A method for preparing an extract of a processed cortex phellodendri for removing dandruff

Abstract

The application belongs to the technical field of traditional Chinese medicine preparation, and relates to a preparation method of an extract of a prepared product of phellodendri cortex for removing dandruff. The preparation method specifies a processing technology of phellodendri cortex carbon, and obtains the prepared product extract of phellodendri cortex carbon by using ethyl acetate to extract the alcohol extract of phellodendri cortex carbon. The extract can play a role in removing dandruff, and provides a new herbal resource for daily chemical products.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of traditional Chinese medicine preparation, and particularly relates to a preparation method of a cortex phellodendri extract for removing dandruff. BACKGROUND

[0002] Cortex Phellodendri is a commonly used traditional Chinese medicinal material, has the effects of clearing heat and drying dampness, purging fire and removing dampness, and detoxifying and treating sores, is commonly known as Sichuan cortex phellodendri, is the dried bark of Phellodendron amurense Rupr. Phellodendron chinense Schneid. of Rutaceae, was first recorded in Shennong's Herbal Classic and was listed as the top grade. The main processed products of cortex phellodendri at present are raw cortex phellodendri, salted cortex phellodendri, wine cortex phellodendri, charred cortex phellodendri and honey cortex phellodendri. In the traditional effects, cortex phellodendri tastes bitter and is cold in nature, has the effects of clearing heat and drying dampness, purging fire and detoxification; and after being charred, cortex phellodendri enhances the astringent property and has the effect of hemostasis.

[0003] According to the theory of traditional Chinese medicine, factors such as blood heat and wind dryness of the body can cause the generation of dandruff. Long-term overtime, spicy diet or poor emotional state can cause blood heat to rise, thereby causing a large amount of dandruff to breed. Traditional Chinese medicine with the effects of clearing heat and drying dampness, astringency and hemostasis can regulate the damp and hot state of the scalp, relieve the problem of dandruff and achieve the effect of removing dandruff. Since ancient times, traditional Chinese medicine cortex phellodendri has had an external application mode, such as treating skin symptoms such as eczema, acne, psoriasis, tinea pedis and burns by virtue of the effects of clearing heat and detoxifying, astringing and promoting skin regeneration, and has good clinical effects, which provides a theoretical basis for the application of charred cortex phellodendri with the effects of astringency, hemostasis, clearing heat and drying dampness to the effect of removing dandruff in terms of traditional effects and application channels.

[0004] According to modern medical theory, when the Malassezia on the scalp grows excessively, it can cause the generation of dandruff. Malassezia can stimulate the scalp by metabolizing sebum to produce oleic acid, causing desquamation. At present, the market uses shampoo or medicine with antifungal effect to reduce the number of Malassezia and relieve dandruff. The above-mentioned cortex phellodendri has the effects of anti-inflammation and bacteriostasis, and since the carbonization of traditional Chinese medicine has the requirement of storing nature, the carbonized cortex phellodendri can retain the bacteriostatic effect of cortex phellodendri and increase the astringent property, thereby reducing the symptoms of blood heat rising. From the present theory, it can also be inferred that carbonized cortex phellodendri can achieve the effect of inhibiting dandruff.

[0005] Therefore, in combination with the traditional Chinese medicine theory and the modern medical theory, the application carries out the research on the application of carbonized cortex phellodendri to the effect of removing dandruff, optimizes the best processing technology of carbonized cortex phellodendri, screens the best bacteriostatic part of carbonized cortex phellodendri, and finally determines a preparation method of a cortex phellodendri extract for removing dandruff. SUMMARY

[0006] The purpose of this invention is to provide a method for preparing an extract from processed Phellodendron amurense charcoal for dandruff removal. This preparation method clarifies the processing technology of Phellodendron amurense charcoal and its dandruff-removing effect, expanding the value and uses of traditional Chinese medicine. This patent provides a charring process for Phellodendron amurense charcoal used for dandruff removal, and also defines the polar parts of the charcoal, which can more effectively achieve the dandruff-removing effect. This invention improves the application value of processed Phellodendron amurense products, expands the medicinal uses of Phellodendron amurense charcoal, and can further develop Phellodendron amurense charcoal into a dedicated dandruff-removing product.

[0007] To achieve the above objectives, the present invention adopts the following technical solution.

[0008] A method for preparing a processed extract of Phellodendron bark for dandruff removal includes the following steps:

[0009] Step 1: Place the raw Phellodendron bark slices into a multi-functional frying machine and fry them over high heat until the Phellodendron bark turns charcoal black on the outside and dark brown on the inside. Remove them and let them cool. Sift out the debris and remove impurities to obtain the Phellodendron bark charcoal product.

[0010] Step 2: Take the above-mentioned processed Phellodendron bark charcoal product, add ethanol solvent for extraction, reflux extraction twice, 1 hour each time, combine the two filtrates, concentrate the filtrate until the extract has no alcohol odor, and obtain Phellodendron bark charcoal extract. Disperse the extract with an appropriate amount of water, extract twice with ethyl acetate, combine the two extraction solvents, and then dissolve the ethyl acetate extract in water and adjust the concentration to 0.10 g / mL to obtain the Phellodendron bark processed product extract for dandruff removal.

[0011] Furthermore, in step 1, the temperature of the flame is 200-300℃.

[0012] Furthermore, in step 1, the roasting time of Phellodendron bark charcoal is 15-35 minutes, preferably 25 minutes.

[0013] Furthermore, in step 2, the mass of ethanol is 5-15 times that of the processed Phellodendron bark charcoal product, and it is 70% ethanol.

[0014] Furthermore, the charred extract of Phellodendron bark used to remove dandruff is used in dandruff-removing medicines.

[0015] Furthermore, the prepared charred extract of Phellodendron bark, which removes dandruff, significantly inhibits the effects of Malassezia furfur and Staphylococcus epidermidis, thereby reducing dandruff growth.

[0016] Compared with the prior art, the beneficial effects of the present invention are as follows.

[0017] Currently, existing technologies lack specific parameters for the processing of Phellodendron bark charcoal, which can easily lead to inconsistent processing results and failure to achieve the desired effect. In addition, this technology clarifies the extraction site for the dandruff-removing effect of Phellodendron bark charcoal and compares the dandruff-removing effects of Phellodendron bark charcoal extracts with different processing degrees and extraction sites of different polarities. It was found that the ethyl acetate extract of Phellodendron bark charcoal has the effect of inhibiting Malassezia furfur and Staphylococcus epidermidis, while also having an astringent effect, which is more conducive to achieving the dandruff-removing effect.

[0018] The preparation method and uses of Phellodendron amurense charcoal provided by this invention are not recorded in existing research reports. The preparation method is characterized by high efficiency, stable process, simple operation and low cost. Moreover, the Phellodendron amurense charcoal extract has a good effect on removing dandruff. Attached Figure Description

[0019] Figure 1 Image of processed Phellodendron bark extract. Detailed Implementation

[0020] The present invention will be further described in detail below with reference to specific embodiments, but it should not be construed as limiting the scope of the above-described subject matter of the present invention to the following examples. All technologies implemented based on the above-described content of the present invention fall within the scope of the present invention.

[0021] A method for preparing a processed extract of Phellodendron bark for dandruff removal includes the following steps:

[0022] Step 1: Place the raw Phellodendron bark slices into a multi-functional frying machine and fry them over high heat until the Phellodendron bark turns charcoal black on the outside and dark brown on the inside. Remove them and let them cool. Sift out the debris and remove impurities to obtain the Phellodendron bark charcoal product.

[0023] Step 2: Take the above-mentioned processed Phellodendron bark charcoal product, add ethanol solvent for extraction, reflux extraction twice, 1 hour each time, combine the two filtrates, concentrate the filtrate until the extract has no alcohol odor, and obtain Phellodendron bark charcoal extract. Disperse the extract with an appropriate amount of water, extract twice with ethyl acetate, combine the two extraction solvents, and then dissolve the ethyl acetate extract in water and adjust the concentration to 0.10 g / mL to obtain the Phellodendron bark processed product extract for dandruff removal.

[0024] Furthermore, in step 1, the temperature of the flame is 200-300℃.

[0025] Furthermore, in step 1, the roasting time of Phellodendron bark charcoal is 15-35 minutes, preferably 25 minutes.

[0026] Furthermore, in step 2, the mass of ethanol is 5-15 times that of the processed Phellodendron bark charcoal product, and it is 70% ethanol.

[0027] Furthermore, the charred extract of Phellodendron bark used to remove dandruff is used in dandruff-removing medicines.

[0028] Furthermore, the prepared charred extract of Phellodendron bark, which removes dandruff, significantly inhibits the effects of Malassezia furfur and Staphylococcus epidermidis, thereby reducing dandruff growth.

[0029] Example 1.

[0030] 1. Instruments and materials.

[0031] 1.1 Instruments: Multifunctional roasting machine (Mais Machinery), METTLER AE240 analytical balance (1 / 100,000), CNC ultrasonic cleaner, clean bench (Sujing Antai), -80℃ refrigerator (Qingdao Haier), micropipette (Thermo Fisher Scientific). Induction cooker, beakers, wide-mouth conical flasks, disposable plastic petri dishes (Beekman Biotechnology), disposable plastic spreading rods (Beekman Biotechnology), disposable plastic inoculation loops (Beekman Biotechnology), sterile filter paper (Beekman Biotechnology), tweezers, etc.

[0032] 1.2 Reagents: Phellodendron bark was purchased from Juyitang Pharmaceutical Co., Ltd.; 75% medical disinfectant alcohol and purified water were used; other reagents were of analytical grade. Beef powder, peptone, sodium chloride, agar, malt extract powder, ox bile powder, Tween 40, and glyceryl monooleate were all purchased from Beijing Solarbio Technology Co., Ltd. Staphylococcus epidermidis and Malassezia furfur were purchased from Beina Biotechnology.

[0033] 2. This embodiment provides a method for preparing an extract from processed Phellodendron amurense charcoal, comprising the following steps:

[0034] Raw Phellodendron bark slices (50 g) were placed in a 270℃ multi-functional roasting machine and roasted for 15 min, 25 min, and 35 min respectively. After cooling, the Phellodendron bark charcoal product was obtained. An appropriate amount of the Phellodendron bark charcoal product was extracted twice with 10 times the amount of 70% ethanol under reflux, each extraction lasting 1 hour. The two extracts were combined, and the filtrate was concentrated until no alcohol odor remained, yielding a Phellodendron bark charcoal extract. The extract was dispersed in an appropriate amount of water and extracted twice with ethyl acetate. The solvent was recovered, and the two extraction solvents were combined to obtain the ethyl acetate extract. The extract was then dissolved in water and the concentration was adjusted to 0.1 g / mL. The obtained Phellodendron bark charcoal extract roasted for 25 min is shown below. Figure 1 .

[0035] 3. The preparation process of the aforementioned Phellodendron bark charcoal.

[0036] The selection of the factor level of the roasting time of Phellodendron bark charcoal during the processing: Since Phellodendron bark charcoal belongs to the bark category of Chinese medicine and has a relatively thick texture, it is processed under high heat (the temperature of the bottom of the pot is 270℃). Under this condition, the roasting time of Phellodendron bark charcoal is optimized. The astringent and hemostatic effect of Phellodendron bark charcoal is used as the evaluation index, and the processing time is examined as the evaluation factor. Finally, the optimal processing technology of Phellodendron bark charcoal is determined.

[0037] Experimental study on hemostasis by tail amputation in mice

[0038] Experimental Methods: Eighteen Kunming mice (half male and half female) were randomly divided into four groups of six: *Phellodendron amurense* charcoal (roasted for 15 minutes), charcoal (roasted for 25 minutes), charcoal (roasted for 35 minutes), a control group, and a Yunnan Baiyao group (positive control). The tails of the mice were severed transversely at 0.5 cm from the tip using surgical scissors. For external application, the *Phellodendron amurense* charcoal powder was applied to each group using a sterile cotton swab; the Yunnan Baiyao group (positive control) had the tail section wrapped with a sterile cotton swab; and the control group received no treatment. The bleeding time was recorded from the onset of bleeding until it ceased. The results are shown in Table 1.

[0039] Table 1. Hemostatic effect of Phellodendron bark charcoal with different processing degrees (mean ± standard deviation n=6).

[0040]

[0041] The above hemostasis experiments show that the mice with charred Phellodendron bark that was stir-fried for 25 minutes experienced the shortest rebleeding time in their tails, indicating that charred Phellodendron bark with a stir-frying time of 25 minutes has a better hemostatic effect. Therefore, it was determined that stir-frying at 270℃ for 25 minutes is the optimal processing method for charred Phellodendron bark.

[0042] 4. To further verify the beneficial effects of the present invention, the following experimental case of "Phellodendron bark charcoal inhibiting Malassezia furfur and Staphylococcus epidermidis" is provided.

[0043] 4.1 Determination method.

[0044] Malassezia furfur and Staphylococcus epidermidis were activated and inoculated onto 9mm × 15mm plates, respectively, and incubated at 30℃ and 37℃. Antimicrobial susceptibility testing discs were placed in wide-mouth bottles, sterilized at 121℃ for 30 min, and then dried for later use. The prepared Phellodendron amurense charcoal extract was added to the antimicrobial susceptibility testing discs, and the discs were soaked at 4℃ for 2 h. 100 μL of the experimental bacterial suspension was added to each plate and spread evenly using a sterile spreader. The prepared antimicrobial susceptibility testing discs were then attached to the plates, with three replicates. The plates with the antimicrobial susceptibility testing discs were inverted and incubated for 24 h, and the diameter of the inhibition zone was measured. The size of the inhibition zone indicates the strength of the antimicrobial effect; a smaller diameter indicates a weaker antimicrobial effect, and a larger diameter indicates a stronger antimicrobial effect.

[0045] A method for preparing an extract from processed Phellodendron amurense charcoal includes the following steps:

[0046] 50 g of raw Phellodendron bark slices were placed in a 270℃ multi-functional roasting machine and roasted for 15 min, 25 min, and 35 min respectively. After cooling, the Phellodendron bark charcoal product was obtained. An appropriate amount of the Phellodendron bark charcoal product was added to 10 times the amount of 70% ethanol for reflux extraction. The extraction was performed twice, each time for 1 hour. The two extracts were combined, and the filtrate was concentrated until there was no alcohol odor in the extract to obtain Phellodendron bark charcoal extract. The extract was dispersed in an appropriate amount of water and extracted twice with petroleum ether, ethyl acetate, and petroleum ether respectively. The solvents were recovered, and the two extraction solvents were combined to obtain the extract. The extract was then dissolved in water and the concentration was adjusted to 0.10 g / mL.

[0047] 4.2 Measurement Results

[0048] 4.2.1 Inhibition of Malassezia by different processed extracts of Phellodendron bark charcoal

[0049] Table 2. Inhibition of Malassezia by different degrees of processing of Phellodendron bark charcoal and non-polar fractions.

[0050]

[0051] ( / indicates no obvious antibacterial effect, ++ indicates a good antibacterial effect, and + indicates a certain antibacterial effect.)

[0052] 4.2.2 Inhibition of Staphylococcus epidermidis by different processed extracts of Phellodendron bark charcoal:

[0053] Table 3. Inhibition of Staphylococcus epidermidis by different degrees of processing of Phellodendron bark charcoal and non-polar fractions.

[0054]

[0055] ( / indicates no obvious antibacterial effect, ++ indicates a good antibacterial effect, and + indicates a certain antibacterial effect.)

[0056] Antibacterial experiments revealed that, in terms of processing time, charred Phellodendron amurense processed for 15 minutes and 25 minutes showed a more significant inhibitory effect on Malassezia furfur and Staphylococcus epidermidis compared to charred Phellodendron amurense processed for 35 minutes. Regarding different polar fractions of the charred Phellodendron amurense, the ethyl acetate layer exhibited significant inhibition of Malassezia furfur and Staphylococcus epidermidis, followed by the n-butanol layer, while the petroleum ether layer showed almost no antibacterial effect. Antibacterial experiments and mouse hemostasis experiments showed that the ethyl acetate polar fraction of charred Phellodendron amurense processed at 270℃ for 25 minutes had a good antibacterial effect, indicating that the extract has a certain anti-dandruff effect. In summary, the preparation of the Phellodendron amurense extract for anti-dandruff purposes in this patent utilizes the ethyl acetate polar fraction for extraction to achieve an anti-dandruff effect.

[0057] Example 2.

[0058] 50g of processed Phellodendron bark slices were placed in a stir-frying container and stir-fried at 270℃ for 25 minutes. After cooling, impurities were removed by sieving to obtain the charred Phellodendron bark product. The charred Phellodendron bark slices were then extracted twice with 15 times the volume of 70% ethanol under reflux, 1 hour each time. The extracts were filtered, and the filtrates were combined. The ethanol was recovered under reduced pressure until no alcohol odor remained, yielding an alcohol extract. The extract was dispersed in an appropriate amount of water and extracted with ethyl acetate. The remaining aqueous layer was then extracted again with ethyl acetate to obtain an ethyl acetate extract. This extract was then dissolved in water, and the concentration was adjusted to 0.10g / mL to obtain the final product.

[0059] Example 3: Typical Case.

[0060] Case 1: Mr. Li, male, 22 years old, often experienced symptoms of seborrheic dermatitis, including thick oily secretions on the scalp or dry hair, accompanied by greasy scales and mild itching. After using the extract of Example 2 of this invention for 5 consecutive days, his symptoms were relieved and his dandruff was significantly reduced.

[0061] Case 2: Ms. Wang, 51 years old, suffered from pityriasis alba, with visible snowflake-like dandruff and itching. The main cause was the disruption of the balance between the proliferation of Malassezia and the secretion of sebum in the body. After intermittent use of the extract of Example 2 of this invention for 15 days, the symptoms were relieved and the dandruff was reduced.

[0062] Comparative Example 1.

[0063] 50g of Phellodendron bark slices were placed in a stir-frying container and stir-fried at 270℃ for 15 minutes. After cooling, impurities were removed by sieving to obtain the Phellodendron bark charcoal product. The charcoal slices were then extracted twice with 5 times the volume of 70% ethanol under reflux, 1 hour each time. The extracts were filtered, and the filtrates were combined. The ethanol was recovered under reduced pressure until no alcohol odor remained, yielding an alcohol extract. The extract was dispersed in an appropriate amount of water and extracted with petroleum ether. The remaining aqueous layer was then extracted with petroleum ether again to obtain a petroleum ether extract. This extract was then dissolved in water, and the concentration was adjusted to 0.10g / mL. Using antibacterial effect as the evaluation index, the Phellodendron bark charcoal extract obtained in Comparative Example 1 showed almost no anti-dandruff effect.

[0064] Comparative Example 2.

[0065] 50g of Phellodendron bark slices were placed in a stir-frying container and stir-fried at 270℃ for 35 minutes. After cooling, impurities were removed by sieving to obtain the Phellodendron bark charcoal product. The charcoal slices were then extracted twice with 10 times the amount of 70% ethanol under reflux, 1 hour each time. The extracts were filtered, and the filtrates were combined. The ethanol was recovered under reduced pressure until no alcohol odor remained, yielding an alcohol extract. The extract was dispersed in an appropriate amount of water and extracted with n-butanol. The remaining aqueous layer was then extracted with n-butanol to obtain the n-butanol extract. The extract was then dissolved in water, and the concentration was adjusted to 0.05g / mL. Using antibacterial effect as the evaluation index, the dandruff-removing effect of the Phellodendron bark charcoal extract obtained in Comparative Example 2 was weaker than that of Example 2.

Claims

1. A method for preparing an extract of processed Phellodendron amurense bark for dandruff removal, characterized in that, The preparation method includes the following steps: Step 1: Place the raw Phellodendron bark slices into a multi-functional frying machine and fry them over high heat until the outside of the Phellodendron bark turns charred black (200-300℃) and the inside turns dark brown. Remove and let cool, sift out the debris and remove impurities to obtain the Phellodendron bark charcoal product. The frying time for Phellodendron bark charcoal is 15-35 minutes. Step 2: Take the above-mentioned processed Phellodendron bark charcoal product, add ethanol solvent for extraction, the ethanol mass should be 5-15 times that of the processed Phellodendron bark charcoal product, use 70% ethanol, reflux extraction twice, 1 hour each time, combine the two filtrates, concentrate the filtrate until the extract has no alcohol odor, to obtain Phellodendron bark charcoal extract, disperse the extract with an appropriate amount of water, extract twice with ethyl acetate, combine the two extraction solvents, obtain ethyl acetate extract, then dissolve in water, adjust the concentration to 0.10 g / mL, to obtain the Phellodendron bark processed product extract for dandruff removal.

2. The method for preparing the Phellodendron amurense extract for dandruff removal according to claim 1, characterized in that, The application of the charred extract of Phellodendron bark for removing dandruff in the preparation of dandruff-removing drugs.

3. The method for preparing the Phellodendron amurense extract for dandruff removal according to claim 1, characterized in that, The prepared charred extract of Phellodendron bark, which removes dandruff, inhibits Malassezia furfur and Staphylococcus epidermidis, thereby reducing dandruff growth.

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