CN114540045A - Soapberry modified attapulgite and preparation method of O/W type Pickering emulsion of plant essential oil of soapberry modified attapulgite - Google Patents
Soapberry modified attapulgite and preparation method of O/W type Pickering emulsion of plant essential oil of soapberry modified attapulgite Download PDFInfo
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Abstract
The invention discloses soapberry modified attapulgite and a preparation method of a plant essential oil O/W type Pickering emulsion thereof. The invention overcomes the defect that the synthetic surfactant is used in the traditional emulsion preparation, the attapulgite modified by adopting the mechanochemical method has the characteristics of environment-friendly process, greenness, simple operation and the like, the prepared plant essential oil O/W type Pickering emulsion overcomes the defects of easy volatilization of active ingredients and the like, and the product can be used as an antibiotic substitute for safe animal breeding.
Description
Technical Field
The invention relates to soapberry modified attapulgite and a preparation method of an O/W type Pickering emulsion of plant essential oil thereof, belongs to the field of fine chemical engineering, and the product is mainly used for replacing antibiotics in livestock and poultry breeding.
Background
The Pickering emulsion is stable emulsion formed by irreversible adsorption of solid particles on an oil-water two-phase interface. Compared with the emulsion stabilized by the traditional surfactant, the Pickering emulsion has the advantages of good thermodynamic stability, wide solid particle source and the like, and is applied to the industries of food, biology, cosmetics, medicine, agriculture, petrochemical industry and the like. The stable Pickering emulsion can be divided into natural particles (such as starch, protein, polysaccharide, cellulose and clay mineral) and synthetic particles (such as SiO)2、TiO2、Fe3O4And graphene, and the like. Compared with synthetic particles, natural particles are green, non-toxic, low in price and unique in performance, and are more and more concerned about stabilization of Pickering emulsion in recent years (grain and oil food technology, 2021, 29 (3): 39-46). The emulsion with special purpose can be prepared by utilizing the functional Pickering emulsion stable particles, thereby expanding the application range of the traditional emulsion.
The stability of Pickering emulsions is affected by a number of factors, including the wettability of the solid particles, the morphology of the particles, the amount of particles used, the type and nature of the oil, the internal (external) phase volume fraction, and the order of addition during the preparation process. The influence of the wettability of solid particles on the stability of the Pickering emulsion and the type of the Pickering emulsion is the most obvious, so that the stability of the Pickering emulsion prepared by using single solid particles is relatively poor, and the stability of the Pickering emulsion can be prolonged by adopting the synergistic stability of a surfactant and the solid particles. However, the addition of synthetic surfactants limits their use in many applications. Therefore, the development of the natural surfactant synergistic solid particle stabilizer and the expansion of the Pickering emulsion in the food and safe breeding industry have important significance.
The main active component of the soapberry is soapberry saponin, is a natural nonionic surfactant, has good decontamination, foaming, sterilization and bacteriostasis, dandruff removal and itching relief, anti-inflammation, antivirus, antioxidation and other effects (chemical development 2015, 34 (12): 4343-4347; scientific report 2014, 30 (3): 35-38; trace element and health research 2016, 33 (6): 34-36). Studies show that sapindoside has excellent antibacterial activity against staphylococcus aureus, bacillus subtilis, escherichia coli and the like, and also has strong inhibitory activity against fungi such as penicillium, candida albicans and aspergillus niger (Anhui medicine, 2021, 25 (10): 1943-. The application of the soapberry saponin in the preparation process of the emulsion provides possibility for developing environment-friendly, safe and stable products, but the extraction process of the soapberry saponin is relatively complex, a large amount of waste is generated, and a new way needs to be explored for realizing the full utilization of soapberry plants in the preparation process of the emulsion.
Attapulgite has the characteristics of unique one-dimensional nanorod shape, nano-pore structure, natural electronegativity, good water dispersibility and the like, has obvious advantages in stabilizing Pickering emulsion, and is widely concerned in the preparation and application of Pickering emulsion (daily chemical industry, 2021, 51 (7): 670) -678.). However, in order to obtain a stable attapulgite Pickering emulsion, the attapulgite must be modified to adjust the surface wettability.
Disclosure of Invention
The invention aims to overcome the defect of preparing Pickering emulsion by using single natural plant particles or attapulgite, and provides soapberry modified attapulgite and a preparation method of O/W type Pickering emulsion of plant essential oil thereof.
Preparation of soapberry modified attapulgite and O/W type Pickering emulsion of plant essential oil of soapberry modified attapulgite
The invention discloses a preparation method of soapberry modified attapulgite and an O/W type Pickering emulsion of plant essential oil thereof, which comprises the following steps:
(1) mixing the soapberry and the attapulgite, uniformly spraying distilled water, and grinding for 15-30 min in a mortar grinder to obtain soapberry modified attapulgite composite particles; mixing the soapberry and the attapulgite in a mass ratio of 1: 1-1: 9; the distilled water accounts for 30-45% of the mass fraction of the attapulgite.
(2) Adding the soapberry modified attapulgite composite particles into a xanthan gum aqueous solution under stirring, continuously stirring for 10-30 min, adding the plant essential oil, and then stirring the obtained mixed system at a high speed for 2-10 min to obtain the plant essential oil O/W type Pickering emulsion.
Wherein the mass fraction of the xanthan gum aqueous solution is 0.1-0.5%. The mass fraction of the soapberry modified attapulgite composite particles in the mixed system is 0.5-2.5%. The mass ratio of the xanthan gum to the soapberry modified attapulgite is 1: 2-1: 15. The plant essential oil is at least one of carvacrol, cinnamaldehyde, oregano oil, garlicin and citral; the vegetable essential oil accounts for 2.5-10% of the mass fraction of the continuous phase. The stirring speed of the high-speed stirring is 3000-6000 r/min.
The principle of the invention is as follows: the attapulgite is modified by using nonionic surface activity and organic active substances of the soapberry through a semidry process, so that the surface hydrophilicity and hydrophobicity of the attapulgite are regulated, and meanwhile, the soapberry solid particles and the soapberry modified attapulgite composite particles are used as a synergistic stabilizer to be applied to preparation of the plant essential oil O/W type Pickering emulsion.
Secondly, the structure and the performance of the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof
FIG. 1 is an FTIR spectrum of the soapberry modified attapulgite composite particle of example 2 of the present invention. As can be seen by FTIR, compared with soapberry, the characteristic peak of the soapberry modified attapulgite composite particle has the blue shift phenomenon of-CH2Characteristic absorption peak of 2935 cm-1Shift to 2930 cm-1The hydroxyl vibration peak of attapulgite is 3620 cm-1And 3552 cm-1Offset to 3556 cm-1And 3403 cm-1. Especially soapberry at 1728 cm-1And 1632 cm-1Has a characteristic absorption peak shifted to 1738 cm-1And 1660 cm-1Further, the soapberry modified attapulgite composite particles are mainly characterized in that a certain hydrogen bond effect exists between small molecular active substances in the soapberry and silicon hydroxyl groups on the surface of the attapulgite, so that part of organic active substances are loaded on the surface of the attapulgite, and the surface hydrophilicity and hydrophobicity of the attapulgite are further changed.
FIG. 2 is an SEM photograph of modified attapulgite composite particles of Sapindus mukurossi in example 2 of the present invention. As shown in FIG. 2, the attapulgite is gathered in rod-shaped crystal bundles, and the rod-shaped crystal bundles are effectively dissociated after being modified by semi-dry grinding. The dissociated rod crystals are beneficial to the surface modification of the attapulgite by the active ingredients of the soapberry and the formation of stable O/W type Pickering emulsion of the plant essential oil.
FIG. 3 shows example 2 of modified attapulgite composite particle with soapberry seeds according to the invention10、D50、D90The value is obtained. As can be seen from FIG. 3, the modified attapulgite composite particles (200 mesh) D of Sapindus mukurossi in example 2 of the present invention10=6.38 μm，D50=25.4 μm，D90=76.9 μm。
FIG. 4 is a surface contact angle measured after tabletting of the soapberry modified attapulgite composite particles in example 2 of the present invention. The surface contact angles of the soapberry and the attapulgite are respectively 32 degrees and 23 degrees, the surface contact angle of the soapberry modified attapulgite composite particle is increased to 39.9 degrees, the surface contact angle is adopted to further prove the surface hydrophobicity change of the soapberry modified attapulgite composite particle, and the contact angle test result shows that the surface hydrophobicity of the soapberry modified attapulgite composite particle is increased, and further proves that in the semi-dry grinding process, the active substances in the soapberry and the surface of the attapulgite react to further change the surface hydrophilicity and hydrophobicity of the attapulgite.
FIG. 5 is the change rule of Zeat potential with pH of the soapberry modified attapulgite composite particle of example 2 of the present invention. Under different pH conditions, the Zeta potential of the soapberry modified attapulgite composite particles becomes more negative along with the increase of the pH, and reaches the most negative value when the pH value of a system is 9.5. When the pH value is 1.2, the Zeat potential of the soapberry modified attapulgite composite particles is a positive value, and the Zeta potential changes greatly when the pH value of the system is more than 3.4. The soapberry modified attapulgite composite particles are used as an emulsion synergistic stabilizer, so that the prepared emulsion can show pH responsiveness under different pH conditions.
FIG. 6 is an optical microscope photograph of an O/W type Pickering emulsion prepared from soapberry modified attapulgite composite particles in example 2 of the present invention. As can be seen from FIG. 6, the obtained emulsion droplets are uniform in size, and the size of the emulsion droplets is 5 to 10 μm.
FIG. 7 is a laser confocal photograph of plant essential oil O/W type Pickering emulsion prepared from soapberry modified attapulgite composite particles in example 2. It can be seen that, the emulsion prepared by repeating the step of example 2 after the attapulgite is dyed by using the safranine T, fluorescence imaging of the emulsion at the excitation wavelength of 488 nm and 559 nm is performed, and the soapberry modified attapulgite composite particles are uniformly distributed on the two-phase interface of the liquid drops, thereby further showing that the soapberry modified attapulgite composite particles realize the synergistic effect of preparing the O/W type Pickering emulsion.
FIG. 8 is a digital photograph of the stability of the emulsion obtained in the example of the present invention after standing for 60 days. As can be seen, the emulsions obtained in examples 1 and 5 were more stable, whereas the emulsions were observed to break when the comparative example was used as a control. Emulsion stability experiments further show that the soapberry modified attapulgite composite particles have good stability compared with an emulsion prepared by the single soapberry and attapulgite composite in a synergistic manner.
The plant essential oil O/W type Pickering emulsion disclosed by the invention adopts a colony counting method for evaluating the antibacterial performance, and the specific test steps refer to the 2002 edition disinfection technical specification 2.1.8 antibacterial (bacteriostasis) test of Ministry of public health. The emulsion prepared by the invention has excellent antibacterial activity on Escherichia coli and staphylococcus aureus, and the highest antibacterial rate on Escherichia coli and staphylococcus aureus can reach 100%.
In summary, the present invention has the following advantages over the prior art:
1. the attapulgite is modified by using the nonionic surface activity of the soapberry by adopting a semidry process, so that the effective dissociation of attapulgite rod crystal beams is realized in the process, the hydrophilic and hydrophobic adjustment of the surface of the attapulgite is realized, and the defect of stable emulsion of single natural plant particles or the attapulgite is overcome.
2. By utilizing the action of the nonionic surfactant contained in the soapberry and the synergistic action of the soapberry plant particles and the modified attapulgite composite particles, the synergistic stability of the plant essential oil O/W type Pickering emulsion is realized, and the defects of easy volatilization of the active ingredients of the plant essential oil and the like are effectively overcome.
3. The attapulgite modified by the mechanochemical method has the characteristics of environment-friendly process, environmental protection, simple operation and the like.
Drawings
FIG. 1 FTIR spectrum of soapberry modified attapulgite composite particle of example 2 of the present invention;
FIG. 2 is an SEM photograph of modified attapulgite composite particles of Sapindus mukurossi in example 2 of the present invention;
FIG. 3 example 2 of the present invention shows modified attapulgite composite particles D of Sapindus mukorossi10、D50、D90A value;
FIG. 4 shows the surface contact angle of the soapberry modified attapulgite composite particle of example 2 of the present invention after tabletting;
FIG. 5 shows the change rule of Zeat potential with pH of the soapberry modified attapulgite composite particle in example 2 of the present invention;
FIG. 6 is an optical microscope photograph of an O/W type Pickering emulsion prepared from soapberry modified attapulgite composite particles in example 2 of the present invention;
FIG. 7 is a laser confocal photograph of plant essential oil O/W type Pickering emulsion prepared by the soapberry modified attapulgite composite particles in example 2;
FIG. 8 is a digital photograph of the stability of the emulsion obtained in the example of the present invention after standing for 60 days.
Detailed Description
The following describes the preparation method of the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion in detail with reference to specific examples.
Example 1
Mixing the soapberry and the attapulgite in a mass ratio of 1: 4, uniformly spraying distilled water with the mass fraction of 35% of the attapulgite, placing the mixture in a grinding instrument, grinding for 30min, and sieving with a 200-mesh sieve to obtain the soapberry modified attapulgite composite particles. Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.25% in a 250 mL beaker, adding soapberry modified attapulgite composite particles with the mass fraction of 1% at the stirring speed of 600 r/min, stirring for 10min, adding carvacrol with the mass fraction of 5% of that of the continuous phase, and stirring for 2 min at the stirring speed of 4000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Example 2
Mixing the soapberry and the attapulgite in a mass ratio of 1:1, uniformly spraying distilled water with the mass fraction of 45% of the attapulgite, placing the mixture in a grinding instrument, grinding for 20 min, and sieving with a 200-mesh sieve to obtain the soapberry modified attapulgite composite particles. Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.35% in a 250 mL beaker, adding soapberry modified attapulgite composite particles with the mass fraction of 2.5% at the stirring speed of 600 r/min, stirring for 10min, adding cinnamaldehyde with the mass fraction of 10% of that of the continuous phase, and stirring for 4min at the stirring speed of 6000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Example 3
Mixing the soapberry and the attapulgite in a mass ratio of 1:9, uniformly spraying distilled water with the mass fraction of the attapulgite being 40%, placing the mixture in a grinding instrument, grinding for 15 min, and sieving with a 200-mesh sieve to obtain the soapberry modified attapulgite composite particles. Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.25% in a 250 mL beaker, adding 0.5% of soapberry modified attapulgite composite particles at the stirring speed of 600 r/min, stirring for 10min, adding oregano oil with the mass fraction of 2.5% of the continuous phase, and stirring for 6 min at the stirring speed of 3000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Example 4
Mixing the soapberry and the attapulgite according to the mass ratio of 3: 7, uniformly spraying distilled water with the mass fraction of 42% of the attapulgite, placing the mixture in a grinding instrument, grinding for 30min, and sieving with a 200-mesh sieve to obtain the soapberry modified attapulgite composite particles. Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.5% in a 250 mL beaker, adding soapberry modified attapulgite composite particles with the mass fraction of 2% at the stirring speed of 600 r/min, stirring for 10min, adding cinnamaldehyde with the mass fraction of 2.5% of that of a continuous phase and citral with the mass fraction of 2.5% of that of the continuous phase, and stirring for 8min at the stirring speed of 4000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Example 5
Mixing the soapberry and the attapulgite according to the mass ratio of 2: 3, uniformly spraying distilled water with the mass fraction of 39% of the attapulgite, placing the mixture in a grinding instrument, grinding for 30min, and sieving with a 200-mesh sieve to obtain the soapberry modified attapulgite composite particles. Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.1% in a 250 mL beaker, adding soapberry modified attapulgite composite particles with the mass fraction of 1.5% at the stirring speed of 600 r/min, stirring for 10min, adding allicin with the mass fraction of 5% of that of the continuous phase, and stirring for 10min at the stirring speed of 5000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Comparative example
Weighing 50 mL of xanthan gum aqueous solution with the mass fraction of 0.35% in a 250 mL beaker, adding attapulgite with the mass fraction of 1.25% and soapberry particles with the mass fraction of 1.25% under the stirring speed of 600 r/min, stirring for 10min, adding cinnamaldehyde with the mass fraction of 10% of that of the continuous phase, and stirring for 4min under the stirring speed of 6000r/min to obtain the plant essential oil O/W type Pickering emulsion.
Table 1 shows the results of the tests of the samples obtained in the examples on the inhibition rate of Escherichia coli and Staphylococcus aureus. It can be seen from the table that the emulsions prepared in the examples have excellent antibacterial activity against escherichia coli and staphylococcus aureus, wherein the emulsion prepared in the example 2 has the best antibacterial activity, the antibacterial rates against escherichia coli and staphylococcus aureus reach 100%, the antibacterial rates against escherichia coli and staphylococcus aureus of the emulsions prepared in the comparative examples are 73% and 79%, respectively, and the antibacterial effect is significantly lower than that of the emulsion prepared in the example 2.
Claims (8)
1. A preparation method of soapberry modified attapulgite and an O/W type Pickering emulsion of plant essential oil thereof comprises the following steps:
(1) mixing the soapberry and the attapulgite, uniformly spraying distilled water, and grinding for 15-30 min in a mortar grinder to obtain soapberry modified attapulgite composite particles;
(2) adding the soapberry modified attapulgite composite particles into a xanthan gum aqueous solution under stirring, continuously stirring for 10-30 min, adding the plant essential oil, and then stirring the obtained mixed system at a high speed for 2-10 min to obtain the plant essential oil O/W type Pickering emulsion.
2. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (1), the soapberry and the attapulgite are mixed according to the mass ratio of 1: 1-1: 9.
3. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (1), the distilled water accounts for 30-45% of the mass fraction of the attapulgite.
4. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (2), the mass fraction of the xanthan gum aqueous solution is 0.1-0.5%.
5. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (2), the mass fraction of the soapberry modified attapulgite composite particles in the mixed system is 0.5-2.5%.
6. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (2), the mass ratio of the xanthan gum to the soapberry modified attapulgite is 1: 2-1: 15.
7. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (2), the plant essential oil is at least one of carvacrol, cinnamaldehyde, oregano oil, garlicin and citral; the vegetable essential oil accounts for 2.5-10% of the mass fraction of the continuous phase.
8. The method for preparing the soapberry modified attapulgite and the plant essential oil O/W type Pickering emulsion thereof according to claim 1, wherein the method comprises the following steps: in the step (2), the stirring speed of the high-speed stirring is 3000-6000 r/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115336598A (en) * | 2022-09-03 | 2022-11-15 | 甘肃中医药大学 | Application and preparation method of cinnamon essential oil Pickering emulsion |
| CN115349529A (en) * | 2022-09-22 | 2022-11-18 | 中国科学院兰州化学物理研究所 | Method for preparing Pickering antibacterial emulsion by dissociating attapulgite by using rod crystal bundles and stabilizing plant essential oil |
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