CN118085331A - Preparation method of double gel - Google Patents
Preparation method of double gel Download PDFInfo
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- CN118085331A CN118085331A CN202410227652.2A CN202410227652A CN118085331A CN 118085331 A CN118085331 A CN 118085331A CN 202410227652 A CN202410227652 A CN 202410227652A CN 118085331 A CN118085331 A CN 118085331A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000499 gel Substances 0.000 claims abstract description 106
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 51
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 51
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000008117 stearic acid Substances 0.000 claims abstract description 51
- 239000003921 oil Substances 0.000 claims abstract description 28
- 235000019198 oils Nutrition 0.000 claims abstract description 25
- 229920001817 Agar Polymers 0.000 claims abstract description 22
- 239000008272 agar Substances 0.000 claims abstract description 22
- 239000000017 hydrogel Substances 0.000 claims abstract description 15
- 238000001879 gelation Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 4
- 239000003549 soybean oil Substances 0.000 claims abstract description 4
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 41
- 239000000600 sorbitol Substances 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 9
- 230000009977 dual effect Effects 0.000 claims description 4
- WERKSKAQRVDLDW-ANOHMWSOSA-N [(2s,3r,4r,5r)-2,3,4,5,6-pentahydroxyhexyl] (z)-octadec-9-enoate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO WERKSKAQRVDLDW-ANOHMWSOSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 238000001514 detection method Methods 0.000 description 9
- 239000000693 micelle Substances 0.000 description 8
- 230000003993 interaction Effects 0.000 description 6
- 230000007704 transition Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000003431 cross linking reagent Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 230000000975 bioactive effect Effects 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000005102 attenuated total reflection Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 230000010355 oscillation Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000013191 viscoelastic testing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000004736 wide-angle X-ray diffraction Methods 0.000 description 1
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- Colloid Chemistry (AREA)
Abstract
The invention belongs to the technical field of double gel, and discloses a preparation method of double gel, which comprises the following steps: dissolving agar powder in 95 ℃ water to obtain agar solution, and cooling to room temperature to induce gelation to obtain hydrogel; compounding the oil gel and stearic acid, adding the oil gel into soybean oil, stirring, heating to 70 ℃ for dissolution to obtain a uniform transparent solution, and cooling to room temperature to induce gelation for 24 hours to obtain oil gel; and uniformly mixing the obtained oleogel and hydrogel, and cooling to room temperature to induce gelation for 24 hours to obtain the double gel. The invention constructs a new double gel system, which has the advantages of good network rigidity, simple preparation process and low material cost.
Description
Technical Field
The invention belongs to the technical field of double gel, and particularly relates to a preparation method of double gel.
Background
The double gel is a semisolid preparation with a network interpenetrating structure, which is constructed by hydrogel and oleogel, is used as a 'double reservoir' of water-soluble and fat-soluble active ingredients and is often used for a delivery system of the bioactive ingredients, and is commonly used in the fields of foods, cosmetics, medicines and the like because of the slow release effect of the double gel on the bioactive ingredients. Double gels are classified into three types (oil-in-water, bicontinuous, water-in-oil), wherein oil-in-water double gels have little ability to load bioactive components due to little oil content, which is unfavorable for the loading of lipophilic components; the water-in-oil double gel also has the same heavy greasy feel as the oil gel, and has limited application. When the water-oil two-phase content in the double gel system is similar, two double continuous double gels which are mutually dispersed phases can be formed, and the double gel system has the maximum loading capacity on hydrophilic and lipophilic components and also has better skin feel and is widely concerned.
The stability of the bicontinuous bisgel is significantly affected by the oleogel. The oleogel is mainly classified into a crystal type and a micelle type. In constructing a bicontinuous dual gel network, a crystalline gellant is typically required to form a stable gel network by the action of a cross-linking agent. However, the cross-linking agent has a certain toxicity, which places a certain limit on the use of the double gel. Sorbitol monostearate is used as a micelle type gel, and is characterized in that a bicontinuous double-gel network can be constructed together with hydrogel without using a cross-linking agent. This feature avoids the toxicity problem of the cross-linking agent, making sorbitol monostearate a good prospect in the application of bicontinuous double gel. However, it is notable that the bicontinuous double gel constructed with sorbitol monostearate has the problem of insufficient stability, which is liable to cause oil leakage. Therefore, how to improve the stability of the bicontinuous type biconcave constructed by sorbitol monostearate is an important problem to be solved currently and urgently, which has an important influence on the practical application of the bicontinuous type biconcave.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention provides a preparation method of double gel.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing a dual gel comprising the steps of:
(1) Preparation of agar hydrogel: dissolving agar powder in 95 ℃ water to obtain agar solution, and cooling to room temperature to induce gelation for 24 hours to obtain hydrogel;
(2) Preparation of oleogel: compounding the oil gel and stearic acid, adding the oil gel into soybean oil, stirring, heating to 70 ℃ for dissolution to obtain a uniform transparent solution, and cooling to room temperature to induce gelation for 24 hours to obtain oil gel;
(3) Preparation of a double gel: the obtained oleogel and hydrogel are uniformly mixed at 70 ℃, and cooled to room temperature to induce gelation for 24 hours to obtain double gel.
Preferably, the mass concentration of the agar solution is 1%.
Preferably, the stirring rate in step (2) is 350rpm.
Preferably, the oil gel is selected from one or more of sorbitol monolaurate, sorbitol monopalmitate, sorbitol monostearate and sorbitol monooleate.
Preferably, the oleogel is sorbitol monostearate.
Preferably, the mass ratio of hydrogel to oleogel in step (3) is 5:5.
Preferably, the mass ratio of the oleogel to the stearic acid in the double gel is 8:2-7:3.
In light of the foregoing, the combination of oleogel and stearic acid is particularly important to the present invention. When the micelle type oil gel is singly used for preparation, and the micelle type oil gel and agar form double gel, the distribution of a double gel network is uneven, so that the capability of intercepting liquid drops is insufficient, the double gel generates a liquid leakage phenomenon, and the double gel is unstable. When the micelle type oil gel and stearic acid are compounded, a synergistic effect is generated between the two gels, so that the interaction between the oil gel and agar is promoted, and the stability of a double gel network is enhanced. However, when stearic acid is added in excess, the stearic acid itself forms a crystal structure, which interferes with the synergistic effect between the oleogel and the agar, resulting in instability of the double gel. Therefore, the mass ratio of the oil gel agent to the stearic acid in the preferable double gel is 8:2-7:3, and the stearic acid can form a synergistic effect with the micelle type oil gel agent within the range of the mass ratio, so that the double gel system is stabilized.
Compared with the prior art, the invention provides a preparation method of the double gel, which has the following beneficial effects:
The invention constructs a new bicontinuous double-gel network system, and the micelle type oil gel and the hydrophobic tail chain of stearic acid can generate synergistic effect when the network is constructed together, so that the micelle type oil gel-agar constructed bicontinuous double-gel is regulated and controlled by the stearic acid, and the performance of the network is changed. The bicontinuous double gel system constructed by the invention does not need to use a cross-linking agent, is green and safe, and the formed bicontinuous gel has no oil leakage phenomenon, so that the shelf life is prolonged. Meanwhile, the invention has the advantages of cheap and easily obtained raw materials, no expensive instrument and equipment in the experimental process, simple and quick operation and good repeatability, and is suitable for further popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is an optical micrograph of examples 1-2 and comparative examples 1-4.
FIG. 2 is XRD patterns of examples 1-2 and comparative examples 1-4.
FIG. 3 is a FTIR spectrum of examples 1-2 and comparative examples 1-4.
FIG. 4 is a graph showing the melting temperature change tendencies of examples 1-2 and comparative examples 1-4.
FIG. 5 is a dynamic frequency scan of examples 1-2 and comparative examples 1-4.
FIG. 6 is a graph showing the phase transition temperature change trend of examples 1-2 and comparative examples 1-4.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for preparing a dual gel comprising the steps of:
(1) Preparation of agar hydrogel: dissolving agar powder in 95 ℃ water to obtain agar solution, and cooling to room temperature to induce gelation for 24 hours to obtain hydrogel;
(2) Preparation of oleogel: the sorbitol monostearate and stearic acid are compounded, added into soybean oil, heated to 70 ℃ for dissolution under stirring to obtain a uniform transparent solution, cooled to room temperature and gelled for 24 hours to obtain oil gel;
(3) Preparation of a double gel: and uniformly mixing the obtained oleogel and hydrogel, and cooling to room temperature to induce gelation for 24 hours to obtain the double gel.
The mass concentration of the agar solution is 1%.
The stirring rate in step (2) was 350rpm.
The mass ratio of sorbitol monostearate to stearic acid in the double gel is 8:2.
The mass ratio of the hydrogel to the oleogel in the step (3) is 5:5.
Example 2
The technical scheme of example 2 is the same as that of example 1, except that the mass ratio of sorbitol monostearate to stearic acid in the double gel is 7:3.
Comparative example 1
The protocol of comparative example 1 is the same as that of example 1, except that the mass ratio of sorbitol monostearate to stearic acid in the double gel is 6:4.
Comparative example 2
The solution of comparative example 2 is the same as in example 1, except that the mass ratio of sorbitol monostearate to stearic acid in the double gel is 10:0.
Comparative example 3
The solution of comparative example 3 is the same as that of example 1, except that the mass ratio of sorbitol monostearate to stearic acid in the double gel is 5:5.
Comparative example 4
The solution of comparative example 4 is the same as in example 1, except that the mass ratio of sorbitol monostearate to stearic acid in the double gel is 4:6.
Characterization experiments:
(1) Morphological analysis
The sorbitol monostearate and stearic acid bicontinuous double gel with different proportions are observed under 400 times magnification by using an XSP-13C-LP optical microscope and a matched digital camera and software.
(2) XRD detection
The oil gel was subjected to X-ray diffraction (XRD) analysis. The sample was mounted on a die and sent to a D8 advanced X-ray diffractometer. The X-ray diffractometer was equipped with a cuka source (λ=1.54), operating at 40kV and 40mA, recording wide angle X-ray diffraction in the range 5 ° to 50 ° at a speed of 2 °/min.
(3) FTIR detection
FTIR experiments were performed on samples lyophilized at different ratios using VERTEX fourier transform infrared spectrometer. The spectrum of the formulation was recorded in ATR (attenuated total reflectance) mode, measured by 16 scans at a speed of 2cm -1 over the wavelength range 4000-400cm -1.
(4) DSC detection
The lyophilized samples (15-20 mg) were precisely weighed into an aluminum crucible and sealed with a perforated aluminum lid, heated at a scanning rate of 5 ℃ min -1 using a STA 409PC differential scanning calorimeter in the temperature range of 30-150 ℃ and the heat distribution of the samples was measured.
(5) Linear viscoelastic detection
The oscillation strain of the linear viscoelasticity was determined to be 0.1% by oscillation-amplitude mode at 25 ℃ using a stress rheometer (TA instruments waters, HR 10, usa) and the accompanying software. The trend of the change in elastic modulus and loss modulus was observed by moving the bicontinuous bisgel from a frequency of 100-0.1rad/s in the linear viscoelastic range.
(6) Temperature ramp detection
The oleogel was subjected to oscillation-temperature ramp scan from a temperature range of 25 ℃ to 120 ℃ at 1Hz and 0.1% strain using an HR 10 rheometer equipped with 40mm parallel plates and associated software.
Results:
(1) Morphological analysis results
FIG. 1 is an optical micrograph of the double gels obtained in examples 1-2 and comparative examples 1-4, each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. According to fig. 1, when the size difference of the entrapped drops of bicontinuous double gel formed by the individual sorbitol monostearate is very different, when stearic acid is added to the sorbitol monostearate and the stearic acid is 8:2-7:3, the entrapped drop difference is reduced, when the stearic acid is added to the sorbitol monostearate and the stearic acid is added to the sorbitol monostearate, aggregation occurs between the drops, and the aggregation phenomenon is aggravated along with the increase of the addition amount of the stearic acid. Thus, the above ratio range can form a good double gel effect.
(2) XRD detection results
FIG. 2 is an XRD spectrum of the double gels obtained in examples 1-2 and comparative examples 1-4, BG representing the double gel, each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. According to fig. 2, there is a peak at 21.539 ° at all ratios, which is not related to stearic acid addition, whereas stearic acid addition in excess of 6:4 forms crystals, possibly interfering with the interaction between sorbitol monostearate and agar.
(3) FTIR detection analysis
FIG. 3 is a FTIR spectrum of the double gel obtained in examples 1-2 and comparative examples 1-4, BG representing the double gel, each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. According to fig. 3, when sorbitol monostearate: stearic acid in a ratio in the range of 10:0 to 4:6, at 3500
A broad peak of hydroxyl stretching vibration at-3700 cm -1 was present, indicating an interaction between sorbitol monostearate and stearic acid. When sorbitol monostearate: at a ratio of stearic acid in the range of 10:0-7:3, an interaction peak between sorbitol monostearate and agar occurs at 3200-3500cm -1, whereas this peak disappears at a ratio of stearic acid exceeding 6:4, indicating that crystals of stearic acid themselves interfere with the interaction between sorbitol monostearate and agar.
(4) DSC detection result
FIG. 4 is a graph showing the melting temperature change trend of the double gels obtained in examples 1-2 and comparative examples 1-4, BG representing the double gel, and each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. According to fig. 4, the melting temperature of the gel network increased significantly when stearic acid was added to 8:2, indicating that stearic acid regulates the gel network of the bicontinuous double gel, which increased stability. As stearic acid increases, the melting temperature decreases, indicating that the addition of excess stearic acid at this time interferes with the interaction between sorbitol monostearate and agar.
(5) Results of the Linear viscoelastic test
FIG. 5 is a dynamic frequency scan of the double gels obtained in examples 1-2 and comparative examples 1-4, BG representing the double gel and each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. According to fig. 5, when stearic acid was added to the bicontinuous double gel of sorbitol monostearate alone to a mass ratio of sorbitol monostearate to stearic acid of 8:2, G' suddenly increased, the rigidity of the gel network increased, and the stability increased. While continuing to add stearic acid, G' begins to decrease and rigidity gradually decreases. Thus, a small amount of stearic acid can enhance the rigidity and stability of the gel network between sorbitol monostearate and agar.
(6) Phase transition temperature detection result
FIG. 6 is a graph showing the change in phase transition temperature of the double gels obtained in examples 1-2 and comparative examples 1-4, BG representing the double gel, and each ratio representing the mass ratio of sorbitol monostearate to stearic acid in the double gel. As can be seen from fig. 6, stearic acid was added to sorbitol monostearate: at 8:2 stearic acid, the phase transition temperature increased significantly, indicating that the addition of a small amount of stearic acid significantly enhanced the stability of the gel network, whereas continuing to increase the stearic acid content, the phase transition temperature did not increase until it was added to 5:5, and the phase transition temperature increased significantly, due to the large amount of crystal structure generated in the gel network.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the solution disclosed in the embodiments, since it corresponds to the method disclosed in the embodiments, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. A method for preparing a dual gel, comprising the steps of:
(1) Preparation of agar hydrogel: dissolving agar powder in 95 ℃ water to obtain agar solution, and cooling to room temperature to induce gelation for 24 hours to obtain hydrogel;
(2) Preparation of oleogel: compounding the oil gel and stearic acid, adding the oil gel into soybean oil, stirring, heating to 70 ℃ for dissolution to obtain a uniform transparent solution, and cooling to room temperature to induce gelation for 24 hours to obtain oil gel;
(3) Preparation of a double gel: and uniformly mixing the obtained oleogel and hydrogel, and cooling to room temperature to induce gelation for 24 hours to obtain the double gel.
2. The method for preparing the double gel according to claim 1, wherein the oil gel is one or more selected from the group consisting of sorbitol monolaurate, sorbitol monopalmitate, sorbitol monostearate and sorbitol monooleate.
3. The method for preparing a double gel according to claim 2, wherein the oleogel is sorbitol monostearate.
4. The method for preparing the double gel according to claim 1, wherein the mass ratio of the oleogel to the stearic acid in the double gel is 8:2-7:3.
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