the storage process, and have the effect of regulating the release rate of the core material.

Description

A kind of peppermint oil gel beads and preparation method thereof

technical field

The invention relates to peppermint oil gel beads and a preparation method thereof, belonging to the technical field of microcapsule technology.

Background technique

Peppermint oil has both antibacterial and fragrance properties, and is widely used in condiments, tobacco and other industries. However, when peppermint oil is exposed to the air, it is prone to volatilization, which also restricts its application range. In order to solve this problem, there are many reports in the prior art that peppermint oil is embedded and protected by the microencapsulation method.

Gel beads are a kind of microcapsules, which are usually prepared from anionic polysaccharides such as sodium alginate and pectin and metal cations through ionic cross-linking. In order to improve the strength of the gel film, a positively charged chitosan solution can also be introduced to make it interact with anionic polysaccharides as a polyelectrolyte, giving the system good stability. The gel film on the outer layer of the gel bead system embeds peppermint oil inside, which not only protects peppermint oil to a certain extent, but also has the advantages of mild preparation conditions, natural embedded raw materials, and timed and fixed-point release. .

Most of the existing reports on gel beads involve the encapsulation of proteins, probiotics, and oily nutrients, and few studies have used oil-soluble and easily lost flavor substances as the core material of gel bead systems. In addition, during the drying process of the prepared wet gel beads, due to the loss of water in the liquid core material, the gel beads are prone to structural collapse and hard texture. Therefore, there is an urgent need to find a suitable method to alleviate the problem that the structure of gel beads is easily collapsed during the drying process, which is beneficial to increase the preparation efficiency of gel beads and improve the utilization rate of raw materials.

Cyclodextrin is a hollow cyclic oligomer formed by glucopyranose, which is hydrophilic on the outside and hydrophobic on the inside, so it can embed oil-soluble flavors and form inclusion complexes. At present, there are mainly three types of cyclodextrins, namely α, β, and γ-cyclodextrin. β-cyclodextrin has a moderate cavity and low production cost, so it is widely used.

SUMMARY OF THE INVENTION

【technical problem】

In order to solve the problem of easy collapse of the structure of peppermint oil gel beads during drying and storage.

【Technical solutions】

In order to prepare a kind of peppermint oil gel beads that can maintain the shape during drying and storage, and are not easy to collapse, the present invention uses sodium alginate, chitosan, calcium chloride, peppermint oil, emulsifier, β-cyclodextrin, etc. As raw materials, different proportions of peppermint oil emulsion and peppermint oil cyclodextrin inclusion compound are mixed as core material, and gel beads are prepared by dropping method. The prepared peppermint oil gel beads have good roundness and are not easy to occur. collapse.

The technical scheme of the present invention is specifically: a preparation method of peppermint oil gel beads, the method comprises the following steps:

(1) Preparation:

Peppermint oil cyclodextrin inclusion complex: dissolve β-cyclodextrin in water to obtain an aqueous solution of β-cyclodextrin, add peppermint oil dropwise to the aqueous solution of β-cyclodextrin, and continue stirring at 45°C to 55°C for 2 After ~4h, the sample was allowed to stand at a low temperature of 0 ~ 10 ℃ for 8 ~ 12h, and the peppermint oil inclusion compound was obtained through solid-liquid separation and drying;

Peppermint oil emulsion: dissolve calcium chloride, Tween 80, Span 80 and polysaccharide thickener in water, stir until completely dissolved, then add peppermint oil, and prepare peppermint oil emulsion through high-speed shearing;

(2) Mixing the peppermint oil inclusion compound and peppermint oil emulsion according to the ratio of 1～5:8 (w/v), that is, the core material dispersion liquid completed by the compounding;

(3) dropping the core material dispersion obtained in step (2) into the sodium alginate solution to form calcium alginate gel beads, stirring and solidifying for 5-15 minutes;

(4) rinsing the solidified gel beads in step (3), put them into a calcium chloride solution, and continue stirring and solidifying for 10 to 30 minutes;

(5) Rinse the solidified gel beads in step (4), put them into the chitosan acetic acid solution, and continuously stir and solidify for 10-30 min;

(6) taking out the solidified gel beads in step (5), rinsing, solid-liquid separation, and drying to obtain peppermint oil gel beads.

In an embodiment of the present invention, the content of β-cyclodextrin in the aqueous solution in step (1) is 10% to 20% (w/v).

In one embodiment of the present invention, in the preparation process of step (1) peppermint oil cyclodextrin inclusion compound, the mass ratio of peppermint oil and β-cyclodextrin is 1:2～1:8(w/w ), preferably 1:4 (w/w).

In an embodiment of the present invention, in the peppermint oil emulsion, the content of calcium chloride is 8% to 15% (w/v), the content of Tween 80 is 0.5% to 1.0% (w/v), and the content of Span 80 is 0.5% to 1.0% (w/v). It is 1.0%-2.0% (w/v), the content of polysaccharide thickener is 0.2%-0.5% (w/v), and the content of peppermint oil is 15%-30% (w/v).

In one embodiment of the present invention, the polysaccharide thickener is one or more of xanthan gum, pectin, gellan gum or carboxymethyl cellulose.

In an embodiment of the present invention, in step (1) during the preparation of the peppermint oil cyclodextrin inclusion complex, the stirring rate is 200-280 r/min.

In one embodiment of the present invention, in the preparation process of step (1) peppermint oil cyclodextrin inclusion compound, the drying method is preferably vacuum drying, the drying temperature is 35-40°C, and the drying time is 1-3h.

In an embodiment of the present invention, the high-speed shearing rate is 7000-12000 r/min, and the time is 1-5 min. In one embodiment of the present invention, the concentration of the sodium alginate solution is 0.5% to 2.0% (w/v).

In one embodiment of the present invention, the dissolving temperature of the sodium alginate solution in step (1) is 40-55°C.

In one embodiment of the present invention, the ratio of the core material solution to the sodium alginate solution in step (3) is 1:20-1:10 (v/v), and the dropping height of the syringe is 4cm-6cm, The dropping rate is 1.5-2.0 mL/min, and the curing time is preferably 8-12 min.

In an embodiment of the present invention, the concentration of the calcium chloride solution in the step (4) is 5% to 20% (w/v), and the ratio of the core material solution to the calcium chloride solution is 1:20～ 1:10(v/v).

In an embodiment of the present invention, the concentration of chitosan in the chitosan acetic acid solution is 0.2%-1.0% (w/v), the concentration of acetic acid is 0.1%-1.5% (w/v), The volume ratio of the core material solution to the chitosan acetic acid solution is 1:20-1:10.

In an embodiment of the present invention, the volume ratio of the core material solution to the chitosan acetic acid solution is 1:20-1:10.

In an embodiment of the present invention, preferably, the curing time in step (4) is 15-25 min.

In an embodiment of the present invention, the stirring and curing time in step (5) is 10-20 min.

In an embodiment of the present invention, the drying in step (6) is: treating in a vacuum drying oven at 35-40° C. for 12-36 hours.

Preferably, in the process of preparing the gel beads in steps (3)-(5), continuous stirring is required, and the stirring rate is 350-550 r/min.

The technical effect obtained by the present invention:

1, the present invention embeds peppermint oil with gel bead system, improves the problem that peppermint oil is prone to volatilization and oxidation at normal temperature to a certain extent, and broadens the application range of peppermint oil in the field of food additives.

2. For the first time, the peppermint oil emulsion and the peppermint oil cyclodextrin inclusion compound are compounded as the core material in a certain proportion, and the peppermint oil cyclodextrin inclusion compound can be used as a filler to maintain the gel beads in the drying process and after drying. structure to prevent it from collapsing.

3. The present invention uses β-cyclodextrin as the wall material to embed peppermint oil, which can not only support the structure of the gel beads in the drying process, but also regulate the release of peppermint aroma.

4. The shape of the peppermint oil gel beads prepared by the present invention is round, and compared with the gel beads that only add peppermint oil emulsion, the hardness is decreased, that is, the crushing pressure is reduced, which is conducive to expanding the size of the gel beads of this type. Application in the field of cigarette popping beads.

Description of drawings

Fig. 1 is the finished product diagram of the gel beads prepared from the peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion with different mass to volume ratios as the core material in Example 1. Wherein, Fig. 1-a is a gel bead without peppermint oil cyclodextrin inclusion compound, and the mass-volume ratio of peppermint oil cyclodextrin inclusion compound and peppermint oil emulsion in the gel beads of Fig. 1-b～e is respectively (b) 1:8; (c) 2:8; (d) 2.5:8; (e) 3:8.

Figure 2(a) shows the storage stability (in terms of loading) of gel beads prepared by mixing different proportions of peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion as the core material in Example 1 at 37°C;

Figure 2(b) shows the storage stability of pure peppermint oil at 37°C (represented by peppermint oil retention rate);

Figure 2(c) is the heat release rate at 37°C of gel beads prepared with different proportions of peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion as core materials in Example 1.

Figure 3 shows the hardness of gel beads prepared by mixing peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion with different mass-to-volume ratios as core materials.

Figure 4 shows the loading (a), yield and efficiency (b) of peppermint oil in the inclusion compound when the ratio of core peppermint oil and wall material β-cyclodextrin is different, Note: Different lowercase letters indicate groups The difference between groups was significant (P<0.05); marked with the same lowercase letter, the difference between groups was not significant (P>0.05).

Detailed ways

In order to better understand the present invention, the content of the invention is further clarified below in conjunction with the examples, but the content of the present invention is not limited to the following examples.

The calculation method of the collapse rate:

Drawing of peppermint oil working curve: Weigh 100 mg of peppermint oil, dilute to 100 mL with 95% ethanol, and prepare a peppermint oil ethanol solution with a concentration of 1 mg/mL. Accurately pipette 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, 3.0mL, 3.5mL, and 4.0mL solutions into a 25mL volumetric flask, use 95% ethanol, and measure the absorbance at 230nm. Taking the concentration of peppermint oil as the abscissa and the absorbance value as the ordinate, draw the working curve. The linear regression equation is: y=2.4089x+0.018, the correlation coefficient R ² =0.9996, where x is the concentration of peppermint oil, and y is the absorbance value.

Determination and calculation of storage stability of pure peppermint oil and gel beads:

(1) Accurately weigh 7 parts of 0.0890g pure peppermint oil, store them in a 37°C incubator, and take them out at 0h, 0.5h, 1h, 1.5h, 2h, 2.5h, and 3.0h respectively, and work through peppermint oil. The retention rate of peppermint oil at different time points is measured by curve, and the retention rate calculation formula is as follows:

Wherein A ₁ is the absorbance value; 0.018, 2.4089 are the intercept and the slope in the peppermint oil standard song respectively; w ₁ is the weight (g) of the pure peppermint oil; d ₁ is the dilution factor, and 1000 is used for unit conversion.

(2) Store the different gel beads samples in a 37°C incubator respectively, take them out every 7 days, and measure their loadings. The determination method is as follows: take about 0.1g of sample, squeeze and dissolve it in 15mL of 95% ethanol, extract it by ultrasonic for 30min at 60°C, centrifuge, take a small amount of supernatant and dilute it to a certain multiple, and measure its absorbance at 230nm. Calculated by the formula of peppermint oil working curve, the calculation formula is as follows:

Wherein A ₂ is the absorbance value; 0.018, 2.4089 are the intercept and slope in the peppermint oil standard song respectively, in order to convert; w ₂ is the mass (g) of the gel beads; d ₂ is the dilution factor, and 15 is 95 % volume of absolute ethanol (mL).

Determination of gel bead yield: yield represents the utilization rate of peppermint oil raw material in the preparation process, and the processing method is the same as the loading method, and the calculation formula is as follows:

Wherein, L is the mass (g) of peppermint oil contained in a certain amount of gel beads, and M is the mass (g) of the peppermint oil raw material consumed to prepare a certain amount of gel beads.

Determination of Embedding Efficiency: Take about 0.2g of sample, wash three times with 95% absolute ethanol, 5mL each time, collect the filtrate, measure its absorbance at 230nm, and calculate through the peppermint oil working curve to obtain the surface of the gel beads The content of peppermint oil and the calculation formula of gel beads embedding efficiency are as follows:

Hardness measurement method: use a physical property analyzer to obtain the hardness information of the gel beads. The hardness of the gel beads was measured with a P/36R cylindrical probe. The speed before the test was 1mm/s, the test speed was 2mm/s, and the speed after the test was 1mm/s. The compression rate was 75%. Each group of samples was tested in parallel for at least 5 Second-rate.

Determination and calculation of heat release rate of L-menthol in gel beads:

Preparation of extractant: Using propyl benzoate as the internal standard, a propyl benzoate-isopropanol solution with a concentration of 0.2 mg/mL was prepared, and after filtering out impurities with a 0.45 μm organic filter membrane, it was used as an extracting agent for later use.

Drawing of L-menthol working curve: Weigh 20 mg of L-menthol standard, dissolve it with an extractant, and transfer it to a 10 mL volumetric flask as a mother solution. Pipette 0.1mL, 0.7mL, 1.3mL, 1.9mL, and 2.5mL of solutions from the mother liquor respectively, and dilute to 10mL with an extractant. The relationship between the concentration of L-menthol and the peak area was obtained by gas chromatography. The linear regression equation is: y=462034x-4290, where R ² =0.9995, x is the concentration of L-menthol (mg/mL), and y is the peak area.

Determination of heat release rate of gel beads: Squeeze the gel beads samples and put them into a simulated heat release device for experiments. new extract. Time-dependent release of menthol from gel beads was determined by gas chromatography. The formula for calculating the heat release rate is as follows:

Wherein S is the peak area obtained by internal standard conversion, m is the weight of the sample (g), L is the load of peppermint oil in the sample (mg/g), and 0.25 is the proportion of L-menthol in peppermint oil. 5 is the volume (mL) of the extractant.

Gas chromatography conditions refer to YC/T 286-2009: DB-WAX (60m×0.25mm×0.25μm) chromatographic capillary column; helium as carrier gas, helium flow rate 30.0mL/min, hydrogen flow rate 40.0mL/min, air The flow rate was 400.0 mL/min; the starting temperature was 160°C and maintained for 2 min. It was then ramped to 200°C at a rate of 5°C/min and held for 5 min with a split ratio of 50:1.

Example 1

(1) First prepare a 15% (w/v) saturated aqueous solution of β-cyclodextrin, place it in a constant temperature water bath at 50°C and stir at a speed of 200 r/min for 3 hours, then use an appropriate amount of peppermint oil as the core material, add to β-cyclodextrin In the saturated aqueous solution of cyclodextrin, keep the mass ratio of peppermint oil and β-cyclodextrin at 1:4, and continue stirring for 3 hours. Filtration to obtain wet capsules, and finally vacuum drying at 40° C. for 2 hours to obtain finished mint oil cyclodextrin inclusion complex powder.

Weigh a certain amount of calcium chloride, Tween 80, Span 80 and xanthan gum and dissolve them in water respectively, the concentrations are 6%, 0.8%, 1.6%, 0.4% (w/v), stir until completely dissolved, and then Add peppermint oil dropwise under stirring state, mix the raw materials fully by high-speed shearing method, set the rotating speed to 10000r/min, and the treatment time is 2min to obtain peppermint oil emulsion, wherein the concentration of peppermint oil in peppermint oil emulsion is 20% (w/v).

(2) Mix peppermint oil cyclodextrin and peppermint oil emulsion at 0:8, 1:8, 2:8, 2.5:8, 3:8, 5:8 (w/v) as the core material to prepare gel beads , the rotational speed of the magnetic stirrer is set to 500r/min;

(3) drop the peppermint oil core material into the 0.7% (w/v) sodium alginate solution at a constant speed with a syringe to form calcium alginate gel beads immediately, stir and solidify for 8min;

(4) Rinse the cured gel beads with deionized water, and then put them into 8% (w/v) calcium chloride solution to cure for 20min;

(5) rinse with deionized water again, put into 0.4% (w/v) chitosan acetic acid solution, wherein the acetic acid content is 0.5% (w/v); continue stirring and curing for 15min;

(6) Take out the solidified gel beads in step (5), rinse with water and then suction filtration, and finally dry the wet gel beads at 37° C. and 0.1 MPa for 12 hours to obtain the finished peppermint oil gel beads.

The photo of the prepared peppermint oil gel beads is shown in Figure 1. It can be seen that when the peppermint oil cyclodextrin inclusion complex is not added, the formed peppermint oil gel beads have obvious depressions, and the collapse rate is 98.7%; When the ratio of fine inclusion complex and peppermint oil emulsion is 1:8 (w/v), the formed peppermint oil gel beads have obvious depressions, and the collapse rate is 95.6%; when the ratio of peppermint oil cyclodextrin and peppermint oil emulsion is 2: At 8(w/v), the depression phenomenon was alleviated, and the collapse rate was 20.6%; when the ratio was greater than 2:8 (w/v), the depression of peppermint oil gel beads almost disappeared, and a round and smooth gel was formed Beads, the collapse rate is less than 1.6%. With the increase of the content of peppermint oil cyclodextrin inclusion complex, the structural collapse rate of the gel beads decreased, indicating that supplementing the core material with an appropriate amount of peppermint oil cyclodextrin inclusion compound can effectively maintain the gel beads during the drying process. and the structure after drying; but when the content of the peppermint oil cyclodextrin inclusion compound is too high, that is, greater than or equal to 5:8 (w/v), the fluidity of the system becomes poor, and the core material dispersion cannot Forms round peppermint oil gel beads.

Figure 2-a characterizes the storage stability of gel beads containing different proportions of peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion as the core material at 37 °C. It can be found from the figure that after 35 days of storage, there is still 25% to 35% of peppermint oil remaining in the gel beads. The loading of the gel beads prepared by the traditional method (without adding cyclodextrin) dropped to about 29% after storage for 35 days, and there was no obvious difference compared with the loading of the improved gel beads. Figure 2-b shows the retention rate of pure peppermint oil when stored at 37°C. After placing the same quality of pure peppermint oil in a 37°C incubator for 3 hours, the retention rate of peppermint oil dropped to 8.5%, indicating that most of the peppermint oil has been in volatilized under these conditions. Figure 2-c shows the heat release rate of the gel beads mixed with peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion in different proportions as the core material at 37°C after being squeezed to simulate the heat release device. The heat release rate of the obtained gel beads and the gel beads prepared by the traditional method has a certain difference, and the addition of the peppermint oil cyclodextrin inclusion compound can improve the release rate of the core material. To sum up, the gel bead system in the present invention can have a good embedding effect on pure peppermint oil and improve its storage stability; the peppermint oil cyclodextrin added in the core material can promote the release of the core material, and The shape of the gel beads can be better maintained, so that they can reach a state of basically no collapse.

In addition, Figure 3 shows the hardness of gel beads prepared by mixing different proportions of peppermint oil emulsion and peppermint oil cyclodextrin inclusion compound as core material. When the core material only contains peppermint oil emulsion, the extrusion pressure of the gel beads is relatively large; however, after adding peppermint oil cyclodextrin inclusion complex as the core material on the basis of peppermint oil emulsion, the hardness of the gel beads drops sharply. The burst pressure is significantly reduced. This kind of characteristic is favorable for the gel beads to be applied to the explosive beads for cigarettes, and the applicable scope of the gel beads is expanded. If the hardness of the gel beads is too high, when they are used as explosive beads for cigarettes, they will not be able to be crushed, which will affect the experience of use.

Example 2

Prepare a 15% (w/v) saturated aqueous solution of β-cyclodextrin, dissolve it in a water bath at 50°C and stir for a period of time at a speed of 200 r/min, then use an appropriate amount of peppermint oil as the core material and add it to the saturated aqueous solution of β-cyclodextrin , the peppermint oil cyclodextrin inclusion complexes with core-to-wall ratios of 1:2, 1:4, 1:6 and 1:8 (w/w) were prepared respectively, and the inclusion complexes were continuously stirred for 3 h. After stirring, put it in a refrigerator at 4 °C and let it stand until it is completely precipitated, filter the precipitate to obtain wet capsules, and finally vacuum dry it at 40 °C for 2 hours to obtain the finished peppermint oil inclusion compound powder, whose properties are shown in Figure 4 shown.

Weigh a certain amount of calcium chloride, Tween 80, Span 80 and xanthan gum and dissolve them in water to make their concentrations 6%, 0.8%, 1.6% and 0.4% (w/v) respectively, and stir until completely dissolved , and then drop peppermint oil in a state of stirring to make its concentration in the emulsion 20% (w/v). The raw materials are fully mixed by the high-speed shearing method, the rotation speed is set at 10000r/min, and the treatment time is 2min, and then the peppermint oil emulsion can be obtained.

Mix the peppermint oil cyclodextrin inclusion complex and peppermint oil emulsion with different core-to-wall ratios at a ratio of 2.5:8 (w/v) as the core material, set the rotating speed to 400r/min, and use a syringe to uniformly speed the peppermint oil core material. Dropped into 0.7% (w/v) sodium alginate solution, calcium alginate gel beads were formed immediately, and the mixture was stirred and solidified for 8 minutes. Rinse the cured gel beads with deionized water, then put them into 8% (w/v) calcium chloride solution to cure for 20 minutes, rinse with deionized water, and put in 0.4% (w/v) chitosan In the solution, the acetic acid content is 0.5% (v/v). After the reaction was continued for 15 min, it was taken out and filtered with suction.

The prepared wet gel beads were dried at 37° C. and 0.1 MPa for 12 h to obtain the finished product of peppermint oil gel beads.

Fig. 4 shows the loading, yield and efficiency of inclusion complexes prepared by different ratios of peppermint oil and cyclodextrin, wherein the yield is the utilization rate of peppermint oil raw materials during the preparation of gel beads, and the efficiency represents free The mass of peppermint oil on the surface of the gel beads, the higher the efficiency indicates that the less peppermint oil is freed from the surface of the inclusion complex. Under the condition that the quality of the core material peppermint oil is constant, with the increase of the quality of the wall material β-cyclodextrin, the loading of the gel beads shows a downward trend. The loading was the highest, reaching 299.41 mg/g, and the yield and embedding efficiency were 62.55% and 68.50%, respectively. It can be seen that the peppermint oil cyclodextrin inclusion complex is prepared with a core-to-wall ratio of 1:2. Although the system loading is high, its embedding efficiency is low, which means that there is more peppermint oil free on the surface of the inclusion complex, indicating that there is more peppermint oil on the surface of the inclusion complex. Under the condition that the ratio is 1:2, the amount of peppermint oil is excessive, resulting in that the limited cyclodextrin cannot encapsulate all the peppermint oil, resulting in a low utilization rate of the peppermint oil raw material.

However, with the increase of the amount of cyclodextrin, both the yield and the entrapment efficiency of the inclusion compound showed an upward trend. When the core-to-wall ratio was 1:6 and 1:8, the yield and efficiency of the peppermint oil inclusion compound reached It is more than 90%, indicating that the utilization rate of the raw peppermint oil is high at this time, and almost no free peppermint oil is attached to the surface of the inclusion compound. But in this case, there is a problem of non-uniform release in the application process. That is, after the release of the peppermint oil emulsion outside the gel beads, since there is almost no free peppermint oil attached to the surface of the inclusion compound, and the release of the peppermint oil inside the inclusion compound takes a certain time, there will be a lower The release concentration of peppermint oil brings about the problem of non-uniform release. However, when the core-to-wall ratio is 1:4, the yield of the inclusion complex is higher, and the entrapment efficiency is about 80%, indicating that there is still a small amount of free peppermint oil on the surface of the inclusion complex. After the emulsion is mixed as a core material, it can not only contribute to the increase of peppermint oil in the emulsion, but also provide support for the uniform release of peppermint oil in the later stage. Therefore, the core-to-wall ratio is preferably 1:4.

Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Anyone who is familiar with this technology can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, The protection scope of the present invention should be defined by the claims.

Claims (25)

1. a preparation method of peppermint oil gel beads, is characterized in that, described method may further comprise the steps: (1) Preparation: Peppermint oil cyclodextrin inclusion complex: dissolve β-cyclodextrin in water to obtain an aqueous solution of β-cyclodextrin, add peppermint oil dropwise to the aqueous solution of β-cyclodextrin, and continue stirring at 45°C to 55°C for 2 After ~4h, the sample was allowed to stand at a low temperature of 0 ~ 10 ℃ for 8 ~ 12h, and the peppermint oil inclusion compound was obtained through solid-liquid separation and drying; Peppermint oil emulsion: dissolve calcium chloride, Tween 80, Span 80 and polysaccharide thickener in water, stir until completely dissolved, then add peppermint oil, and prepare peppermint oil emulsion by high-speed shearing; (2) Mix the peppermint oil inclusion compound with the peppermint oil emulsion according to the ratio of 2～3:8 (w/v), that is, the composite core material dispersion; (3) dropping the core material dispersion obtained in step (2) into the sodium alginate solution to form calcium alginate gel beads, stirring and solidifying for 5-15 minutes; (4) rinsing the gel beads cured in step (3), put them into a calcium chloride solution, and continue stirring and curing for 10 to 30 minutes; (5) Rinse the solidified gel beads in step (4), put them into the chitosan acetic acid solution, and continuously stir and solidify for 10-30 min; (6) Take out the solidified gel beads in step (5), rinse, separate and dry to obtain peppermint oil gel beads. 2. the preparation method of a kind of peppermint oil gel beads according to claim 1, is characterized in that, the concentration of β-cyclodextrin aqueous solution described in step (1) is 10%～20% (w/v) . 3. the preparation method of a kind of peppermint oil gel beads according to claim 1 and 2 is characterized in that, in the preparation process of step (1) peppermint oil cyclodextrin inclusion compound, peppermint oil and β-cyclodextrin The mass ratio of fines is 1:2 to 1:8. 4. the preparation method of a kind of peppermint oil gel beads according to claim 1 and 2, is characterized in that, in described peppermint oil emulsion, calcium chloride content 8%～15% (w/v), Tween 80 content 0.5%～1.0% (w/v), Span 80 content 1.0%～2.0% (w/v), polysaccharide thickener content 0.2%～0.5% (w/v), peppermint oil content 15% ~30% (w/v). 5. the preparation method of a kind of peppermint oil gel beads according to claim 3, is characterized in that, in described peppermint oil emulsion, calcium chloride content 8%～15% (w/v), Tween 80 content 0.5%～1.0% (w/v), Span 80 content is 1.0%～2.0% (w/v), polysaccharide thickener content is 0.2%～0.5% (w/v), peppermint oil content is 15%～30% % (w/v). 6. the preparation method of a kind of peppermint oil gel beads according to any one of claim 1,2 or 5, is characterized in that, the concentration of described sodium alginate solution is 0.5%～2.0% (w/v), The concentration of the calcium chloride solution in the step (4) is 5% to 20% (w/v). 7. the preparation method of a kind of peppermint oil gel beads according to claim 3, is characterized in that, the concentration of described sodium alginate solution is 0.5%～2.0% (w/v), described step (4) The concentration of the calcium chloride solution is 5% to 20% (w/v). 8. the preparation method of a kind of peppermint oil gel beads according to claim 4, is characterized in that, the concentration of described sodium alginate solution is 0.5%～2.0% (w/v), described step (4) The concentration of the calcium chloride solution is 5% to 20% (w/v). 9. according to the preparation method of a kind of peppermint oil gel beads described in any one of claim 1,2,5 or 7～8, it is characterized in that, the speed of described high-speed shearing is 7000-12000r/min, and the time is 1 to 5 minutes. 10 . The preparation method of peppermint oil gel beads according to claim 3 , wherein the high-speed shearing rate is 7000-12000 r/min, and the time is 1-5 min. 11 . 11 . The preparation method of peppermint oil gel beads according to claim 4 , wherein the high-speed shearing rate is 7000-12000 r/min, and the time is 1-5 min. 12 . 12 . The method for preparing peppermint oil gel beads according to claim 6 , wherein the high-speed shearing rate is 7000-12000 r/min, and the time is 1-5 min. 13 . 13. The preparation method of a peppermint oil gel beads according to any one of claims 1, 2, 5, 7-8 or 10-12, wherein the chitosan in the chitosan acetic acid solution has The concentration is 0.2% to 1.0% (w/v), and the concentration of acetic acid is 0.1% to 1.5% (v/v). 14 . The method for preparing peppermint oil gel beads according to claim 3 , wherein the concentration of chitosan in the chitosan acetic acid solution is 0.2% to 1.0% (w/v), and the acetic acid The concentration of 0.1% ~ 1.5% (v/v). 15 . The method for preparing peppermint oil gel beads according to claim 4 , wherein the concentration of chitosan in the chitosan acetic acid solution is 0.2% to 1.0% (w/v), the acetic acid The concentration of 0.1% ~ 1.5% (v/v). 16 . The method for preparing peppermint oil gel beads according to claim 6 , wherein the concentration of chitosan in the chitosan acetic acid solution is 0.2% to 1.0% (w/v), the acetic acid The concentration of 0.1% ~ 1.5% (v/v). 17 . The method for preparing peppermint oil gel beads according to claim 9 , wherein the concentration of chitosan in the chitosan acetic acid solution is 0.2% to 1.0% (w/v), the acetic acid The concentration of 0.1% ~ 1.5% (v/v). 18. The preparation method of a peppermint oil gel beads according to any one of claims 1, 2, 5, 7-8, 10-12 or 14-17, wherein the core material of step (3) The ratio of the dispersion liquid to the sodium alginate solution is 1:20～1:10 (v/v), the dropping height of the syringe is 4cm～6cm, and the dropping rate is 1.5～2.0mL/min. 19. the preparation method of a kind of peppermint oil gel beads according to claim 3, is characterized in that, the ratio of core material dispersion liquid and sodium alginate solution described in step (3) is 1:20～1:10( v/v), the dripping height of the syringe is 4cm～6cm, and the dripping acceleration rate is 1.5～2.0mL/min. 20. the preparation method of a kind of peppermint oil gel beads according to claim 4, is characterized in that, the ratio of core material dispersion liquid and sodium alginate solution described in step (3) is 1:20～1:10( v/v), the dripping height of the syringe is 4cm～6cm, and the dripping acceleration rate is 1.5～2.0mL/min. 21. the preparation method of a kind of peppermint oil gel beads according to claim 6, is characterized in that, the ratio of the core material dispersion liquid and sodium alginate solution described in step (3) is 1:20～1:10( v/v), the dripping height of the syringe is 4cm～6cm, and the dripping acceleration rate is 1.5～2.0mL/min. 22. the preparation method of a kind of peppermint oil gel beads according to claim 9, is characterized in that, the ratio of the core material dispersion liquid and sodium alginate solution described in step (3) is 1:20～1:10( v/v), the dripping height of the syringe is 4cm～6cm, and the dripping acceleration rate is 1.5～2.0mL/min. 23. the preparation method of a kind of peppermint oil gel beads according to claim 13, is characterized in that, the ratio of core material dispersion liquid and sodium alginate solution described in step (3) is 1:20～1:10( v/v), the dripping height of the syringe is 4cm～6cm, and the dripping acceleration rate is 1.5～2.0mL/min. 24. Peppermint oil gel beads prepared by the method for preparing peppermint oil gel beads according to any one of claims 1 to 23. 25. A product comprising the peppermint oil gel beads of claim 24.

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