Oil-control soothing composition as well as preparation method and application thereof

Abstract

The invention provides an oil-control soothing composition as well as a preparation method and application thereof, and belongs to the technical field of daily chemicals. The invention relates to an oil-controlling and soothing composition, which is prepared by compounding the following components in parts by weight: 1 to 4 parts of cortex magnoliae officinalis extract, 0.5 to 3 parts of fructus crataegi extract, 0.2 to 2 parts of lemon peel extract, 0.5 to 3 parts of tea extract, 0.2 to 2 parts of sophora flower bud extract and 0.5 to 3 parts of fructus cnidii extract. 0.2-2 parts of a sophora flower bud extract and 0.1-3 parts of a fructus cnidii extract. The composition disclosed by the invention has the obvious effects of being mild and safe, efficiently controlling oil and relieving scalp.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of daily chemicals, and particularly relates to an oil control and soothing composition based on magnolia officinalis bark molecular imprinting extract, a preparation method and application thereof. BACKGROUND

[0002] The structure of the scalp includes epidermis, dermis and subcutaneous tissue. The dermis contains more sebaceous glands and hair follicles, and the sweat glands are located deeper, with some hair follicles reaching the subcutaneous fat. The structure of the scalp hair follicle includes hair shaft, hair root, hair bulb, hair papilla and surrounding structure. Among them, the hair papilla provides nutrition and signals for the hair matrix cells in the hair bulb, promoting their continuous division and growth; the sebum secreted by the sebaceous glands in the surrounding structure of the hair follicle plays an important role in lubrication and protection of the scalp and hair, moisture retention, antibacterial and antifungal properties, and maintenance of acid-base balance. Scalp itching may be a manifestation of scalp neurodermatitis, which sometimes presents as multiple.

[0003] Commercial anti-dandruff shampoos often rely on chemical anti-dandruff agents such as zinc pyrithione and ketoconazole, which have irritant properties, drug resistance and long-term use safety concerns. Although plant-based formulations are mild, they are limited by the selectivity and insufficient purity of conventional extraction, and the effective concentration and stability of active ingredients are difficult to guarantee, resulting in unstable dandruff / oil control effects. Magnolol and honokiol in magnolia officinalis bark have anti-inflammatory, antibacterial and scalp soothing potential, but the selectivity of traditional alcohol extraction / water-alcohol extraction for these components is limited, with high impurity interference, limited yield and purity, making it difficult to achieve repeatable significant effects in the final formulation.

[0004] Chinese patent application 202110766391.8 discloses an anti-dandruff and oil control composition, its preparation method and application, which contains an anti-dandruff component or / and an oil control component. The anti-dandruff component can be selected from sulfur, colloidal sulfur, piroctone olamine, etc., and the oil control component can be selected from capryloyl glycine, undecylenoyl glycine, zinc gluconate, etc. The composition has certain anti-dandruff and oil control effects, but sulfur in the anti-dandruff component has good bactericidal effect, but it can cause certain damage to hair quality and scalp.

[0005] In view of the problems of scalp sensitivity and oiliness that cause trouble to consumers, it is urgent to develop a safe and effective composition with natural oil control and soothing and itching-relieving effects, its preparation method and application. SUMMARY

[0006] Therefore, the technical problem to be solved by the present application is to provide an oil control and soothing composition containing natural ingredients, which has the remarkable effects of mild safety, high-efficiency oil control and scalp soothing.

[0007] In a first aspect, the present application provides an oil control and itch relieving composition, which is composed of Magnolia officinalis bark extract, Crataegus monogyna Jacq extract, Citrus limonum fruit extract, Camellia sinensis extract, Sophora japonica flower bud extract and Cnidium monnieri extract.

[0008] The Magnolia officinalis bark extract, Crataegus monogyna Jacq extract, Citrus limonum fruit extract, Camellia sinensis extract, Sophora japonica flower bud extract and Cnidium monnieri extract are compounded as the oil control and itch relieving composition, which has significant synergistic effect and can effectively reduce the secretion of sebum, relieve the itch and dandruff.

[0009] Preferably, the oil control and itch relieving composition is composed of 1-4 parts of Magnolia officinalis bark extract, 0.5-3 parts of Crataegus monogyna Jacq extract, 0.2-2 parts of Citrus limonum fruit extract, 0.5-3 parts of Camellia sinensis extract, 0.2-2 parts of Sophora japonica flower bud extract and 0.1-3 parts of Cnidium monnieri extract.

[0010] Preferably, the Magnolia officinalis bark extract is extracted by molecular imprinting polymerization method, and the preparation method comprises the following steps: Step a: mixing pseudo-template molecules, functional monomers, cross-linking agents, initiators and a first solvent, and polymerizing at 40-60°C under nitrogen protection for 6-8h to obtain a molecular imprinting polymer; Step b: recycling eluting the molecular imprinting polymer to HPLC template peak disappearance by using a second solvent; Step c: mixing Magnolia officinalis bark crude extract and the molecular imprinting polymer treated in step b, and oscillating at room temperature for 1-3h; Step d: selectively eluting the extract obtained in step c by using a third solvent to obtain Magnolia officinalis bark extract.

[0011] In step b, the molecularly imprinted polymer is eluted with the second solvent until the template peak disappears. Specifically, the molecularly imprinted polymer is eluted with the second solvent. The elution process continues until the detection result of the pseudo-template molecule (the retention time RT is about 6.20 min, and the MS spectrum is completely consistent with the standard) is lower than the limit of quantification (LOQ is not greater than 0.30 µg / g) of the method or cannot be detected (the signal-to-noise ratio S / N is less than 3) under the detection conditions of the methodologically verified GC-MS (or LC-MS / MS). During the elution process, each elution solution is collected and detected for the content of the pseudo-template molecule. The elution continues until the residual amount of the pseudo-template molecule in the molecularly imprinted polymer sample is not more than LOQ. For example, the related experimental data show that the content of the pseudo-template molecule in the molecularly imprinted polymer sample is 120.0 ± 5.0 µg / g without elution. After 4 rounds of elution, the residual amount is reduced to 0.45 ± 0.05 µg / g. After 5 rounds of elution, the residual amount is less than or equal to 0.30 µg / g (the data is the average result of 3 parallel experiments). Through the above complete elution and detection process, it can be fully proved that the pseudo-template molecule has been effectively removed, thereby meeting the related process requirements and safety standards.

[0012] As preferred, the pseudo-template molecule is 5,5'-dipropyl-2,2'-diphenol; The functional monomer is methacrylic acid or acrylamide or 4-vinylpyridine, and the molar ratio of the pseudo-template molecule to the functional monomer is 1: (4-6); The crosslinking agent is divinylbenzene or ethylene glycol dimethacrylate or TRIM (1,1,1,3,5,7,7,7-octamethyl-3,5-bis(trimethylsilyloxy)tetrasiloxane), and the molar ratio of the sum of the moles of the pseudo-template molecule and the functional monomer to the crosslinking agent is 1: (20-30); The initiator is azobisisobutyronitrile, and the amount is 0.5-1.5 wt% of the functional monomer; The first solvent is a mixed solution of acetonitrile and toluene, and the volume ratio of acetonitrile to toluene is 1:1, or an equivalent inert solvent; The second solvent is a mixed solution of ethanol and acetic acid, and the volume ratio of ethanol to acetic acid is 9:1; The crude magnolia bark extract is an extract obtained by reflux extraction of magnolia bark with ethanol; The third solvent is a mixed solution of an ethanol aqueous solution and an organic acid, the volume fraction of ethanol in the ethanol aqueous solution is 95-100%, the organic acid is acetic acid, and the volume ratio of ethanol to acetic acid is 9:1.

[0013] In a second aspect, the present application provides a preparation method of the oil control and itch relieving composition, comprising the following steps: Step 1, mixing and stirring the Magnolia officinalis bark extract, the Crataegus monogyna Jacq. extract and the Cnidium monnieri extract uniformly to prepare a mixture; Step 2, adding the Citrus limonum peel extract, the tea extract and the Sophora japonica flower bud extract into the mixture, stirring uniformly to prepare the oil control and itch relieving composition.

[0014] The oil control and itch relieving composition is prepared in two steps, so that the components can be fully dispersed, and the oil control and itch relieving composition has good stability.

[0015] In a third aspect, the present application provides an application of the oil control and itch relieving composition in hair products, wherein the hair products include scalp essence, hair conditioner, hair mask and shampoo, and the mass fraction of the oil control and itch relieving composition in the hair products is 2-12%.

[0016] The oil control and itch relieving composition is applied in hair products such as scalp essence, hair conditioner, hair mask and shampoo, and by controlling the mass fraction of the oil control and itch relieving composition in the hair products to be 2-12%, the hair products have good oil control and itch relieving effects.

[0017] Compared with the prior art, the present application has the following beneficial effects: The Magnolia officinalis bark extract, the Crataegus monogyna Jacq. extract, the Citrus limonum peel extract, the tea extract, the Sophora japonica flower bud extract and the Cnidium monnieri extract are compounded as the oil control and itch relieving composition, have significant synergistic effect, and can effectively reduce the secretion of scalp oil, relieve scalp itching and dandruff.

[0018] The properties of the extracts in the oil control and itch relieving composition are as follows: The Magnolia officinalis bark extract contains Magnolia officinalis total phenol which has a bacteriostatic effect on Staphylococcus aureus, and the core component is honokiol which is isomeric with magnolol and is one of the effective components of magnolol. Studies have shown that honokiol has strong antioxidant capacity, can inhibit the up-regulation of inflammatory factor-related genes and TLR2 gene expression levels caused by Staphylococcus aureus stimulation, reduce the abundance of Malassezia on the scalp and promote the recovery of beneficial flora; secondly, it has a broad-spectrum anti-inflammatory effect, and its anti-inflammatory mechanism is to block the PI3K / Akt, ERK / MAPK and TLR / MAPK signaling pathways, inhibit the expression of inflammatory cytokines, and also can block the synthesis and release of nitric oxide, TGs, LTs by directly inhibiting the enzyme activity of iNOS, COX-2 and 5-LO, and inhibit the release of histamine, etc., to produce a broad-spectrum anti-inflammatory effect, and researchers have found that Magnolia officinalis extract can regulate GABA receptors, relieve neuropathic pain and inflammation.

[0019] In the present application, the Magnolia officinalis bark extract is extracted by molecular imprinting polymerization method, and the purity of honokiol in the obtained extract is 30-35%, which is increased by more than 10% compared with the conventional alcohol extraction method, and the impurities are reduced by more than 20%, which significantly improves the effects of dandruff removal, moisturizing, oil control, soothing and the like.

[0020] The Crataegus monogyna fruit extract contains flavonoids, including quercetin and quercetin glycosides, and triterpenoids, including oleanolic acid; wherein, the natural product oleanolic acid (3β-hydroxyolean-12-en-28-oic acid, OA) is a bioactive pentacyclic triterpenoid compound existing in some foods and plants, and research has found that oleanolic acid has the effect of targeting androgen signaling, reducing the expression of DHT and 5α-reductase, reducing the thickening of the prostate epithelial layer, and inhibiting the excessive proliferation of epithelial and interstitial cells. Quercetin glycoside derivatives have been found to have good inhibitory effect and selectivity on Malassezia beta-carbonic anhydrase (MgCA) in the present research. The above research shows that the Crataegus monogyna fruit extract has the effects of oil control and antibacterial.

[0021] The Cnidium fruit extract is rich in coumarin compounds (such as cnidimide and imperatorin), volatile oil components (such as cnidimene), flavonoids and other active ingredients, and has significant anti-inflammatory, antibacterial and antifungal effects. Research has shown that cnidimide can inhibit the expression of inflammatory factors IL-6 and TNF-α, and has the effect of relieving itching and soothing. At the same time, it has a strong inhibitory effect on skin pathogenic bacteria such as Staphylococcus aureus and Candida albicans. The volatile oil of Cnidium has the effects of inhibiting allergic reactions and stabilizing mast cells, which helps to relieve itching and inflammation caused by allergic reactions or barrier damage. In addition, its antioxidant activity can reduce the level of free radicals and protect skin cells, and has the functions of skin itching relief and sensitive care.

[0022] The oil control soothing composition of the present application is composed of a plurality of plant-derived ingredients, and has significant stability, safety and mildness. It not only has excellent oil control effect, but also can soothe the scalp, reduce scalp itching and inflammation and hair loss caused by excessive secretion of oil, thereby significantly preventing and relieving related scalp health problems. DETAILED DESCRIPTION

[0023] In order to better understand the present application, the content of the present application will be further clarified in combination with the examples below, but the protection content of the present application is not limited to the following examples. In the following description, a large number of specific details are given in order to provide a more thorough understanding of the present application. However, it is obvious to those skilled in the art that the present application can be implemented without one or more of these details.

[0024] The various raw materials of the present application can be commercially available or prepared according to the conventional methods in the technical field, unless otherwise specified.

[0025] Example 1 The oil-controlling and itching-relieving composition is composed of Magnolia officinalis bark extract, Crataegus monogyna Jacq. extract, Citrus limonum fruit extract, Camellia sinensis extract, Sophora japonica flower bud extract and Cnidium monnieri extract; and the composition is composed of 2 parts of Magnolia officinalis bark extract, 1 part of Crataegus monogyna Jacq. extract, 0.5 part of Citrus limonum fruit extract, 1 part of Camellia sinensis extract, 0.5 part of Sophora japonica flower bud extract and 0.2 part of Cnidium monnieri extract by weight.

[0026] The preparation method comprises the following steps: mixing and stirring Magnolia officinalis bark extract, Crataegus monogyna Jacq. extract and Cnidium monnieri extract to prepare a mixture; adding Citrus limonum fruit extract, Camellia sinensis extract and Sophora japonica flower bud extract into the mixture and stirring uniformly to prepare the oil-controlling and itching-relieving composition.

[0027] The Magnolia officinalis bark extract is extracted by a molecular imprinting polymerization method, and the preparation method comprises the following steps: Step a: mixing a pseudo-template molecule, a functional monomer, a crosslinking agent, an initiator and a first solvent, polymerizing at 50°C under nitrogen protection for 7h to obtain a molecular imprinting polymer; Step b: recycling eluting the molecular imprinting polymer with a second solvent until the template peak of HPLC disappears; Step c: mixing the crude extract of Magnolia officinalis bark with the molecular imprinting polymer treated in step b, and oscillating at room temperature of 25°C for 2h; Step d: selectively eluting the extract obtained in step c with a third solvent to obtain the Magnolia officinalis bark extract.

[0028] The pseudo-template molecule is 5,5'-dipropyl-2,2'-diphenol; the functional monomer is methacrylic acid, and the molar ratio of the pseudo-template molecule to the functional monomer is 1:5; the crosslinking agent is divinylbenzene, and the molar ratio of the sum of the moles of the pseudo-template molecule and the functional monomer to the crosslinking agent is 1:25; the initiator is azobisisobutyronitrile, and the amount is 1.0wt% of the functional monomer; the first solvent is a mixed solution of acetonitrile and toluene, and the volume ratio of acetonitrile to toluene is 1:1; The second solvent is a mixed solution of ethanol and acetic acid, and the volume ratio of ethanol to acetic acid is 9:1; The crude extract of Magnolia officinalis bark is obtained by refluxing Magnolia officinalis bark with 70% ethanol for 1.5h and concentrating under reduced pressure; The third solvent is a mixed solution of an ethanol aqueous solution and an organic acid, the volume fraction of ethanol in the ethanol aqueous solution is 95%, and the organic acid is acetic acid, and the volume ratio of ethanol to acetic acid is 9:1.

[0029] Example 2The oil-controlling and itching-relieving composition is composed of Magnolia officinalis bark extract, Crataegus pinnatifida Bunge extract, lemon peel extract, tea extract, Sophora japonica flower bud extract and Cnidium monnieri extract; the composition is as follows in terms of weight parts: Magnolia officinalis bark extract 2.5 parts, Crataegus pinnatifida Bunge extract 2 parts, lemon peel extract 1.5 parts, tea extract 2 parts, Sophora japonica flower bud extract 0.5 part and Cnidium monnieri extract 0.2 part. The preparation method refers to Example 1.

[0030] The Magnolia officinalis bark extract is extracted by a molecular imprinting polymerization method, and the preparation method comprises the following steps: Step a: the pseudo-template molecule, functional monomer, crosslinking agent, initiator and first solvent are mixed, and the mixture is polymerized at 40 DEG C under nitrogen protection for 8 hours to obtain a molecular imprinting polymer; Step b: the molecular imprinting polymer is eluted with a second solvent until the template peak of HPLC disappears; Step c: the crude extract of Magnolia officinalis bark is mixed with the molecular imprinting polymer treated in step b, and the mixture is oscillated at room temperature of 25 DEG C for 1 hour; Step d: the extract obtained in step c is selectively eluted with a third solvent to obtain the Magnolia officinalis bark extract.

[0031] The pseudo-template molecule is 5,5'-dipropyl-2,2'-diphenol; the functional monomer is acrylamide, and the molar ratio of the pseudo-template molecule to the functional monomer is 1:4; the crosslinking agent is ethylene glycol dimethacrylate, and the molar ratio of the sum of the moles of the pseudo-template molecule and the functional monomer to the crosslinking agent is 1:30; the initiator is azobisisobutyronitrile, and the amount is 0.5-1.5 wt% of the functional monomer; the first solvent is a mixed solution of acetonitrile and toluene, and the volume ratio of acetonitrile to toluene is 1:1; The second solvent is a mixed solution of ethanol and acetic acid, and the volume ratio of ethanol to acetic acid is 9:1; The crude extract of Magnolia officinalis bark is obtained by refluxing Magnolia officinalis bark with 80% ethanol for 1 hour and concentrating under reduced pressure; The third solvent is a mixed solution of ethanol aqueous solution and organic acid, the volume fraction of ethanol in the ethanol aqueous solution is 95%, the organic acid is acetic acid, and the volume ratio of ethanol to acetic acid is 9:1.

[0032] Example 3 The oil-controlling and itching-relieving composition is composed of Magnolia officinalis bark extract, Crataegus pinnatifida Bunge extract, lemon peel extract, tea extract, Sophora japonica flower bud extract and Cnidium monnieri extract; the composition is as follows in terms of weight parts: Magnolia officinalis bark extract 2.5 parts, Crataegus pinnatifida Bunge extract 2 parts, lemon peel extract 1.5 parts, tea extract 2 parts, Sophora japonica flower bud extract 0.5 part and Cnidium monnieri extract 0.2 part. The preparation method refers to Example 1.

[0033] The Magnolia officinalis bark extract is extracted by a molecular imprinting polymerization method, and the preparation method comprises the following steps: Step a: mix pseudo-template molecule, functional monomer, crosslinking agent, initiator with first solvent, polymerize at 40-60℃ under nitrogen protection for 6-8h to obtain molecularly imprinted polymer; Step b: use second solvent to elute molecularly imprinted polymer to HPLC template peak disappears; Step c: mix Magnolia officinalis bark extract with molecularly imprinted polymer after step b treatment, oscillate at room temperature 23℃ for 3h; Step d: use third solvent to selectively elute extract obtained in step c to obtain Magnolia officinalis bark extract.

[0034] Wherein: pseudo-template molecule is 5,5'-dipropyl-2,2'-diphenol; functional monomer is 4-vinylpyridine, molar ratio of pseudo-template molecule to functional monomer is 1:(4-6); crosslinking agent is TRIM (1,1,1,3,5,7,7,7-octyl-3,5-bis(trimethylsilyloxy) tetrasiloxane), molar ratio of sum of moles of pseudo-template molecule and functional monomer to crosslinking agent is 1:(20-30); initiator is azobisisobutyronitrile, amount is 0.5-1.5wt% of functional monomer; first solvent is mixed solution of acetonitrile and toluene, volume ratio of acetonitrile to toluene is 1:1, or equivalent inert solvent; Second solvent is mixed solution of ethanol and acetic acid, volume ratio of ethanol to acetic acid is 9:1; Magnolia officinalis bark extract is obtained by refluxing Magnolia officinalis bark with 60% ethanol for 2h and concentrating under reduced pressure; Third solvent is mixed solution of ethanol aqueous solution and organic acid, volume fraction of ethanol in ethanol aqueous solution is 100%, organic acid is acetic acid, volume ratio of ethanol to acetic acid is 9:1.

[0035] Example 4 Oil-controlling and itching-relieving composition, which is composed of Magnolia officinalis bark extract, Crataegus monogyna Jacq. extract, Citrus limonum fruit peel extract, tea extract, Sophora japonica flower bud extract and Cnidium monnieri extract; composition is as follows in terms of weight parts: Magnolia officinalis bark extract 1 part, Crataegus monogyna Jacq. extract 3 parts, Citrus limonum fruit peel extract 0.2 part, tea extract 3 parts, Sophora japonica flower bud extract 2 parts and Cnidium monnieri extract 0.1 part. Its preparation method refers to Example 1.

[0036] Magnolia officinalis bark extract is obtained by molecularly imprinted polymerization method, and its preparation method refers to Example 1.

[0037] Example 5The oil-control and itching-relieving composition is composed of Magnolia officinalis bark extract, Malus prunifolia extract, Citrus limon fruit extract, Camellia sinensis extract, Sophora japonica flower bud extract and Cnidium monnieri extract; the composition is as follows in terms of weight parts: Magnolia officinalis bark extract 4 parts, Malus prunifolia extract 0.5 part, Citrus limon fruit extract 2 parts, Camellia sinensis extract 0.5 part, Sophora japonica flower bud extract 0.2 part and Cnidium monnieri extract 3 parts. The preparation method refers to Example 1.

[0038] The Magnolia officinalis bark extract is extracted by a molecular imprinting polymerization method, and the preparation method refers to Example 1.

[0039] Comparative Example 1 The oil-control and itching-relieving composition is different from Example 1 in that the Magnolia officinalis bark extract is extracted by an alcohol extraction method, and the process parameters are as follows: 70% ethanol, reflux for 1.5 hours and concentration under reduced pressure.

[0040] Comparative Example 2 The oil-control and itching-relieving composition is different from Example 1 in that the Magnolia officinalis bark extract is composed of 35% pure product and Magnolia officinalis bark extract.

[0041] Purity test of honokiol : The purity of Magnolia officinalis bark extract and Magnolia officinalis bark extract in Examples 1-5 and Comparative Examples 1-2 is tested by HPLC, C18 column, mobile phase A: water (containing 0.1% formic acid); mobile phase B: acetonitrile; gradient elution program: 0-5 min, B=10%; 5-15 min, B from 10% linearly rises to 70%; 15-18 min, B=70%; 18-22 min, B from 70% to 10%, balance. The flow rate is 1.0 mL / min, and the detection wavelength is 294 nm.

[0042] The test results are shown in Table 1.

[0043] Table 1 Purity of Magnolia officinalis bark extract and Magnolia officinalis bark extract

[0044] Application example Preparation of shampoo The shampoo formula is shown in Table 2.

[0045] Table 2 Shampoo formula

[0046] Note: the sum of the mass fractions of the components is 100%; The active substance is the oil-control and itching-relieving composition prepared by Example 1-3 or Comparative Example 1-2.

[0047] The preparation method of the above shampoo comprises the following steps: (1) Table active phase: dissolve and mix sodium laureth sulfate, ammonium lauryl sulfate and cocamidopropyl betaine at 75-85°C; (2) Pearl phase: dissolve and disperse glycol distearate at 75-85°C under heat and stirring; (3) Conditioning phase: pre-disperse quaternary ammonium salt-80, cocamide MEA, TEA-dodecylbenzenesulfonate, guar hydroxypropyltrimonium chloride, dimethicone and disodium EDTA, and then incorporate; (4) Add oil control and anti-itch composition, deionized water, and stir and disperse until uniform; (5) Adjust pH to 5.5-6.5 with citric acid; (6) Add fragrance, sodium chloride and phenoxyethanol to adjust viscosity, and filter to obtain the product.

[0048] Effect example : 1. Malassezia activity inhibition and scalp irritation score test The oil control and anti-itch composition prepared in Example 1, Comparative Example 1 and Comparative Example 2 was subjected to a Malassezia activity inhibition and scalp irritation score test.

[0049] In this test, Malassezia furfur ATCC standard strain was used as the test strain for determination.

[0050] Inhibition zone diameter: agar diffusion method. Spread the bacterial suspension on a Lioyd's agar plate, place an Oxford cup and add an equal amount of sample solution, incubate at 32°C for 5-7 days, and then measure the inhibition zone diameter (mm).

[0051] Minimum inhibitory concentration (MIC): micro broth dilution method. Dilute the sample in a 96-well plate with a series of concentration gradients, inoculate the bacterial solution and incubate for 5-7 days, and then observe the minimum concentration without bacterial growth with the naked eye as the MIC value (μg / mL).

[0052] Inhibition rate: quantitative killing test. After mixing the sample with the bacterial suspension for a specific time, count the viable bacteria, and calculate the inhibition rate = (control CFU - treatment CFU) / control CFU x 100%. All in vitro experiments were repeated at least 3 times (n=3).

[0053] Scalp irritation scoring test method: A randomized, single-blind design, n=30 / group. Scalp irritation reactions were assessed by a clinician using a 0-3 scoring scale, 0 = no visible irritation or reaction, 1 = mild erythema or mild pruritus (subjectively felt but does not interfere with daily activities), 2 = moderate erythema / obvious pruritus / mild edema (requires observation or brief treatment), 3 = severe erythema / obvious edema / pain / desquamation or requires medical treatment. Evaluation time points: baseline, week 1, week 2, week 4 of use. HRIPT time points: 24h, 48h of patching. Recording: Each assessment was recorded by the same standardized trained dermatologist, and if necessary, photographs were taken for archiving and reviewed by an independent reviewer. Calculation: The highest score for each subject for each reading was recorded, and the final result was the average score ± standard deviation for all subjects at all reading times.

[0054] The test results are shown in Table 3.

[0055] Table 3 Test results

[0056] Table 3 shows that the magnolol enriched by the molecular imprinting method in Example 1 of the present application has more significant performance in dandruff removal, antibacterial and scalp soothing compared with the Magnolia officinalis bark extract obtained by the same raw material alcohol extraction method in Comparative Example 1. The malassezia inhibitory activity of Example 1 of the present application is higher than that of Comparative Example 2 using 35% pure magnolol and active substances, and the scalp irritation is significantly reduced, which shows that under the same purity, the synergistic effect of the Magnolia officinalis bark extract prepared by the extraction method of the present application and the extract of Malus prunifolia, lemon peel, tea, sophora flower bud and cnidium fruit is more significant.

[0057] 2. Multidimensional efficacy evaluation test Multidimensional efficacy evaluation tests were conducted on the shampoos prepared by Examples 1-3 and Comparative Example 1.

[0058] Test design: Single-blind randomized grouping, n=30 / group; test period 4 weeks. Evaluation indexes include: ① Sebumeter to determine sebum excretion, reflecting oil regulation; ② Corneometer to determine the water content of the stratum corneum to obtain the moisturizing index; ③ Visioscan (VC20) skin texture detection analyzer was used to directly observe the dandruff morphology, distribution and quantity on the scalp surface, combined with the dandruff scoring standard, to calculate the dandruff removal rate; ④ Tewameter to determine the trans-epidermal water loss (TEWL) to analyze the relative change (%); ⑤Subjective scale score (7-point scale, evaluating tightness, refreshness, smoothness, etc.), each item is scored from 1 to 7 (1 = very bad / extremely uncomfortable, 7 = very good / completely no discomfort); comprehensive evaluation of refreshness, tightness, smoothness, etc. The use experience, all results are expressed as mean ± SD.

[0059] The test results are shown in Table 4.

[0060] Table 4 Multidimensional efficacy evaluation test results

[0061] Note: * indicates compared with Comparative Example 1, p <0.05.

[0062] Table 4 shows that the shampoo of the present application has significant advantages (p <0.05) in dandruff removal, moisturizing, oil control, soothing, etc. Compared with Comparative Example 1.

[0063] 3. Microecological detection test (high-throughput sequencing method) Microecological detection tests were conducted on the shampoos prepared by Example 1 and Comparative Examples 1-2.

[0064] The microbial community in the scalp samples of the volunteers was analyzed in depth by high-throughput sequencing, including beneficial bacteria, harmful bacteria, neutral bacteria, etc. The richness and distribution balance of the bacterial species were measured, and the imbalance mode of the bacterial community related to specific problems such as dandruff was identified. The test results are shown in Tables 5 and 6.

[0065] Table 5 Test results of Malassezia abundance change

[0066] Table 6 Test results of fungal alpha diversity

[0067] Table 5 shows that the shampoo formula of the present application reduces the abundance of Malassezia by more than 34%, and significantly promotes the rebound of epidermal resident beneficial bacteria (p <0.05). p<0.05 Comparative Example 1 has no significant improvement, and Comparative Example 2 has less improvement than Example 1.

[0068] Table 6 shows that the Shannon index and Simpson index of Example 1 are significantly higher than those of Comparative Examples 1 and 2, indicating that Example 1 can significantly improve the alpha diversity of the fungal community on the scalp and improve the balance of the community structure.

[0069] 4. Stability and safety test The shampoo prepared by Example 1 of the present application was subjected to stability and safety tests, and the test results showed that: (1) Stability: no phase separation, pH and viscosity change <10%, normal odor after 3 months at 40℃ / 75% RH and 3 freeze-thaw cycles at-5~45℃; (2) Safety: no obvious irritation after 24 / 48h (HRIPT negative), and the incidence of adverse reactions of volunteers was 0%, i.e. "no adverse reactions".

[0070] The above results all show that the oil control soothing composition is mild and safe, and has the remarkable effects of efficient oil control, dandruff removal, moisturization and soothing scalp.

[0071] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and not to limit it, and other modifications or equivalent replacements of the technical solutions of the present application made by those skilled in the art should be covered in the scope of the claims of the present application.

Claims

1. An oil control soothing composition characterized in that: The thick-bark extract, single-fruit hawthorn extract, lemon peel extract, tea extract, sophora flower bud extract and cnidium fruit extract are compounded to form, and the weight parts of each component are as follows: thick-bark extract 1-4 parts, single-fruit hawthorn extract 0.5-3 parts, lemon peel extract 0.2-2 parts, tea extract 0.5-3 parts, sophora flower bud extract 0.2-2 parts, and cnidium fruit extract 0.1-3 parts.

2. The oil control soothing composition of claim 1, wherein: The preparation method of the thick-bark extract comprises the following steps: Step a: mixing a pseudo-template molecule, a functional monomer, a crosslinking agent, an initiator and a first solvent, polymerizing at 40-60°C under nitrogen protection for 6-8 hours to obtain a molecularly imprinted polymer; Step b: recycling eluting the molecularly imprinted polymer to HPLC template peak disappearance by using a second solvent; Step c: mixing thick-bark crude extract and the molecularly imprinted polymer treated in step b, and oscillating at room temperature for 1-3 hours; Step d: selectively eluting the extract obtained in step c by using a third solvent to obtain the thick-bark extract.

3. The oil control soothing composition of claim 2, wherein: In step a, the pseudo-template molecule is 5,5'-dipropyl-2,2'-diphenol; The functional monomer is methacrylic acid or acrylamide or 4-vinylpyridine, and the molar ratio of the pseudo-template molecule to the functional monomer is 1:(4-6); The crosslinking agent is divinylbenzene or ethylene glycol dimethacrylate or TRIM, and the molar ratio of the sum of the moles of the pseudo-template molecule and the functional monomer to the crosslinking agent is 1:(20-30); The initiator is azobisisobutyronitrile, and the amount is 0.5-1.5wt% of the functional monomer; The first solvent is a mixed solution of acetonitrile and toluene, and the volume ratio of acetonitrile to toluene is 1:

1.

4. The oil control soothing composition of claim 3, wherein: In step b, the second solvent is a mixed solution of ethanol and acetic acid, and the volume ratio of ethanol to acetic acid is 9:

1.

5. The oil control soothing composition of claim 4, wherein: In step c, the thick-bark crude extract is an extract obtained by reflux extraction of thick-bark with ethanol.

6. The oil control soothing composition of claim 5, wherein: In step d, the third solvent is a mixed solution of an ethanol aqueous solution and an organic acid, the volume fraction of ethanol in the ethanol aqueous solution is 95-100%, the organic acid is acetic acid, and the volume ratio of ethanol to acetic acid is 9:

1.

7. The method of making an oil control soothing composition according to claim 6, wherein: The method comprises the following steps: Step 1: mixing the thick-bark extract, single-fruit hawthorn extract and cnidium fruit extract and stirring uniformly to obtain a mixture; Step 2: adding the lemon peel extract, tea extract and sophora flower bud extract to the mixture and stirring uniformly to obtain an oil-controlling soothing composition.

8. Application of the oil-controlling soothing composition of any one of claims 1-6 or the oil-controlling soothing composition obtained by the preparation method of claim 7 in a hair product, wherein the hair product comprises a scalp serum, a hair conditioner, a hair mask, and a shampoo.

9. Use of the oil control soothing composition according to claim 8 in a hair product, characterized in that: The mass fraction of the oil-controlling soothing composition in the hair product is 2-12%.

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