A bacteriostatic soap containing Catalpa bungei var. aurea and its preparation method

Abstract

A Catalpa bungei antibacterial composition, the Catalpa bungei antibacterial composition comprising a mixture formed by catalpol and 4,9-dihydroxy-α-lapachone. The mass fraction of catalpol is 50-65%, and the mass fraction of 4,9-dihydroxy-α-lapachone is 20-30%. The steps for separation and extraction using Catalpa bungei as a raw material are as follows: The powder of the heartwood part of Catalpa bungei is placed in dichloromethane solvent for cold soaking at room temperature, and the obtained extract is evaporated to dryness under reduced pressure to obtain a dark brown extract; the obtained dark brown extract is separated by silica gel column chromatography, eluted with a mixed solvent of dichloromethane and methanol, and then eluted with pure methanol after the elution is completed. The methanol eluate is collected and concentrated under reduced pressure to obtain the Catalpa bungei composition. The present invention not only has a decontamination function on human skin, but also has a good antibacterial effect, and can also enhance the market competitiveness.

Description

Technical Field

[0001] The present invention relates to the field of antibacterial skin care product formulations and their preparation methods, and in particular to a formulation and preparation method of an antibacterial soap containing a Catalpa bungei “Jinsi” composition. Background Art

[0002] Toilet soap is a daily chemical product we often use, and its main function is to remove dirt on the surface of the human skin. Existing toilet soaps have a weak effect on skin sterilization due to their single composition, while natural active ingredients from plants provide a source for screening new antibacterial agents. New toilet soap products with natural plant extracts as active ingredients are gradually emerging, which not only have a strong cleaning function but also special effects such as antioxidant and antibacterial effects.

[0003] Catalpa bungei belongs to the genus Catalpa of the family Bignoniaceae and is an important native tree species in China. "Chinese Medicinal Resources Compendium" records the extensive medicinal value of Catalpa bungei. Its root bark and bark (Catalpa wood bark) are bitter and cool. It has the functions of clearing heat and detoxifying, dispersing stasis and detumescence. It is used for traumatic injuries, fractures, carbuncles and sores, hemorrhoids and fistulas, vomiting, and cough. Its leaves (Catalpa leaves) are bitter and cool. It has the functions of detumescence and removing toxins, discharging pus and promoting granulation. It is used for scrofula. Its flowers are bitter and cool. It has the functions of detoxifying, relieving pain, and promoting granulation. Its fruits and seeds are bitter and cool. It has the function of clearing heat and diuresis. It is used for stranguria, calculus stranguria, heat toxin, and scabies.

[0004] Currently, the research on Catalpa bungei mainly focuses on its flowers, leaves, fruits, seeds, etc., and there is almost no research on its heartwood, especially on its chemical components, medicinal activities and related mechanisms, and there are few reports. In view of the literature reports on the chemical components and antibacterial research of Catalpa bungei, the present invention takes the heartwood of the unique variety Catalpa bungei “Jinsi” in China as the object, and obtains an extract rich in antibacterial components through extraction, column chromatography, and concentration, and adds it to the soap-making process to prepare a new type of plant extract antibacterial soap. Summary of the Invention

[0005] To solve the problem that existing toilet soaps have a weak antibacterial and bacteriostatic effect on human skin due to their single composition. The present invention provides a formulation and preparation method of an antibacterial soap containing a Catalpa bungei “Jinsi” composition. The finished product prepared by combining the added Catalpa bungei “Jinsi” composition with the traditional soap-making process not only has a function of removing dirt from human skin but also has a good antibacterial effect, and at the same time can enhance the market competitiveness.

[0006] The specific technical solution to achieve the above technical effects is as follows:

[0007] An antibacterial composition of Catalpa bungei “Jinsi” includes a mixture formed by catalpolide and 4,9-dihydroxy-α-lapachone.

[0008] The mass fraction of catalpolide is 50 - 65%, and the mass fraction of 4,9-dihydroxy-α-lapachone is 20 - 30%.

[0009] As a preferred embodiment, the mass fraction of catalpolide is 62 - 65%, and the mass fraction of 4,9-dihydroxy-α-lapachone is 20 - 23%.

[0010] The catalpa ovata antibacterial composition is obtained by mixing catalpolide and 4,9-dihydroxy-α-lapachone in a raw material compounding manner; or is obtained by a separation and extraction method using catalpa ovata as a raw material.

[0011] As a preferred embodiment, the steps for obtaining by a separation and extraction method using catalpa ovata as a raw material are as follows:

[0012] Powder of the heartwood part of catalpa ovata is placed in dichloromethane solvent for cold soaking at room temperature. The obtained extract is evaporated to dryness under reduced pressure to obtain a dark brown extract; the obtained dark brown extract is separated by silica gel column chromatography, eluted with a mixed solvent of dichloromethane and methanol, eluted with pure methanol after the elution is completed, the methanol eluate is collected, and concentrated under reduced pressure to obtain the catalpa ovata composition.

[0013] The obtained catalpa ovata composition is analyzed by AQ-C18 high performance liquid chromatography. The AQ-C18 high performance liquid chromatography analysis conditions are as follows: the chromatographic column is an AQ-C18 column 4.6×250mm, 5μm; the mobile phase is methanol (phase A) - water (phase B) (gradient: 0 - 20 min, 10% - 100% methanol; 20 - 30 min, 100% methanol; 30 - 35 min, 100% - 10% methanol); the flow rate is 1.0 mL / min; the injection volume is 10.0 μL; the detection wavelength is 254 nm; the column temperature is 30°C.

[0014] In the catalpa ovata antibacterial composition obtained by the separation and extraction method using catalpa ovata as a raw material, the mass fraction of catalpolide is 50 - 65%, and the mass fraction of 4,9-dihydroxy-α-lapachone is 20 - 30%.

[0015] As a preferred embodiment, the mass fraction of catalpolide is 62 - 65%, and the mass fraction of 4,9-dihydroxy-α-lapachone is 20 - 23%.

[0016] In the mixed solvent of dichloromethane and methanol, the volume ratio of dichloromethane to methanol is 25 - 35:1.

[0017] The present invention also provides an antibacterial soap, which includes the above-mentioned catalpa ovata antibacterial composition, and the bacteria include Staphylococcus aureus.

[0018] The present invention also provides an antibacterial soap formulation comprising the above-mentioned antibacterial soap formulation, wherein the soap solution containing olive oil and the Catalpa bungei antibacterial composition have a volume ml / quality mg ratio of 50:3 - 12.

[0019] The soap solution of olive oil is a mixed solution formed by olive oil and an aqueous solution of sodium hydroxide at 50°C. The Catalpa bungei antibacterial composition is dissolved in DMSO. The specific operation steps are as follows: Put sodium hydroxide and distilled water into a stirring container and stir. After fully dissolving, let it stand and cool down to about 50°C. Place the olive oil in a constant temperature water bath and heat it while stirring to about 50°C. When the temperature is between 40 - 50°C, mix and stir the olive oil and the aqueous sodium hydroxide solution. Take an appropriate amount of soap solution, add the Catalpa bungei composition (dissolved in DMSO) and stir evenly. Product packaging can be carried out 3 - 5 minutes after demolding.

[0020] The beneficial effects of the present invention are as follows: The present invention uses the Catalpa bungei composition from natural sources and having a sterilization effect as the sterilization formula. The finished product prepared by the present invention by combining olive oil, sodium hydroxide, and distilled water using the traditional soap-making process not only has a decontamination function for human skin (olive oil, sodium hydroxide, and distilled water achieve the purpose of decontamination by forming soap salts to emulsify the substances on the skin surface), but also has good sterilization and antibacterial effects. Based on the above, the present invention has broad application prospects. Description of the Drawings

[0021] The present invention will be further described below in conjunction with the drawings and embodiments.

[0022] Figure 1 It is a flow chart of the production process of an antibacterial soap containing the Catalpa bungei composition according to the present invention.

[0023] Figure 2 It is the liquid phase analysis spectrum of the Catalpa bungei composition and the ultraviolet absorption spectrum of the main components prepared in Example 2 of the present invention.

[0024] Figure 3 It is the standard product of catalpolide and its ultraviolet absorption spectrum.

[0025] Figure 4 It is the standard product of 4,9-dihydroxy-α-lapachone and its ultraviolet absorption spectrum.

[0026] Figure 5 It is a sample of an antibacterial soap containing the Catalpa bungei composition according to the present invention. Detailed Embodiments

[0027] Example 1

[0028] A Catalpa bungei antibacterial composition, the Catalpa bungei antibacterial composition comprising a mixture formed by catalpol and 4,9-dihydroxy-α-lapachone, the mass fraction of catalpol being 62%, the mass fraction of 4,9-dihydroxy-α-lapachone being 23%, and the remainder being water.

[0029] Example 2

[0030] Using Catalpa bungei as a raw material, the Catalpa bungei antibacterial composition of Example 1 was separated and extracted as follows:

[0031] The powder of the heartwood of Catalpa bungei was placed in dichloromethane solvent 5 times its mass and cold soaked at room temperature for 72 h, filtered to obtain the extract, and the solvent was evaporated under reduced pressure, that is, the dichloromethane in the extract was evaporated under reduced pressure to obtain a dark brown extract; 6.5 g of the extract was taken, dissolved in 1.5 mL of dichloromethane, and mixed with 14.6 g of silica gel of 200-300 mesh, and then loaded onto a chromatography column (column size: 90×500 mm, column packing height: 200 mm); after loading, elution was carried out with dichloromethane:methanol = 30:1 (v / v), the elution volume was 4.5 L, after the elution was completed, pure methanol was used for elution, the methanol eluate was collected, and concentrated under reduced pressure to obtain 4.5 g of an extract, with a yield of 69.2%. The main components of the Catalpa bungei composition were analyzed by AQ-C18 high performance liquid chromatography to be catalpol (content 62%) and 4,9-dihydroxy-α-lapachone (content 23%). As Figure 2 shown, Figure 3 is the standard product of catalpol and the ultraviolet absorption spectrum. Figure 4 is the standard product of 4,9-dihydroxy-α-lapachone and the ultraviolet absorption spectrum.

[0032] AQ-C18 high performance liquid chromatography analysis conditions: the chromatographic column was an AQ-C18 column 4.6×250 mm, 5 μm; the mobile phase was methanol (phase A) - water (phase B) (gradient: 0 - 20 min, 10% - 100% methanol; 20 - 30 min, 100% methanol; 30 - 35 min, 100% - 10% methanol); the flow rate was 1.0 mL / min; the injection volume was 10.0 μL; the detection wavelength was 254 nm; the column temperature was 30 °C.

[0033] Example 3

[0034] Preparation of olive oil soap solution: 17.42 g of sodium hydroxide and 69.68 mL of distilled water were placed in a stirring container and stirred until fully dissolved, then left to stand and cool down to 50 °C; 130 g of olive oil was placed in a constant temperature water bath and heated with stirring to 50 °C. The two were mixed and stirred to obtain the olive oil soap solution;

[0035] Add 50 mL of olive oil soap solution to 3 mg of the Catalpa bungei composition prepared in Example 2 (the 3 mg of the Catalpa bungei composition is dissolved in 1 mL of DMSO) and stir evenly to obtain the formula of the antibacterial soap containing the Catalpa bungei composition.

[0036] Example 4

[0037] The method and steps are the same as those in Example 3, except that the added amount of the Catalpa bungei composition prepared in Example 2 is 7.5 mg.

[0038] Example 5

[0039] The method and steps are the same as those in Example 3, except that the added amount of the Catalpa bungei composition prepared in Example 2 is 12 mg.

[0040] Example 6

[0041] The method and steps are the same as those in Example 3, except that the added amount of the Catalpa bungei composition prepared in Example 2 is 4.5 mg.

[0042] Example 7

[0043] To further prove the feasibility of the present invention, the inventor conducted the following experiments:

[0044] I. Sensory index detection

[0045] Standard requirements: Appearance: The soap shape is regular, the color is uniform, without obvious impurities and stains; Odor: There is a stable odor, without bad odors such as rancid oil.

[0046] Detect the sensory properties of Examples 3-6 of the present invention, and the results are shown in Table 1.

[0047] Table 1. Sensory evaluation of the sample soaps in the examples

[0048]

[0049] Result: As can be seen from Table 1, the sensory inspections of Examples 3-6 are all qualified.

[0050] II. Antibacterial effect test

[0051] The antibacterial soaps containing Catalpa bungei obtained in Examples 3-6 above were tested for antibacterial effect by the "paper disk test method", and all operations were completed on a "clean bench", and the results are shown in Table 2. The specific steps are as follows:

[0052] (1) The four groups of antibacterial soaps were longitudinally divided into upper, middle, and lower layers. Then, three soap grains in the central part were pressed out from each layer with a cylindrical column (Ф5mm). Nine soap grains were obtained respectively and weighed 0.6g each with an electronic balance. First, 8 - 10 drops of distilled water were added to each group, and the soap grains were mashed with a glass rod and dissolved into soap solution in a water bath at 40 - 50°C. Five sterile filter paper disks (Ф9mm) were immersed in the soap solution to prepare drug - sensitive filter paper disks.

[0053] (2) 100 μL of Staphylococcus aureus liquid was aspirated with a pipette and put into the prepared LB medium. The bacterial liquid was evenly spread on the medium with a spreader. The culture dish was divided into 3 areas, and 3 drug - sensitive filter paper disks were randomly placed in each group.

[0054] (3) After the treated culture dishes were incubated at room temperature (29°C) for 8 - 9 h, the diameter of the antibacterial circle was measured to judge the antibacterial effect.

[0055] The antibacterial effects of Examples 3 - 6 of the present invention were detected, and the results are shown in Table 2.

[0056] Table 2. Evaluation of the antibacterial effect of the sample soaps in the examples

[0057]

[0058]

[0059] Result: The Catalpa bungei C. A. Mey. antibacterial soaps provided in Examples 3 - 6 of the present invention have good antibacterial effects.

[0060] The above general description, specific implementation methods, and test examples have described the present invention in detail, showing the main features and advantages of the present invention. For those skilled in the art, obviously, the present invention is limited to the details of the above - mentioned exemplary embodiments. Therefore, any modifications or improvements made without departing from the spirit of the present invention fall within the scope of the present invention claimed.

Claims

1. Use of a composition containing Catalpa bungei in the preparation of an antibacterial soap, characterized in that Preparation of olive oil soap solution: Put 17.42 g of sodium hydroxide and 69.68 mL of distilled water into a stirring container and stir. After complete dissolution, let it stand and cool down to 50 °C; Place 130 g of olive oil in a constant temperature water bath and heat it with stirring to 50 °C. After mixing and stirring the two, obtain the olive oil soap solution; Add 50 mL of the olive oil soap solution to 3 mg of the Catalpa bungei composition. The 3 mg of the Catalpa bungei composition is dissolved in 1 ml of DMSO, and stir evenly to obtain the formula of the antibacterial soap containing the Catalpa bungei composition; The preparation method of the Catalpa bungei composition is as follows: Put the powder of the heartwood part of Catalpa bungei into dichloromethane solvent with a mass 5 times that of it and carry out cold immersion at room temperature for 72 h. Filter to obtain the extract, and evaporate the solvent under reduced pressure, that is, evaporate the dichloromethane in the extract under reduced pressure to obtain a dark brown extract; Take 6.5 g of the extract, dissolve it with 1.5 mL of dichloromethane, mix the sample with 14.6 g of silica gel with a mesh size of 200-300, load the sample into a chromatography column, column size: 90×500 mm, loading column height: 200 mm; After loading the sample, elute with dichloromethane:methanol = 30:1 v / v, elution volume 4.5 L. After the elution is completed, elute with pure methanol, collect the methanol eluate, and concentrate it under reduced pressure to obtain 4.5 g of extract, with a yield of 69.2%. The main components of the Catalpa bungei composition obtained by AQ-C18 high performance liquid chromatography analysis are catalpolide, with a content of 62% and 4,9-dihydroxy-α-lapachone, with a content of 23%.

2. Use of a composition containing Catalpa bungei in the preparation of an antibacterial soap, characterized in that Preparation of olive oil soap solution: Put 17.42 g of sodium hydroxide and 69.68 mL of distilled water into a stirring container and stir. After complete dissolution, let it stand and cool down to 50 °C; Place 130 g of olive oil in a constant temperature water bath and heat it with stirring to 50 °C. After mixing and stirring the two, obtain the olive oil soap solution; Add 50 mL of the olive oil soap solution to 7.5 mg of the Catalpa bungei composition. The 7.5 mg of the Catalpa bungei composition is dissolved in 1 ml of DMSO, and stir evenly to obtain the formula of the antibacterial soap containing the Catalpa bungei composition; The preparation method of the Catalpa bungei composition is as follows: The heartwood powder of Catalpa bungei C. A. Mey. is placed in dichloromethane solvent at 5 times its mass and cold-soaked at room temperature for 72 h. The extract is filtered, and the solvent is evaporated under reduced pressure, that is, the dichloromethane in the extract is evaporated under reduced pressure to obtain a dark brown extract. Take 6.5 g of the extract, dissolve it with 1.5 mL of dichloromethane, mix the sample with 14.6 g of silica gel with a mesh size of 200 - 300, load the sample into a chromatography column, column size: 90×500 mm, column loading height: 200 mm. After loading the sample, elute with dichloromethane:methanol = 30:1 v / v, elution volume 4.5 L. After the elution is completed, elute with pure methanol, collect the methanol eluate, and concentrate it under reduced pressure to obtain 4.5 g of extract, with a yield of 69.2%. Through AQ-C18 high performance liquid chromatography analysis, the main components of the Catalpa bungei C. A. Mey. composition are catalpol, with a content of 62% and 4,9-dihydroxy-α-lapachone, with a content of 23%.

3. Use of a Catalpa bungei C. A. Mey. composition in the preparation of an antibacterial soap, characterized in that Preparation of olive oil soap solution: Put 17.42 g of sodium hydroxide and 69.68 mL of distilled water into a stirring container and stir. After fully dissolving, let it stand and cool down to 50 °C. Place 130 g of olive oil in a constant temperature water bath and heat it while stirring until 50 °C. Mix the two and stir to obtain olive oil soap solution; Add 50 mL of olive oil soap solution to 12 mg of Catalpa bungei C. A. Mey. composition. The 12 mg of Catalpa bungei C. A. Mey. composition is dissolved with 1 ml of DMSO, and stir evenly to obtain the formula of the antibacterial soap containing Catalpa bungei C. A. Mey. composition; The preparation method of the Catalpa bungei C. A. Mey. composition is as follows: The heartwood powder of Catalpa bungei C. A. Mey. is placed in dichloromethane solvent at 5 times its mass and cold-soaked at room temperature for 72 h. The extract is filtered, and the solvent is evaporated under reduced pressure, that is, the dichloromethane in the extract is evaporated under reduced pressure to obtain a dark brown extract. Take 6.5 g of the extract, dissolve it with 1.5 mL of dichloromethane, mix the sample with 14.6 g of silica gel with a mesh size of 200 - 300, load the sample into a chromatography column, column size: 90×500 mm, column loading height: 200 mm. After loading the sample, elute with dichloromethane:methanol = 30:1 v / v, elution volume 4.5 L. After the elution is completed, elute with pure methanol, collect the methanol eluate, and concentrate it under reduced pressure to obtain 4.5 g of extract, with a yield of 69.2%. Through AQ-C18 high performance liquid chromatography analysis, the main components of the Catalpa bungei C. A. Mey. composition are catalpol, with a content of 62% and 4,9-dihydroxy-α-lapachone, with a content of 23%.

4. Use of a Catalpa bungei C. A. Mey. composition in the preparation of an antibacterial soap, characterized in that Preparation of olive oil soap solution: Put 17.42 g of sodium hydroxide and 69.68 mL of distilled water into a stirring container and stir. After fully dissolving, let it stand and cool down to 50 °C. Place 130 g of olive oil in a constant temperature water bath and heat it while stirring until 50 °C. Mix the two and stir to obtain olive oil soap solution; Add 50 mL of olive oil soap solution to 4.5 mg of Catalpa bungei composition. The 4.5 mg of Catalpa bungei composition is dissolved in 1 mL of DMSO and stirred evenly to obtain the formula of the antibacterial soap containing Catalpa bungei composition. The preparation method of the Catalpa bungei composition is as follows: Place the powder of the heartwood of Catalpa bungei in dichloromethane solvent 5 times its mass and soak it at room temperature for 72 h. Filter to obtain the extract, and evaporate the solvent under reduced pressure, that is, evaporate the dichloromethane in the extract under reduced pressure to obtain a dark brown extract. Take 6.5 g of the extract, dissolve it in 1.5 mL of dichloromethane, mix the sample with 14.6 g of silica gel with a mesh size of 200-300, load the sample into a chromatography column. Column size: 90×500 mm, column loading height: 200 mm. After loading the sample, elute with dichloromethane:methanol = 30:1 v / v, elution volume 4.5 L. After the elution is completed, elute with pure methanol, collect the methanol eluate, and concentrate it under reduced pressure to obtain 4.5 g of extract, with a yield of 69.2%. The main components of the Catalpa bungei composition obtained by AQ-C18 high performance liquid chromatography analysis are catalpolide with a content of 62% and 4,9-dihydroxy-α-lapachone with a content of 23%.

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