Demulsification method and embedding rate detection method of oral emulsion containing eucalyptol, limonene and α-pinene
By mixing isopropanol with oral emulsions containing eucalyptus, limonene and alpha-pinene, cracking the emulsion and releasing eucalyptus, the problem of difficulty in detecting embedding rates in the prior art is solved, and rapid and accurate Detection effect.
Patent Information
- Application Number
- CN202010986954.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2020-09-18
- Publication Date
- 2025-02-11
- Estimated Expiration
- 2040-09-18
AI Technical Summary
The prior art is difficult to effectively crack oral emulsions containing eucalyptus, limonene and alpha-pinene, resulting in difficulty in detecting the embedding rate.
Isopropanol is mixed with oral emulsion, and through the action of isopropanol and the interface mask, the emulsion is cracked and the eucalyptus is released, thereby achieving accurate detection of the emulsion rate.
It achieves rapid and complete demulsification of oral emulsion, obtains a clear and transparent solution, ensuring accurate detection of eucalyptus cerevisiae, good repeatability, and is suitable for promotion and application.
Abstract
Description
Technical Field
[0001] The present invention relates to the field of medicine. Specifically, the present invention relates to a method for demulsifying an oral emulsion containing eucalyptol, limonene and α-pinene and a method for detecting the embedding rate of eucalyptol, limonene and α-pinene. Background Art
[0002] In the oral emulsion containing eucalyptol, limonene and α-pinene, eucalyptol, limonene and α-pinene (referred to as eucalyptol), water, surfactant and co-surfactant form an oil-in-water microemulsion.
[0003] Encapsulation rate refers to the percentage of the encapsulated eucalyptus citrinum and pinene in the total amount of active ingredients in the oral emulsion. It is an important indicator for the preparation process and quality evaluation of the preparation, and is also the key to improving the drug therapeutic index, reducing adverse drug reactions and reducing drug dosage. Therefore, the encapsulation rate is an important inspection item for the quality evaluation of eucalyptus citrinum and pinene oral emulsion. Its calculation formula is as follows:
[0004]
[0005] From the above formula, it can be seen that to calculate the encapsulation rate of eucalyptol citrinum pine oral emulsion, it is necessary to detect the total amount of eucalyptol citrinum pine in the emulsion and the amount of free eucalyptol citrinum pine. The determination of the total amount of eucalyptol citrinum pine requires breaking the microemulsion and releasing eucalyptol citrinum pine from the microemulsion droplets, so that the measured encapsulation rate is accurate and reliable. The free eucalyptol citrinum pine oil can be directly extracted.
[0006] Since the particle size of eucalyptus citronella oral emulsion is at the nanometer level, the microemulsion formed is very stable, which makes demulsification difficult. Therefore, the detection method of eucalyptus citronella encapsulation rate in eucalyptus citronella oral emulsion still needs to be studied. Summary of the invention
[0007] The present invention aims to solve the problems of the prior art at least to a certain extent. To this end, the present invention proposes a demulsification method for an oral emulsion containing eucalyptol, limonene and α-pinene, a method for detecting the embedding rate of eucalyptol, limonene and α-pinene in the oral emulsion containing eucalyptol, limonene and α-pinene, and a method for controlling the quality of the oral emulsion containing eucalyptol, limonene and α-pinene. The demulsification method can completely demulsify the oral emulsion to release the eucalyptol, limonene and α-pinene embedded therein, thereby accurately determining the embedding rate thereof, with good repeatability, and is suitable for popularization and application.
[0008] In one aspect of the present invention, the present invention provides a method for demulsifying an oral emulsion containing eucalyptol, limonene and α-pinene. According to an embodiment of the present invention, the method comprises: mixing the oral emulsion with isopropyl alcohol.
[0009] Since the particle size of eucalyptus, lemon and pinene oral liquid is nanometer-level, the microemulsion is very stable. The inventor has tried a variety of conventional demulsification methods, such as acetonitrile, anhydrous sodium sulfate, concentrated HCl, freezing and other methods. Even after auxiliary treatments such as ultrasound and centrifugation, it is impossible to achieve rapid and complete demulsification of the emulsion. Methanol, ethanol and n-octanol cannot demulsify. Attempts to use dextran gel resin G25 and G50 column chromatography to extract the emulsion layer by layer also cannot achieve complete demulsification. Then, after a large number of theoretical analyses and experimental optimizations, the inventor found that the use of isopropanol can effectively achieve the purpose of demulsification. After it acts on the interface film, it replaces the emulsifier on the oil-water interface film to form a new interface film. The elasticity, tension and life of the interface film are all reduced. Since there are side chains in the chemical structure of isopropanol and the molecular weight is small, under external force (such as manual shaking), the side chain molecules of isopropanol can enter the gap of the surfactant molecular structure, and the interface film breaks, so that eucalyptus, lemon and pinene are released from the film. Due to the good solubility of isopropanol, all components are miscible with it after demulsification, and the whole system forms a clear, transparent and stable solution. Eucalyptus citronella is completely dissolved without affecting the texture and properties of eucalyptus citronella. This is helpful for subsequent testing of eucalyptus citronella, such as determining the encapsulation rate, and has broad application prospects.
[0010] According to an embodiment of the present invention, the demulsification method of the oral emulsion containing eucalyptol, limonene and α-pinene may also have the following additional technical features:
[0011] According to an embodiment of the present invention, the volume ratio of the oral emulsion to isopropanol is 1: (4-8). When the amount of isopropanol added is low, it is necessary to assist with ultrasound and centrifugation to achieve complete demulsification of the emulsion. The entire experimental process is cumbersome and time-consuming. In addition, since the oral emulsion contains oil (such as soybean oil) and eucalyptus citrinum has good solubility in oil, if the content of eucalyptus citrinum is to be accurately determined, the oil needs to be completely dissolved. If there is less isopropanol, the water content in the entire system is relatively high, and it is difficult to completely dissolve the system with a solvent with a strong polarity or a polarity greater than isopropanol (such as methanol, ethanol, acetonitrile, etc.) to form a clear and transparent solution. Therefore, it is necessary to extract the main component with a weakly polar solvent (such as n-hexane). In the step of collecting the extract, it is difficult to completely collect the supernatant and accurately determine it. Therefore, the detected eucalyptus citrinum content is not accurate enough.
[0012] To this end, the inventor further increased the amount of isopropanol added. When the volume ratio of the oral emulsion to isopropanol is 1: (4-8), no auxiliary ultrasound, centrifugation or other equipment is required, and only manual shaking can be used to achieve complete demulsification to obtain a clear and transparent solution. In addition, the water content in the entire system is reduced, and the components in the oral emulsion are well dissolved in isopropanol. The experimental results show that under the selected isopropanol ratio, eucalyptus, lemon and pinene can be well dissolved in isopropanol to form a clear and transparent solution. Therefore, there is no need to extract the main components. The entire demulsification process has few steps, simple operation, less time consumption, no loss of active ingredients, and the content results detected are accurate and reliable.
[0013] According to an embodiment of the present invention, the oral emulsion comprises eucalyptol, limonene, α-pinene, oil, emulsifier, co-emulsifier and water. The present invention does not strictly limit the types of oil, emulsifier and co-emulsifier, and substances known in the art can be used, which can be flexibly selected according to actual conditions.
[0014] In another aspect of the present invention, the present invention provides a method for detecting the embedding rate of eucalyptol, limonene and α-pinene in an oral emulsion containing eucalyptol, limonene and α-pinene. According to an embodiment of the present invention, the method includes: using the above-mentioned demulsification method to demulsify an oral emulsion containing eucalyptol, limonene and α-pinene to obtain a demulsified liquid; diluting the demulsified liquid with a first diluent to obtain a demulsified sample solution; mixing the oral emulsion with a second diluent, standing, and taking the supernatant to obtain an undemulsified sample solution; diluting eucalyptol, limonene, α-pinene and a third diluent to obtain a reference solution; respectively determining the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution; based on the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution, determining the embedding rate of eucalyptol, limonene and α-pinene in the oral emulsion.
[0015] As mentioned above, isopropanol can be used to quickly and completely break the emulsion. In addition, due to the good solubility of isopropanol, all components are miscible with it after breaking the emulsion, and the entire system forms a clear, transparent, and stable solution. The eucalyptus citronella oil is completely dissolved without affecting the texture and characteristics of the eucalyptus citronella oil, thereby accurately determining its embedding rate with good repeatability. No auxiliary treatment such as ultrasound and centrifugation is required, and the entire detection step is simple to operate and takes a short time.
[0016] According to an embodiment of the present invention, the first diluent is selected from ethyl acetate. If the amount of isopropanol added is increased to replace the addition of the diluent, on the one hand, the detection cost is increased due to the high price of isopropanol. On the other hand, for oral emulsions with high oil content, even if the amount of isopropanol added is increased, it is difficult to completely dissolve the oil, and ethyl acetate with weaker polarity than it needs to be added to assist dissolution. After a large number of experimental screenings, the inventor found that ethyl acetate can dissolve components such as eucalyptus, citronella, oil, surfactant, water, and form a homogeneous system with isopropanol. Moreover, ethyl acetate plays a certain role in promoting demulsification, further achieving complete demulsification. Other solvents, such as n-hexane, although they can also dissolve all components, their mutual solubility with isopropanol is low, and stratification is easy to occur, that is, some eucalyptus, citronella are dissolved in n-hexane, and some are dissolved in isopropanol. The subsequent detection of the eucalyptus, citronella content in n-hexane only causes the loss of eucalyptus, citronella in isopropanol, resulting in a low embedding rate test result.
[0017] According to an embodiment of the present invention, the second diluent is selected from n-hexane or cyclohexane. The second diluent is used to dilute the oral emulsion so as to dissolve the free eucalyptol citrinum pinene (i.e., the eucalyptol citrinum pinene that is not embedded) therein. The inventors have screened through a large number of experiments that n-hexane and cyclohexane can effectively extract the free eucalyptol citrinum pinene so as to facilitate the subsequent determination of its content. If other solvents, such as ethyl acetate, are used, they will play a certain role in demulsification, resulting in the freeing of the embedded eucalyptol citrinum pinene, thereby making the detection result of the embedding rate higher.
[0018] According to an embodiment of the present invention, the third diluent is selected from ethyl acetate or n-hexane. Both ethyl acetate and n-hexane can effectively dissolve Eucalyptus citratus and form a homogeneous system, so as to facilitate the subsequent determination of its content.
[0019] According to an embodiment of the present invention, the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution are detected by gas chromatography, thereby improving the accuracy of the detection results and simplifying the operation.
[0020] According to an embodiment of the present invention, the embedding rate of eucalyptol, limonene and α-pinene in the oral emulsion is calculated based on the following formula: embedding rate = (the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution - the sum of the contents of eucalyptol, limonene and α-pinene in the undemulsified sample solution) × 100% ÷ (the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution). Thus, the embedding rate of eucalyptol, limonene and α-pinene in the oral emulsion can be calculated.
[0021] It should be noted that the characteristics and advantages described above for the demulsification method of the oral emulsion containing eucalyptol, limonene and α-pinene are also applicable to the embedding rate detection method and will not be described in detail here.
[0022] In another aspect of the present invention, the present invention proposes a quality control method for an oral emulsion containing eucalyptol, limonene and α-pinene. According to an embodiment of the present invention, the method comprises: determining the embedding rate of the oral emulsion according to the embedding rate detection method described above; if the embedding rate of the oral emulsion is less than the threshold value, it indicates that the quality of the oral emulsion does not meet the standard; if the embedding rate of the oral emulsion is greater than or equal to the threshold value, it indicates that the quality of the oral emulsion meets the standard. As mentioned above, the embedding rate of eucalyptol, limonene and α-pinene in the oral emulsion can be accurately determined by the aforementioned method for detecting the embedding rate, so as to determine whether the quality of the oral emulsion meets the requirements. Specifically, the threshold value is not strictly limited and can be flexibly selected according to actual needs.
[0023] It should be noted that the features and advantages described above for the embedding rate detection method are also applicable to this quality control method and will not be repeated here.
[0024] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. DETAILED DESCRIPTION
[0025] The scheme of the present invention will be explained below in conjunction with the embodiments. It will be appreciated by those skilled in the art that the following embodiments are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. Where specific techniques or conditions are not indicated in the embodiments, the techniques or conditions described in the literature in this area or the product specifications are used. The reagents or instruments used are not indicated by the manufacturer and are all conventional products that can be obtained commercially.
[0026] Composition of Eucalyptus citrinum oral emulsion:
[0027] 14 parts of eucalyptol, 15 parts of limonene, 6 parts of α-pinene, 15 parts of soybean oil, 2 parts of Tween 80 and Span 80 composite emulsifier, 6 parts of 1,2-propylene glycol, and 30 parts of water.
[0028] Example 1
[0029] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 50 mL volumetric flask, add ethyl acetate to dissolve, dilute and make up to the mark.
[0030] (2) Demulsified sample solution: Take 0.5 mL of milky white eucalyptus, lemon and pinene oral emulsion and place it in a 10 mL volumetric flask, add 3 mL of isopropanol, and gently shake to obtain a clear and transparent solution. Dilute with ethyl acetate, make up to the mark, and shake to obtain the solution.
[0031] (3) Undemulsified sample solution: Take 0.5 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 10 mL volumetric flask. Add n-hexane to dilute and adjust the volume to the mark. Shake well and extract. After standing for 10 min, take the supernatant.
[0032] (4) Take 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution and inject them into a gas chromatograph for detection. Calculate the contents of the three main components by the external standard method. According to the encapsulation efficiency calculation formula, the encapsulation efficiencies of eucalyptol, limonene, and α-pinene are calculated to be 69.7%, 87.6%, and 88.5%, respectively.
[0033] Embedding rate = (the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution - the sum of the contents of eucalyptol, limonene and α-pinene in the undemulsified sample solution) × 100% ÷ the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution.
[0034] Example 2
[0035] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 100 mL volumetric flask, add ethyl acetate to dissolve, dilute and make up to the mark.
[0036] (2) Demulsified sample solution: Take 0.2 mL of milky white eucalyptus, lemon and pinene oral emulsion and place it in a 10 mL volumetric flask, add 1 mL of isopropanol, and gently shake to obtain a clear and transparent solution. Dilute with ethyl acetate, make up to the mark, and shake to obtain the solution.
[0037] (3) Undemulsified sample solution: Take 0.2 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 10 mL volumetric flask. Add n-hexane to dilute and adjust the volume to the mark. Shake well and extract. After standing for 10 min, take the supernatant.
[0038] 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution was injected into a gas chromatograph for detection. The contents of the three main components were calculated by the external standard method, and according to the encapsulation rate calculation formula, the encapsulation rates of eucalyptol, limonene, and α-pinene were calculated to be 67.3%, 86.7%, and 88.5%, respectively.
[0039] Example 3
[0040] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 100 mL volumetric flask, add ethyl acetate to dissolve, dilute and make up to the mark.
[0041] (2) Demulsified sample solution: Take 0.5 mL of the milky white eucalyptus, lemon and pinene oral emulsion and place it in a 10 mL volumetric flask, add 4 mL of isopropanol, and gently shake to obtain a clear and transparent solution. Dilute with ethyl acetate, make up to the mark, and shake to obtain the solution.
[0042] (3) Undemulsified sample solution: Take 0.5 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 10 mL volumetric flask. Add n-hexane to dilute and adjust the volume to the mark. Shake well and extract. After standing for 10 min, take the supernatant.
[0043] 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution was injected into a gas chromatograph for detection. The contents of the three main components were calculated by the external standard method, and according to the encapsulation rate calculation formula, the encapsulation rates of eucalyptol, limonene, and α-pinene were calculated to be 67.5%, 87.8%, and 88.3%, respectively.
[0044] Example 4
[0045] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 100 mL volumetric flask, add ethyl acetate to dissolve, dilute and make up to the mark.
[0046] (2) Demulsified sample solution: Take 0.5 mL of milky white eucalyptus, lemon and pinene oral emulsion and place it in a 10 mL volumetric flask. Add 3 mL of ethanol and shake gently to obtain a pale white milky solution. Dilute with ethyl acetate and make up to the mark. Shake well to obtain the solution.
[0047] (3) Undemulsified sample solution: Take 0.5 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 10 mL volumetric flask. Add n-hexane to dilute and adjust the volume to the mark. Shake well and extract. After standing for 10 min, take the supernatant.
[0048] 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution was injected into a gas chromatograph for detection. The contents of the three main components were calculated by the external standard method, and according to the encapsulation rate calculation formula, the encapsulation rates of eucalyptol, limonene, and α-pinene were calculated to be 12.9%, 1.7%, and 3.9%, respectively.
[0049] Example 5
[0050] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 100 mL volumetric flask, add ethyl acetate to dissolve, dilute and make up to the mark.
[0051] (2) Demulsified sample solution: Take 0.2 mL of milky white eucalyptus, lemon and pinene oral emulsion and place it in a 10 mL volumetric flask, add 1 mL of isopropanol, and gently shake to obtain a clear and transparent solution. Dilute with ethyl acetate, make up to the mark, and shake to obtain the solution.
[0052] (3) Undemulsified sample solution: Take 0.2 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 10 mL volumetric flask, add cyclohexane to dilute and adjust the volume to the mark, shake well, extract, let stand for 10 min, and take the supernatant.
[0053] 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution was injected into a gas chromatograph for detection. The contents of the three main components were calculated by the external standard method, and according to the encapsulation rate calculation formula, the encapsulation rates of eucalyptol, limonene, and α-pinene were calculated to be 68.1%, 86.7%, and 88.2%, respectively.
[0054] Comparative Example 1
[0055] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 50 mL volumetric flask, add n-hexane to dissolve, dilute and make up to the mark.
[0056] (2) Demulsified sample solution: Take 10 mL of the milky white eucalyptus citronella oral emulsion and place it in a 20 mL sample bottle, add 5 mL of isopropanol, shake well, and ultrasonicate for 20 minutes to obtain a turbid suspension solution. After centrifugation at 12,000 rpm for 10 minutes, transfer to a 25 mL separatory funnel and add 2 mL of n-hexane for three consecutive extractions. After collecting the supernatant, weigh it accurately. Take 300 mg of the supernatant, place it in a 10 mL volumetric flask, dilute it with n-hexane, make up to the mark, and shake well to obtain the solution.
[0057] (3) Undemulsified sample solution: Take 10 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 100 mL volumetric flask, add n-hexane to dilute and adjust the volume to the mark, shake well, extract, let stand for 10 min, and take the supernatant.
[0058] (4) Take 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution and inject them into a gas chromatograph for detection. Calculate the contents of the three main components by the external standard method. According to the encapsulation rate calculation formula, the encapsulation rates of eucalyptol, limonene, and α-pinene are calculated to be 60.0%, 84.9%, and 86.2%, respectively.
[0059] In this comparative example, due to the small amount of isopropanol added, the demulsification is incomplete, resulting in a low encapsulation rate of eucalyptol, limonene and α-pinene. In addition, auxiliary ultrasound and centrifugation are required to achieve demulsification. In addition, since soybean oil is contained in the oral emulsion, and eucalyptol, limonene and α-pinene have good solubility in soybean oil, if the content of eucalyptol, limonene and α-pinene is to be accurately determined, the soybean oil needs to be completely dissolved. Since the isopropanol used is less, the water content in the whole system is relatively high, and it is difficult to completely dissolve the system with a solvent with a strong polarity or a polarity greater than isopropanol (such as methanol, ethanol, acetonitrile, etc.) to form a clear and transparent solution. Therefore, it is necessary to extract the main component with a weak polar solvent (such as n-hexane). In the step of collecting the extract, it is difficult to collect the supernatant completely and accurately determine it, so the detected eucalyptol, limonene and α-pinene content is not accurate enough. The whole detection process has many steps, complicated operation and long time.
[0060] Comparative Example 2
[0061] (1) Reference solution: Accurately weigh 50 mg of the working reference substance eucalyptol, 35 mg of limonene, and 12 mg of α-pinene, place them in the same 100 mL volumetric flask, add n-hexane to dissolve, dilute and make up to the mark.
[0062] (2) Demulsified sample solution: Take 1 mL of the milky white eucalyptus citronella oral emulsion and place it in a 15 mL centrifuge tube, accurately weigh it, add 10 mL of acetonitrile, shake it well, and oscillate it horizontally at 150 rpm for 30 min in a constant temperature water bath oscillator. Then centrifuge it at 2500 rpm for 20 min, transfer it to a 50 mL volumetric flask, add n-hexane to the mark, shake it well, and let it stand. Take the supernatant for detection.
[0063] (3) Undemulsified sample solution: Take 1 mL of the milky white eucalyptus, lemon and pinine oral emulsion and place it in a 5 mL centrifuge tube. Centrifuge it at 2500 rpm for 20 min. Then transfer it to a 50 mL volumetric flask. Add n-hexane to dilute and adjust the volume to the mark. Shake well, extract, let it stand for 10 min, and take the supernatant.
[0064] (4) Take 1 μL of each of the reference solution, demulsified sample solution, and undemulsified sample solution and inject them into a gas chromatograph for detection. Calculate the contents of the three main components by the external standard method. According to the encapsulation efficiency calculation formula, the encapsulation efficiencies of eucalyptol, limonene, and α-pinene are calculated to be 14.1%, 60.4%, and 64.6%, respectively.
[0065] In this comparative example, acetonitrile was used for demulsification, but the demulsification effect was poor, resulting in low encapsulation rates of eucalyptol, limonene, and α-pinene. In addition, an auxiliary oscillator was required for demulsification, and the entire detection process had many steps, complicated operations, and took a long time.
[0066] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.
[0067] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.
Claims
1. A method for detecting the embedding rate of eucalyptol, limonene and α-pinene in an oral emulsion containing eucalyptol, limonene and α-pinene, characterized in that: include: The oral emulsion containing eucalyptol, limonene and α-pinene is mixed with isopropyl alcohol for demulsification to obtain a demulsified liquid, wherein the volume ratio of the oral emulsion to the isopropyl alcohol is 1:(4-8); Diluting the demulsified liquid with a first diluent to obtain a demulsified sample solution; The oral emulsion is mixed with a second diluent, and the mixture is allowed to stand, and the supernatant is collected to obtain an unbroken emulsion sample solution; Diluting eucalyptol, limonene, α-pinene and a third diluent to obtain a reference solution; Determine the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution respectively; Determining the embedding rates of eucalyptol, limonene and α-pinene in the oral emulsion based on the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution; The first diluent is selected from ethyl acetate; The second diluent is selected from n-hexane or cyclohexane.
2. The method according to claim 1, characterized in that The third diluent is selected from ethyl acetate or n-hexane.
3. The method according to claim 1, characterized in that The contents of eucalyptol, limonene and α-pinene in the demulsified sample solution, the undemulsified sample solution and the reference solution are detected by gas chromatography.
4. The method according to claim 1, characterized in that The embedding rates of eucalyptol, limonene and α-pinene in the oral emulsion were calculated based on the following formula: Embedding rate = (the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution - the sum of the contents of eucalyptol, limonene and α-pinene in the undemulsified sample solution) × 100% ÷ (the sum of the contents of eucalyptol, limonene and α-pinene in the demulsified sample solution).
5. The method according to claim 1, characterized in that The particle size of the oral emulsion is nanometer level.
6. A method for detecting the quality of an oral emulsion containing eucalyptol, limonene and α-pinene, characterized in that: include: Determining the embedding rate of the oral emulsion according to the method according to any one of claims 1 to 5; If the embedding rate of the oral emulsion is less than the threshold value, it indicates that the quality of the oral emulsion does not meet the standard; If the embedding rate of the oral emulsion is greater than or equal to the threshold, it indicates that the quality of the oral emulsion meets the standard.
Citation Information
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