Toothpaste containing ipomoea bambusae extract
By adding plum tree branch and leaf extract to the toothpaste, using its natural antibacterial and anti-inflammatory effects, the problems of environmental pollution and high production costs caused by the use of chemical synthetic agents in existing toothpaste are solved, and good cleaning, antibacterial and anti-inflammatory effects are achieved.
Patent Information
- Application Number
- CN202510305692.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-14
- Publication Date
- 2025-06-13
AI Technical Summary
Chemical synthetic agents such as copper chlorophenol and tranexamic acid are often used in existing toothpastes. Although they have excellent antibacterial or anti-inflammatory effects, precious metal catalysts and highly toxic neutralizers may be used during their production process, resulting in high production costs and environmental pollution.
Develop a toothpaste containing plum tree extract. By adding plum tree branch and leaf extract to the toothpaste, it uses its natural antibacterial and anti-inflammatory effects to replace some chemical synthetic agents.
This toothpaste not only has good cleaning and antibacterial effects, but also significantly improves the anti-inflammatory effect through plum tree extract, reduces environmental pollution, and has relatively low production costs.
Abstract
Description
Technical Field
[0001] The present invention relates to the technical fields of natural product chemistry and daily chemical product preparation, and particularly relates to a toothpaste containing extracts of Dryobalanops aromatica Background Art
[0002] Oral health is an important part of overall health, and good oral hygiene habits can effectively prevent various diseases. As a basic product for daily oral care, toothpaste plays a key role in cleaning teeth, removing food residues, and preventing dental caries. In recent years, with the increasing attention to oral health, the demand for antibacterial or anti-inflammatory functions has also been growing. Therefore, developing toothpaste with antibacterial or anti-inflammatory effects has important application value.
[0003] Two chemical synthetic drugs, sodium copper chlorophyllin and tranexamic acid, have excellent antibacterial or anti-inflammatory effects. Currently, some commercially available antibacterial drug toothpastes and anti-inflammatory drug ointments often add these two ingredients. However, chemical synthetic drugs often bring some side effects, or require the use of precious metal catalysts and highly toxic neutralizing agents in the synthesis process, which not only increases production costs but also harms the environment.
[0004] In summary, developing a toothpaste with natural antibacterial or anti-inflammatory effects has broad application prospects. Summary of the Invention
[0005] In order to overcome at least one of the technical problems existing in the prior art, the present invention first provides a toothpaste containing extracts of Dryobalanops aromatica.
[0006] The technical solution of the present invention is as follows:
[0007] The present invention first provides a toothpaste containing extracts of Dryobalanops aromatica, which comprises the following raw material components: aluminum hydroxide, glycerol, polyethylene glycol - 400, sodium lauryl sulfate, sodium lauroyl sarcosinate, sodium saccharin, sodium benzoate, sodium carboxymethyl cellulose, hydroxypropyl cellulose, extracts of Dryobalanops aromatica branches and leaves, and water.
[0008] Preferably, the toothpaste containing extracts of Dryobalanops aromatica comprises the following raw material components in weight percentages:
[0009] aluminum hydroxide 50 - 65%; glycerol 8 - 15%; polyethylene glycol - 400 8 - 15%; sodium lauryl sulfate 0.6 - 1.2%; sodium lauroyl sarcosinate 0 - 0.6%; sodium saccharin 0.1 - 0.3%; sodium benzoate 0.05 - 0.15%; sodium carboxymethyl cellulose 1.5 - 3%; hydroxypropyl cellulose 0 - 1.5%; extracts of Dryobalanops aromatica branches and leaves 0.1 - 1%; and the balance is water.
[0010] The inventors found in their research that adding the extract of the leaves and branches of Dryobalanops aromatica to toothpaste can make the prepared toothpaste have an anti-inflammatory effect.
[0011] Further preferably, the toothpaste containing the extract of Dryobalanops aromatica comprises the following raw material components in percentage by weight:
[0012] Aluminum hydroxide 50 - 60%; glycerol 10 - 15%; polyethylene glycol - 400 10 - 15%; sodium lauryl sulfate 0.6 - 1.2%; sodium saccharin 0.1 - 0.3%; sodium benzoate 0.05 - 0.1%; sodium carboxymethyl cellulose 1.5 - 2.5%; extract of the leaves and branches of Dryobalanops aromatica 0.1 - 0.5%; the balance is water.
[0013] Most preferably, the toothpaste containing the extract of Dryobalanops aromatica comprises the following raw material components in percentage by weight:
[0014] Aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of the leaves and branches of Dryobalanops aromatica 0.1 - 0.5%; the balance is water.
[0015] Preferably, the water is deionized water.
[0016] Preferably, the extract of the leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0017] Take the leaves and branches of Dryobalanops aromatica and add them to a steam distillation device, then add water, heat to boiling and carry out steam distillation for 1 - 2 h. After the distillation is completed, obtain the essential oil of the leaves and branches of Dryobalanops aromatica, and take the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of the leaves and branches of Dryobalanops aromatica.
[0018] Preferably, the weight ratio of the leaves and branches of Dryobalanops aromatica to water is 1:2 - 5.
[0019] Most preferably, the weight ratio of the leaves and branches of Dryobalanops aromatica to water is 1:3.
[0020] Preferably, the preparation method of the extract of the leaves and branches of Dryobalanops aromatica further comprises the following steps:
[0021] After the distillation is completed, take the residue of the leaves and branches of Dryobalanops aromatica, then carry out heating reflux extraction with an organic solvent. After the extraction is completed, take the extract, concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica;
[0022] Take the organic solvent extract of the leaves and branches of Dryobalanops aromatica and mix it with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica.
[0023] In further research, the inventor found that in toothpaste, adding the extract of Cinnamomum camphora leaves and twigs obtained by mixing the organic solvent extract of Cinnamomum camphora leaves and twigs with the essential oil of Cinnamomum camphora leaves can significantly improve the anti-inflammatory effect of toothpaste compared to adding only the essential oil of Cinnamomum camphora leaves.
[0024] Preferably, the organic solvent consists of cyclohexane and acetone.
[0025] In further research, the inventor found that the selection of the extraction solvent for the organic solvent extract of Cinnamomum camphora leaves and twigs is crucial; in toothpaste, only by adding the extract of Cinnamomum camphora leaves and twigs obtained by mixing the organic solvent extract of Cinnamomum camphora leaves and twigs extracted with an organic solvent consisting of cyclohexane and acetone with the essential oil of Cinnamomum camphora leaves can the anti-inflammatory effect of toothpaste be significantly improved compared to adding only the essential oil of Cinnamomum camphora leaves; however, adding the extract of Cinnamomum camphora leaves and twigs obtained by mixing the organic solvent extract of Cinnamomum camphora leaves and twigs extracted with a single cyclohexane or acetone or other organic solvent with the essential oil of Cinnamomum camphora leaves cannot significantly improve the anti-inflammatory effect of toothpaste.
[0026] More preferably, the volume ratio of cyclohexane to acetone is 100:50 - 60.
[0027] Most preferably, the volume ratio of cyclohexane to acetone is 100:55.
[0028] Preferably, the dosage ratio of the residue of Cinnamomum camphora leaves and twigs to the organic solvent is 1 kg:5 - 10 L.
[0029] Most preferably, the dosage ratio of the residue of Cinnamomum camphora leaves and twigs to the organic solvent is 1 kg:8 L.
[0030] Preferably, the weight ratio of the organic solvent extract of Cinnamomum camphora leaves and twigs to the essential oil of Cinnamomum camphora leaves is 1 - 3:1 - 3.
[0031] Most preferably, the weight ratio of the organic solvent extract of Cinnamomum camphora leaves and twigs to the essential oil of Cinnamomum camphora leaves is 1:1.
[0032] Preferably, the preparation method of the extract of Cinnamomum camphora leaves and twigs further comprises the following steps:
[0033] After the distillation is completed, take the residue of Cinnamomum camphora leaves and twigs, then carry out heating and reflux extraction with an organic solvent, take the extract after the extraction is completed, and concentrate and dry the extract to obtain the organic solvent extract of Cinnamomum camphora leaves and twigs;
[0034] The organic solvent extract of the leaves and branches of Dryobalanops aromatica is loaded onto a silica gel column. First, it is eluted and defatted with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:5 - 10 and a volume of 3 - 6 times the column volume. Then, it is further eluted with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:20 - 25 and a volume of 3 - 6 times the column volume. The eluate eluted with the mixed solvent composed of chloroform and methanol with a volume ratio of 100:20 - 25 is collected, concentrated and dried to obtain the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica.
[0035] The Dryobalanops aromatica extract is obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica.
[0036] Most preferably, the organic solvent extract of the leaves and branches of Dryobalanops aromatica is loaded onto a silica gel column. First, it is eluted and defatted with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:7 and a volume of 3 - 6 times the column volume. Then, it is further eluted with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:22 and a volume of 3 - 6 times the column volume. The eluate eluted with the mixed solvent composed of chloroform and methanol with a volume ratio of 100:22 is collected, concentrated and dried to obtain the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica.
[0037] The inventors further found in their research that in toothpaste, adding the Dryobalanops aromatica extract obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica prepared under the above silica gel column elution conditions with the essential oil of the leaves and branches of Dryobalanops aromatica can further significantly improve the anti - inflammatory effect of the toothpaste compared to adding the Dryobalanops aromatica extract obtained by mixing the organic solvent extract of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica.
[0038] The inventors also found in their further research that the silica gel column elution conditions of the present invention are very crucial. In toothpaste, only by adding the Dryobalanops aromatica extract obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica eluted under the silica gel column elution conditions of the present invention with the essential oil of the leaves and branches of Dryobalanops aromatica can the anti - inflammatory effect of the toothpaste be further significantly improved. However, adding the Dryobalanops aromatica extract obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica eluted under other silica gel column elution conditions with the essential oil of the leaves and branches of Dryobalanops aromatica cannot further significantly improve the anti - inflammatory effect of the toothpaste.
[0039] Beneficial effects: The present invention provides a toothpaste containing Dryobalanops aromatica extract with a completely new composition. The toothpaste uses aluminum hydroxide, which has good cleaning and antibacterial effects, as an abrasive, so that the prepared toothpaste has good cleaning and antibacterial effects. In addition, by adding the extract of the leaves and branches of Dryobalanops aromatica to the toothpaste, the prepared toothpaste has an anti - inflammatory effect, which has important application value. Detailed implementation mode
[0040] The following specific examples are used to further explain the present invention, but the examples do not limit the present invention in any form.
[0041] Preparation of Toothpaste Containing Extract of Dryobalanops aromatica
[0042] Composition by weight percentage of raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of Dryobalanops aromatica branches and leaves 0.1%; the balance is deionized water;
[0043] The extract of Dryobalanops aromatica branches and leaves is prepared by the following method: Take the branches and leaves of Dryobalanops aromatica and add them to a steam distillation device, then add water with a weight 3 times that of the branches and leaves of Dryobalanops aromatica. After heating to boiling, carry out steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of Dryobalanops aromatica branches and leaves. Take the essential oil of Dryobalanops aromatica branches and leaves to obtain the extract of Dryobalanops aromatica branches and leaves.
[0044] Preparation method of toothpaste containing extract of Dryobalanops aromatica: Mix the raw materials such as aluminum hydroxide, glycerol, polyethylene glycol - 400, sodium lauryl sulfate, sodium saccharin, sodium benzoate, sodium carboxymethyl cellulose, extract of Dryobalanops aromatica branches and leaves and deionized water evenly to obtain the toothpaste containing extract of Dryobalanops aromatica.
[0045] Preparation of Toothpaste Containing Extract of Dryobalanops aromatica in Example 2
[0046] Composition by weight percentage of raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of Dryobalanops aromatica branches and leaves 0.1%; the balance is deionized water;
[0047] The extract of Dryobalanops aromatica branches and leaves is prepared by the following method:
[0048] (1) Take the branches and leaves of Dryobalanops aromatica and add them to a steam distillation device, then add water with a weight 3 times that of the branches and leaves of Dryobalanops aromatica. After heating to boiling, carry out steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of Dryobalanops aromatica branches and leaves;
[0049] (2) After the distillation ends, take the residue of Dryobalanops aromatica branches and leaves, then heat it to boiling with an organic solvent and carry out heating and reflux extraction for 1.5 h. After the extraction ends, take the extract, and concentrate and dry the extract to obtain the organic solvent extract of Dryobalanops aromatica branches and leaves; among them, the dosage ratio of the residue of Dryobalanops aromatica branches and leaves to the organic solvent is 1 kg:8 L; the organic solvent consists of cyclohexane and acetone with a volume ratio of 100:55;
[0050] (3) Mix the organic solvent extract of Dryobalanops aromatica branches and leaves and the essential oil of Dryobalanops aromatica branches and leaves to obtain the extract of Dryobalanops aromatica; among them, the weight ratio of the organic solvent extract of Dryobalanops aromatica branches and leaves to the essential oil of Dryobalanops aromatica branches and leaves is 1:1.
[0051] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica trees is the same as that in Example 1.
[0052] Preparation of the toothpaste containing the extract of Dryobalanops aromatica trees in Example 3
[0053] The weight percentage composition of raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of Dryobalanops aromatica tree branches and leaves 0.1%; the balance is deionized water;
[0054] The extract of Dryobalanops aromatica tree branches and leaves is prepared by the following method:
[0055] (1) Take the branches and leaves of Dryobalanops aromatica trees and add them to a steam distillation device, then add water with a weight three times that of the branches and leaves of Dryobalanops aromatica trees. After heating to boiling, carry out steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of Dryobalanops aromatica tree branches and leaves;
[0056] (2) After the distillation ends, take the residue of Dryobalanops aromatica tree branches and leaves, then heat it to boiling with an organic solvent and carry out heating and reflux extraction for 1.5 h. After the extraction ends, take the extract. After concentrating and drying the extract, obtain the organic solvent extract of Dryobalanops aromatica tree branches and leaves; among them, the dosage ratio of the residue of Dryobalanops aromatica tree branches and leaves to the organic solvent is 1 kg:8 L; the organic solvent is composed of cyclohexane and acetone with a volume ratio of 100:55;
[0057] (3) Load the organic solvent extract of Dryobalanops aromatica tree branches and leaves onto a silica gel column (the packing in the silica gel column is silica gel with a mesh size of 200 - 300, and the weight dosage of the packing is 30 times that of the organic solvent extract of Dryobalanops aromatica tree branches and leaves). First, elute and remove impurities with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:7 and a volume five times that of the column volume; then elute with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:22 and a volume five times that of the column volume. Collect the eluate eluted by the mixed solvent composed of chloroform and methanol with a volume ratio of 100:22. After concentrating and drying, obtain the elution part of the silica gel column of Dryobalanops aromatica tree branches and leaves;
[0058] (3) Mix the elution part of the silica gel column of Dryobalanops aromatica tree branches and leaves with the essential oil of Dryobalanops aromatica tree branches and leaves to obtain the extract of Dryobalanops aromatica trees; among them, the weight ratio of the elution part of the silica gel column of Dryobalanops aromatica tree branches and leaves to the essential oil of Dryobalanops aromatica tree branches and leaves is 1:1.
[0059] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica trees is the same as that in Example 1.
[0060] Preparation of the toothpaste containing the extract of Dryobalanops aromatica trees in Comparative Example 1
[0061] Raw material weight percentage composition: aluminum hydroxide 60%; glycerin 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of leaves and branches of Dryobalanops aromatica 0.1%; the balance is deionized water;
[0062] The extract of leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0063] (1) Take the leaves and branches of Dryobalanops aromatica and add them to a steam distillation device. Then add water with a weight three times that of the leaves and branches of Dryobalanops aromatica. Heat to boiling and carry out steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of the leaves and branches of Dryobalanops aromatica;
[0064] (2) After the distillation ends, take the residue of the leaves and branches of Dryobalanops aromatica. Then heat it to boiling with an organic solvent and carry out heating reflux extraction for 1.5 h. After the extraction ends, take the extract. Concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica; among them, the dosage ratio of the residue of the leaves and branches of Dryobalanops aromatica to the organic solvent is 1 kg:8 L; the organic solvent is ethanol with a volume fraction of 95%;
[0065] (3) Take the organic solvent extract of the leaves and branches of Dryobalanops aromatica and mix it with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica; among them, the weight ratio of the organic solvent extract of the leaves and branches of Dryobalanops aromatica to the essential oil of the leaves and branches of Dryobalanops aromatica is 1:1.
[0066] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica is the same as that in Example 1.
[0067] Preparation of the toothpaste containing the extract of Dryobalanops aromatica in Comparative Example 2
[0068] Raw material weight percentage composition: aluminum hydroxide 60%; glycerin 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of leaves and branches of Dryobalanops aromatica 0.1%; the balance is deionized water;
[0069] The extract of leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0070] (1) Take the leaves and branches of Dryobalanops aromatica and add them to a steam distillation device. Then add water with a weight three times that of the leaves and branches of Dryobalanops aromatica. Heat to boiling and carry out steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of the leaves and branches of Dryobalanops aromatica;
[0071] (2) After the distillation ends, take the residue of the leaves and branches of Dryobalanops aromatica. Then heat it to boiling with an organic solvent and carry out heating reflux extraction for 1.5 h. After the extraction ends, take the extract. Concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica; among them, the dosage ratio of the residue of the leaves and branches of Dryobalanops aromatica to the organic solvent is 1 kg:8 L; the organic solvent is cyclohexane;
[0072] (3) Mix the organic solvent extract of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica; wherein, the weight ratio of the organic solvent extract of the leaves and branches of Dryobalanops aromatica to the essential oil of the leaves and branches of Dryobalanops aromatica is 1:1.
[0073] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica is the same as that in Example 1.
[0074] Preparation of Toothpaste Containing Extract of Dryobalanops aromatica in Comparative Example 3
[0075] The weight percentage composition of the raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; saccharin sodium 0.2%; sodium benzoate 0.1%; sodium carboxymethylcellulose 2.5%; extract of the leaves and branches of Dryobalanops aromatica 0.1%; the balance is deionized water;
[0076] The extract of the leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0077] (1) Take the leaves and branches of Dryobalanops aromatica and add them to a steam distillation device, then add water with a weight three times that of the leaves and branches of Dryobalanops aromatica, heat to boiling and carry out steam distillation for 1.5 h. After the distillation is completed, obtain the essential oil of the leaves and branches of Dryobalanops aromatica;
[0078] (2) After the distillation is completed, take the residue of the leaves and branches of Dryobalanops aromatica, then heat it to boiling with an organic solvent and carry out heating and reflux extraction for 1.5 h. After the extraction is completed, take the extract, concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica; wherein, the dosage ratio of the residue of the leaves and branches of Dryobalanops aromatica to the organic solvent is 1 kg:8 L; the organic solvent is acetone;
[0079] (3) Mix the organic solvent extract of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica; wherein, the weight ratio of the organic solvent extract of the leaves and branches of Dryobalanops aromatica to the essential oil of the leaves and branches of Dryobalanops aromatica is 1:1.
[0080] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica is the same as that in Example 1.
[0081] Preparation of Toothpaste Containing Extract of Dryobalanops aromatica in Comparative Example 4
[0082] The weight percentage composition of the raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; saccharin sodium 0.2%; sodium benzoate 0.1%; sodium carboxymethylcellulose 2.5%; extract of the leaves and branches of Dryobalanops aromatica 0.1%; the balance is deionized water;
[0083] The extract of the leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0084] (1) Add the leaves and branches of Dryobalanops aromatica to a steam distillation apparatus, then add water with a weight three times that of the leaves and branches of Dryobalanops aromatica. Heat to boiling and perform steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of the leaves and branches of Dryobalanops aromatica;
[0085] (2) After the distillation ends, take the residue of the leaves and branches of Dryobalanops aromatica, then heat to boiling with an organic solvent and perform heating and reflux extraction for 1.5 h. After the extraction ends, take the extract, concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica; wherein, the dosage ratio of the residue of the leaves and branches of Dryobalanops aromatica to the organic solvent is 1 kg:8 L; the organic solvent is composed of cyclohexane and acetone with a volume ratio of 100:55;
[0086] (3) Load the organic solvent extract of the leaves and branches of Dryobalanops aromatica onto a silica gel column (the packing in the silica gel column is silica gel with a mesh size of 200 - 300, and the weight dosage of the packing is 30 times that of the organic solvent extract of the leaves and branches of Dryobalanops aromatica). First, elute and remove impurities with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:20 and a volume five times that of the column volume; then elute with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:40 and a volume five times that of the column volume. Collect the eluate eluted by the mixed solvent composed of chloroform and methanol with a volume ratio of 100:40, concentrate and dry it to obtain the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica;
[0087] (3) Mix the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica tree; wherein, the weight ratio of the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica to the essential oil of the leaves and branches of Dryobalanops aromatica is 1:1.
[0088] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica tree is the same as that in Example 1.
[0089] Preparation of the toothpaste containing the extract of Dryobalanops aromatica tree in Comparative Example 5
[0090] Composition by weight percentage of raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; sodium saccharin 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; extract of the leaves and branches of Dryobalanops aromatica 0.1%; the balance is deionized water;
[0091] The extract of the leaves and branches of Dryobalanops aromatica is prepared by the following method:
[0092] (1) Add the leaves and branches of Dryobalanops aromatica to a steam distillation apparatus, then add water with a weight three times that of the leaves and branches of Dryobalanops aromatica. Heat to boiling and perform steam distillation for 1.5 h. After the distillation ends, obtain the essential oil of the leaves and branches of Dryobalanops aromatica;
[0093] (2) After the distillation is completed, take the residue of the leaves and branches of Dryobalanops aromatica. Then, heat it with an organic solvent to boiling and carry out heating reflux extraction for 1.5 h. After the extraction is completed, take the extract. Concentrate and dry the extract to obtain the organic solvent extract of the leaves and branches of Dryobalanops aromatica. Among them, the dosage ratio of the residue of the leaves and branches of Dryobalanops aromatica to the organic solvent is 1 kg:8 L. The organic solvent is composed of cyclohexane and acetone with a volume ratio of 100:55.
[0094] (3) Load the organic solvent extract of the leaves and branches of Dryobalanops aromatica onto a silica gel column (the packing in the silica gel column is silica gel with a mesh size of 200 - 300, and the weight dosage of the packing is 30 times that of the organic solvent extract of the leaves and branches of Dryobalanops aromatica). First, elute and remove impurities with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:30 and a volume of 5 times the column volume. Then, elute with a mixed solvent composed of chloroform and methanol with a volume ratio of 100:50 and a volume of 5 times the column volume. Collect the eluate eluted by the mixed solvent composed of chloroform and methanol with a volume ratio of 100:50. Concentrate and dry it to obtain the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica.
[0095] (3) Mix the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica with the essential oil of the leaves and branches of Dryobalanops aromatica to obtain the extract of Dryobalanops aromatica. Among them, the weight ratio of the elution part of the silica gel column of the leaves and branches of Dryobalanops aromatica to the essential oil of the leaves and branches of Dryobalanops aromatica is 1:1.
[0096] The preparation method of the toothpaste containing the extract of Dryobalanops aromatica is the same as that in Example 1.
[0097] Preparation of the toothpaste containing tranexamic acid in Comparative Example 6
[0098] The weight percentage composition of the raw materials: aluminum hydroxide 60%; glycerol 10%; polyethylene glycol - 400 10%; sodium lauryl sulfate 0.7%; saccharin sodium 0.2%; sodium benzoate 0.1%; sodium carboxymethyl cellulose 2.5%; tranexamic acid 0.1%; the balance is deionized water.
[0099] Preparation method of the toothpaste containing the extract of Dryobalanops aromatica: Mix the raw materials such as aluminum hydroxide, glycerol, polyethylene glycol - 400, sodium lauryl sulfate, saccharin sodium, sodium benzoate, sodium carboxymethyl cellulose, tranexamic acid and deionized water evenly to obtain the toothpaste containing tranexamic acid.
[0100] Experimental Example
[0101] The periodontal tissue is mainly composed of cells and extracellular matrix. Human gingival fibroblasts (HGFs) are an important component of the periodontal tissue. Human gingival fibroblasts play an important role in the formation, regeneration, function implementation and repair of the periodontal tissue. Lipopolysaccharide (LPS) is one of the main virulence factors of periodontal pathogenic bacteria, which can induce a large number of inflammatory response mediators and cytokines in different types of cells, causing periodontal tissue damage. In this experiment, the regulatory effect of the test sample on the inflammatory response of LPS-induced human gingival fibroblasts was tested through the IL-6 signaling pathway, as one of the supports for products to relieve gum problems.
[0102] Human gingival fibroblasts were seeded in 96-well plates and cultured with DMEM medium containing LPS (200 ng / g) for 24 h, and then changed to DMEM medium containing the test sample (160 mg / g). After 24 h, the cell supernatant was collected and centrifuged. The supernatant was aspirated, and the IL-6 content in the cell culture supernatant was measured using an ELISA kit to obtain the effect of the test sample on the IL-6 content of human gingival fibroblasts; 3 replicate wells were set for each test sample, and the experiment was repeated 3 times. At the same time, a negative control group without the test sample was tested according to the above method; the IL-6 inhibition rate was calculated; IL-6 inhibition rate (%) = [1 - (average IL-6 content of the test sample / average IL-6 content of the negative control)] * 100%.
[0103] In addition, the antibacterial rate of the test sample against Staphylococcus aureus was tested according to the method in the standard of "WS / T 650 - 2019 5.1.2".
[0104] The test samples were toothpastes containing extracts of Dryobalanops aromatica Gaertn. f. prepared in Examples 1 - 3 and Comparative Examples 1 - 5, and a toothpaste containing tranexamic acid prepared in Comparative Example 6; the test results are shown in Table 1.
[0105] Table 1. Anti-inflammatory experimental results of the toothpastes of the present invention
[0106] IL-6 inhibition rate Bacteriostatic rate Toothpaste containing borneol tree extract prepared in Example 1 12.38％ 96.2％ Toothpaste containing borneol tree extract prepared in Example 2 20.49％ 99.8％ Toothpaste containing borneol tree extract prepared in Example 3 33.75％ 97.3％ Toothpaste containing borneol tree extract prepared in Comparative Example 1 12.79％ 96.8％ Toothpaste containing borneol tree extract prepared in Comparative Example 2 16.82％ 94.5％ Toothpaste containing borneol tree extract prepared in Comparative Example 3 15.75％ 99.6％ Toothpaste containing borneol tree extract prepared in Comparative Example 4 23.18％ 96.4％ Toothpaste containing borneol tree extract prepared in Comparative Example 5 21.72％ 97.9％ Toothpaste containing tranexamic acid prepared in Comparative Example 6 27.69％ 94.3％
[0107] It can be seen from the experimental results in Table 1 that the antibacterial rates of the toothpastes containing extracts of Dryobalanops aromatica Gaertn. f. prepared in the present invention are all above 90%; this shows that the toothpastes containing extracts of Dryobalanops aromatica Gaertn. f. prepared in the present invention have good antibacterial effects.
[0108] It can be seen from the experimental results in Table 1 that the IL-6 inhibition rate of the toothpaste containing extracts of Dryobalanops aromatica Gaertn. f. prepared in Example 1 is 12.38%; this shows that adding the essential oil of the leaves and branches of Dryobalanops aromatica Gaertn. f. to the toothpaste can make the prepared toothpaste have an anti-inflammatory effect.
[0109] As can be seen from the experimental results in Table 1, the IL-6 inhibition rate of the toothpaste containing the extract of Dryobalanops aromatica Gagnep. prepared in Example 2 is much higher than that in Example 1. This indicates that in toothpaste, the extract of Dryobalanops aromatica Gagnep. obtained by mixing the organic solvent extract of the leaves and branches of Dryobalanops aromatica Gagnep. with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. can significantly enhance the anti-inflammatory effect of the toothpaste compared to simply adding the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep.
[0110] As can be seen from the experimental results in Table 1, the increase in the IL-6 inhibition rate of the toothpaste containing the extract of Dryobalanops aromatica Gagnep. prepared in Comparative Examples 1-3 is not significant compared to that in Example 1. This indicates that the selection of the extraction solvent for the organic solvent extract of the leaves and branches of Dryobalanops aromatica Gagnep. is crucial. In toothpaste, only by adding the extract of Dryobalanops aromatica Gagnep. obtained by mixing the organic solvent extract of the leaves and branches of Dryobalanops aromatica Gagnep. extracted with an organic solvent composed of cyclohexane and acetone with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. can the anti-inflammatory effect of the toothpaste be significantly enhanced compared to simply adding the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. However, adding the extract of Dryobalanops aromatica Gagnep. obtained by mixing the organic solvent extract of the leaves and branches of Dryobalanops aromatica Gagnep. extracted with a single cyclohexane or acetone or other organic solvents with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. cannot significantly enhance the anti-inflammatory effect of the toothpaste compared to simply adding the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep.
[0111] As can be seen from the experimental results in Table 1, the IL-6 inhibition rate of the toothpaste containing the extract of Dryobalanops aromatica Gagnep. prepared in Example 3 reaches 33.75%, which is further much higher than that in Example 2. At the same time, it is also significantly higher than that of the toothpaste containing tranexamic acid prepared in Comparative Example 6, showing excellent anti-inflammatory effects. This indicates that in toothpaste, adding the extract of Dryobalanops aromatica Gagnep. obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica Gagnep. prepared under the silica gel column elution conditions of the present invention with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. can further significantly enhance the anti-inflammatory effect of the toothpaste compared to adding the extract of Dryobalanops aromatica Gagnep. obtained by mixing the organic solvent extract of the leaves and branches of Dryobalanops aromatica Gagnep. with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep., making the prepared toothpaste have excellent anti-inflammatory effects.
[0112] As can be seen from the experimental results in Table 1, the increase in the IL-6 inhibition rate of the toothpaste containing the extract of Dryobalanops aromatica Gagnep. prepared in Comparative Examples 4 and 5 is not significant compared to that in Example 2. This indicates that the silica gel column elution conditions of the present invention are crucial. In toothpaste, it is necessary to add the extract of Dryobalanops aromatica Gagnep. obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica Gagnep. eluted under the silica gel column elution conditions of the present invention with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. to further significantly enhance the anti-inflammatory effect of the toothpaste. However, adding the extract of Dryobalanops aromatica Gagnep. obtained by mixing the silica gel column elution fraction of the leaves and branches of Dryobalanops aromatica Gagnep. eluted under other silica gel column elution conditions with the essential oil of the leaves and branches of Dryobalanops aromatica Gagnep. cannot further significantly enhance the anti-inflammatory effect of the toothpaste.
Claims
1. A toothpaste containing a Prunus armeniaca extract, characterized in that: The invention comprises the following raw materials: aluminum hydroxide, glycerin, polyethylene glycol-400, sodium lauryl sulfate, sodium lauryl sarcosinate, sodium saccharin, sodium benzoate, sodium carboxymethyl cellulose, hydroxypropyl cellulose, extract of twigs and leaves of plum blossoms, and water.
2. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that The raw material components include the following weight percentages: Aluminum hydroxide 50-65%; glycerol 8-15%; polyethylene glycol-400 8-15%; sodium lauryl sulfate 0.6-1.2%; sodium lauryl sarcosinate 0-0.6%; sodium saccharin 0.1-0.3%; sodium benzoate 0.05-0.15%; sodium carboxymethyl cellulose 1.5-3%; hydroxypropyl cellulose 0-1.5%; extract of Prunus mume branches and leaves 0.1-1%; the balance is water.
3. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that: The raw material components include the following weight percentages: Aluminum hydroxide 50-60%; glycerol 10-15%; polyethylene glycol-400 10-15%; sodium lauryl sulfate 0.6-1.2%; sodium saccharin 0.1-0.3%; sodium benzoate 0.05-0.1%; sodium carboxymethyl cellulose 1.5-2.5%; extract of Prunus mume branches and leaves 0.1-0.5%; the balance is water.
4. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that The extract of Prunus mume branches and leaves is prepared by the following method: Take the branches and leaves of the plum tree and add them into a steam distillation device, then add water, heat to boiling and perform steam distillation for 1 to 2 hours, and obtain the essential oil of the branches and leaves of the plum tree after the distillation. Take the essential oil of the branches and leaves of the plum tree to obtain the said branches and leaves of the plum tree extract.
5. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that: The preparation method of the extract of Prunus mume branches and leaves further comprises the following steps: After the distillation is completed, the residue of the branches and leaves of the plum blossoms is taken, and then heated and refluxed with an organic solvent for extraction. After the extraction is completed, the extract is taken, and the extract is concentrated and dried to obtain the organic solvent extract of the branches and leaves of the plum blossoms; The Prunus mume tree extract is obtained by mixing the organic solvent extract of the Prunus mume tree branches and leaves with the essential oil of the Prunus mume tree branches and leaves.
6. The toothpaste containing the extract of Prunus armeniaca according to claim 5, characterized in that The organic solvent consists of cyclohexane and acetone.
7. The toothpaste containing the extract of Prunus armeniaca according to claim 6, characterized in that The volume ratio of cyclohexane to acetone is 100:50-60.
8. The toothpaste containing the extract of Prunus armeniaca according to claim 6, characterized in that: The weight ratio of the organic solvent extract of the branches and leaves of Prunus mume to the essential oil of the branches and leaves of Prunus mume is 1-3:1-3.
9. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that: The toothpaste is a toothpaste with antibacterial effect.
10. The toothpaste containing the extract of Prunus armeniaca according to claim 1, characterized in that: The toothpaste is a toothpaste with anti-inflammatory effect.