Platycladus orientalis leaf extract for natural cosmetics, preparation method and shampoo containing same

Abstract

The invention provides a Platycladus orientalis leaf extract for natural cosmetics, a preparation method and a shampoo containing the extract, relating to the field of natural raw material extraction. The extract is a transparent solution at room temperature and has a precipitate at low temperature. The main components of the extract include secondary metabolite compounds that are soluble in CO2 and water, including volatile oil, α-thujone, thujene and alkaloids. The extraction method is a subcritical CO2 extraction method combined with a hand soap mist washing and absorption process, which improves the extraction rate of the Platycladus orientalis leaves, increases the content of alkaloids, and reduces the content of oil and wax. The extract can be effectively used in shampoo, and the extract is in liquid form, which is completely different from traditional extracts that are in a paste form.

Description

Technical Field

[0001] The present application belongs to the technical field of natural raw material production of cosmetics, and specifically relates to a Platycladus orientalis leaf extract for natural cosmetics, a preparation method, and a shampoo containing the extract. Background Art

[0002] Natural cosmetics refer to cosmetics developed using ingredients extracted from natural plant extracts. Currently, my country's cosmetics regulations explicitly encourage and support the use of modern science and technology, combined with traditional Chinese advantages and unique plant resources, in the research and development of cosmetics. Consequently, the use of natural plant extracts in high-end cosmetics is gaining increasing popularity and recognition among consumers.

[0003] As is known to all, Chinese herbal medicines contain nutrients such as saponins, polysaccharides, flavonoids, alkaloids and trace elements that are needed by the skin. When using Chinese herbal skin care products, the medication can be adjusted according to skin symptoms, so as to better exert the therapeutic effect under the premise of safety. Chinese herbal skin care products are rare in terms of allergies because the ingredients they contain are "homologous" to the body and will not be treated as "enemies" by the immune system. Therefore, they are also very friendly to people with sensitive skin. Therefore, more and more cosmetics companies, including some well-known foreign cosmetics brands, are committed to discovering various natural compounds or effective parts with significant efficacy from Chinese herbal medicines, and developing a batch of functional cosmetics with independent intellectual property rights. Based on the concept of attaching importance to natural, green and biosafety in the field of cosmetics, this application provides an extract of Chinese herbal medicine with the effect of promoting hair growth and blackening hair and its preparation process, in response to the prominent problems of gray hair and hair loss in middle-aged and elderly people.

[0004] Platycladus orientalis leaves are the dried branches and leaves of Platycladus orientalis (L.) Franco, a plant of the Cupressaceae family. They are bitter and astringent, with a slightly cold nature. They enter the lung, liver, and large intestine meridians, and have the effects of cooling blood and stopping bleeding, resolving phlegm and relieving coughs, and promoting hair growth and darkening. According to "Sun Zhenren's Food Taboos," drying Platycladus orientalis leaves in the shade, grinding them into powder, and applying them with sesame oil can promote hair growth. According to "New Medicine," applying an ethanol-soaked solution of fresh Platycladus orientalis leaves to areas of hair loss can treat hair loss, resulting in new hair that is black and shiny. Therefore, Platycladus orientalis leaves are a rare natural cosmetic ingredient for hair care and growth, worthy of further research and development.

[0005] Currently, a number of technologies are used to prepare and mass-produce extracts from Platycladus orientalis leaves. It's well known that different extraction processes applied to the same medicinal material yield natural products with varying properties, composition, and efficacy. Due to the significant differences in quality and efficacy, these products represent distinct forms—"one ingredient, multiple products." The advantage of this "one ingredient, multiple products" approach is that it provides a diverse array of new raw materials for cosmetics research and development, fostering a new trend of technological advancement characterized by "multiple uses of one ingredient" and "innovation through the old."

[0006] Patent CN201010181979 discloses a Platycladus orientalis leaf extract and its preparation method, characterized by including drying, crushing, screening, acetone extraction, filtration, filtrate combination, concentration, and refrigeration. The resulting Platycladus orientalis leaf extract can be used as a plant inducer for protecting Cucurbitaceae crops against downy mildew. Patent "A Preparation Method and Process for Platycladus orientalis Leaf Extract" discloses another similar method for producing Platycladus orientalis leaf extract, which includes microwave-assisted steam distillation, macroporous resin adsorption, elution with ethanol solution, concentration, polyamide resin adsorption and elution, and subsequent purification by recrystallization to produce the Platycladus orientalis leaf extract. This technology is characterized by a complex process and low yield. It is acceptable for scientific research, but not suitable as a cosmetic raw material. Wang Jun et al. studied a supercritical extraction method for terpene compounds from Platycladus orientalis leaves [Analytical Instruments, Issue 6, 2011, p. 85]. This study shows that the products of supercritical CO2 extraction of Platycladus orientalis leaves are mostly relatively polar, high-molecular-weight compounds, which has certain extraction limitations. Using anhydrous ethanol as an entrainer can improve the extraction yield of natural products, but increasing the entrainer significantly increases the impurities in the extract. This suggests that a simple supercritical CO2 extraction process is incomplete in extracting the active ingredients from Platycladus orientalis leaves, leaving flavonoids in the raffinate. Furthermore, the transfer rate of alkaloids in the supercritical fluid extract of Platycladus orientalis leaves is also quite low.

[0007] In addition, patent CN201811391260.0 discloses a method for preparing an ethanol extract of Platycladus orientalis leaves, characterized in that Platycladus orientalis leaf powder is used as raw material, 50%, 70%, and 95% ethanol is used as solvent, and the extract is filtered under reduced pressure. The filtrate is placed in an evaporating dish and concentrated in a 70°C water bath to a dry extract. Patent CN101550081A relates to an effective component of Platycladus orientalis leaves and its preparation method and use. The preparation process includes the following steps: extracting Platycladus orientalis leaves with a mixture of ethyl acetate and ethanol as a solvent, subjecting the extract to chromatographic column chromatography to obtain an eluent, and performing preparative liquid chromatography gradient elution to obtain the eluent, with the mobile phase being water and acetonitrile. The eluents at different time periods are collected to obtain the effective component. Patent CN202111510576.9 discloses a method for preparing a Platycladus orientalis leaf extract and a shampoo, characterized in that the method comprises the following steps: heating the Platycladus orientalis leaf for extraction, filtering, and concentrating under reduced pressure to obtain a concentrated extract; subjecting the concentrated extract to macroporous resin adsorption, sequentially eluting with deionized water and ethanol solution, and concentrating under reduced pressure to obtain a crude Platycladus orientalis leaf extract; drying, dissolving, settling, filtering, and concentrating the filtrate, settling, centrifuging, and discarding the supernatant to obtain a Platycladus orientalis leaf extract. The characteristics of these two technologies are that the process is complicated, the production cost is high, and the yield of effective substances is low, which is very unfavorable for the development of cosmetic raw materials. Summary of the Invention

[0008] (1) Technical problems solved

[0009] In view of the shortcomings of the existing technology, the present invention solves the above problems by using subcritical CO2 as the extraction medium and aqueous solution as the absorbent, thereby achieving the characteristics of liquidization of Platycladus orientalis leaf extract at room temperature, less impurities, and high content of effective substances.

[0010] (2) Technical solution

[0011] To achieve the above objectives, the present invention proposes a first solution:

[0012] A Platycladus orientalis leaf extract for natural cosmetics is a transparent solution at room temperature and produces a precipitate at low temperature. The main components of the extract have secondary metabolite compounds that are soluble in CO2 and water, including volatile oil, α-thujone, thujene and alkaloids.

[0013] The extract becomes transparent without precipitation after being stored at 20-45°C for 24 hours, and becomes turbid after being stored at 0-5°C for 24 hours. At room temperature, it is a transparent aqueous solution suitable for direct addition to cosmetics.

[0014] The volatile oil content ranges from 0.15% to 2.0%, and the alkaloid content is not less than 0.08%; the concentration of the active ingredient is appropriate to ensure that it achieves its due efficacy, and the alkaloid content enhances the effect of hair growth and darkening, and the preferred range is 0.15% to 0.30%.

[0015] The fat content of the solid matter after drying the extract does not exceed 5%. The fat-soluble components of the macromolecules in the Platycladus orientalis leaf extract should be effectively controlled, and the waxy compounds are not fully extracted.

[0016] In order to achieve better extraction, the present invention proposes a second solution:

[0017] A method for preparing a Platycladus orientalis leaf extract for natural cosmetics comprises the following steps:

[0018] S1: Extraction: Place the crushed Platycladus orientalis leaves in an extraction column and extract the active ingredients in parallel with subcritical CO2;

[0019] S2: Absorption: The subcritical CO2 fluid is heated, enters the absorption tower, undergoes water mist countercurrent interaction, and finally enters the aqueous solution for absorption;

[0020] S3: Repeat: The subcritical CO2 fluid after the countercurrent interaction of water mist is cooled, the temperature and pressure are reduced, and it reaches the recovery tank, and then pressurized to enter the extraction column to extract the effective components.

[0021] The main process parameters for the extraction and absorption of Platycladus orientalis leaves are: an extraction pressure of 12-15 MPa and an extraction temperature of 40-50°C in step S1; an absorption pressure of 8-10 MPa and an absorption temperature of 45-50°C in step S2. An absorbent is added in step S3; the absorbent is a mixture of pure water and protonated active water, with a weight ratio of pure water to protonated active water ranging from 8 to 10:1.

[0022] Protonated active water is an entrainer for subcritical extraction, which helps some weakly polar compounds dissolve in CO2, thereby improving the extraction efficiency of active ingredients, increasing the molecular diversity of Platycladus orientalis leaf extract, and overcoming the defect of the existing SFE process that is limited to the extraction of fat-soluble compounds.

[0023] It is also an absorbent, cleverly transferring the active ingredients from CO2 into the solution while removing some large molecular fat-soluble compounds.

[0024] The protonated active water used in this process is the cosolvent of alkaloids. + Combined with the alkaloids contained in Platycladus orientalis leaves, it increases the solubility of alkaloids in CO2 water and solution, thereby improving the efficiency of alkaloid extraction.

[0025] In order to achieve better application, the present invention proposes a third solution:

[0026] A natural raw material shampoo containing Platycladus orientalis leaf extract comprises 50 parts of the Platycladus orientalis leaf extract for natural cosmetics described in the first embodiment, 3 parts of sapindus mukorossi saponins (80%), 1 part of honeysuckle flower extract, 1 part of ginseng extract, 1 part of Polygonum multiflorum extract, 0.7 parts of cinnamon essential oil, and 0.3 parts of lavender essential oil. The mixed preparation has the effect of replenishing qi and blood, and can promote microcirculation in the head, with a more obvious effect.

[0027] (3) Beneficial effects

[0028] The invention has the characteristics of high extraction rate, high alkaloid content, few impurities, etc., and the extract is soluble in both CO2 and water. The extract is a transparent liquid at room temperature and produces precipitation when placed at 0-5°C for 24 hours. The process is simple to produce. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a process flow chart of the present invention;

[0030] Figure 2 Schematic diagram of the subcritical CO2 extraction and countercurrent absorption linkage operation device of the present invention;

[0031] Figure 3 This is a diagram of the supercritical CO2 extraction device;

[0032] Figure 4 Diagram of the apparatus for distillation extraction. DETAILED DESCRIPTION

[0033] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0034] Example 1:

[0035] like Figure 1 、 Figure 2 As shown, 15.8 kg of Platycladus orientalis leaves are crushed and placed in an extraction column. Subcritical CO2 is heated and pressurized and then introduced into the extraction column. The temperature is controlled at 40-50 ° C and the pressure is controlled at 12-15 MPa. Then, the subcritical CO2 with the extract enters a heat exchanger to adjust the pressure and temperature, and enters an absorption tower with an absorption pressure of 8-10 MPa and an absorption temperature of 45-50 ° C. The absorption tower is equipped with a water mist elution device to elute the subcritical CO2. The eluent is a mixture of pure water and protonated active water. The pure water is 8 kg and the protonated active water is 1 kg. The absorbent is pure water (produced by Wahaha Company). and protonated active water (high concentration, provided by Hangzhou Shanshangshui Technology Co., Ltd.), through the absorption of the mixture, the absorbed subcritical CO2 enters the recovery tank, and then the subcritical CO2 is pressurized and heated through a booster pump and a heat exchanger. The temperature is controlled at 40-50°C and the pressure is controlled at 12-15MPa, and then enters the extraction column again to realize the circulation of subcritical CO2 in the system, thereby realizing the transfer of effective substances in the Platycladus orientalis leaves from the medicinal materials to the aqueous solution. The experiment is carried out for 5 hours, and 7.2-8.0KG of absorption liquid is obtained. The absorption liquid is a brown transparent liquid with a faint unique fragrance of Platycladus orientalis leaves.

[0036] Among them, the content of Platycladus orientalis leaf extract is 0.9-1.2kg, the content of Platycladus orientalis leaf volatile oil is 12-14%, and the content of alkaloids is 1.8-2.2%.

[0037] In this example, the volatile oil content of medicinal materials and extracts was determined according to the method in the appendix "Determination of Volatile Oils" of the 2015 edition of the Chinese Pharmacopoeia. The alkaloid content of Platycladus orientalis leaf extract was analyzed using an acid dye colorimetric method. The dye used was 0.001 mol / L bromothymol blue, the standard was betaine, and the buffer was acetic acid-sodium acetate buffer.

[0038] For the above extraction method, this applicant has designed an extraction system, including a CO2 storage tank, an extraction column, a first heat exchanger, an absorption tower, a water mist scrubber, a cooler, a recovery tank, a booster pump, and a second heat exchanger, along with necessary accessories such as piping, valves, thermometers, and pressure gauges. The extraction column has a capacity of 24L, with a height-to-diameter ratio of 5:1; the absorption tower has a volume of 200L. The system is designed for a pressure of 18MPa, with an actual operating pressure of no more than 15MPa.

[0039] The above extracts were subjected to experiments as follows:

[0040] Three 20ml portions of the extract were taken and placed into volumetric flasks (A, B, and C). Flask A was placed in a 0-5°C low-temperature oven, flask B was placed in a 45°C constant-temperature oven, and flask C was kept at room temperature (20-25°C). After 24 hours, the extracts were taken out and compared. A small amount of precipitate was visible in flask A, while flasks B and C were transparent. These test results indicate that the concentration of the extract solution obtained in Example 1 meets the requirements for cosmetic development.

[0041] Comparative Example 1:

[0042] The supercritical CO2 extraction experiment of Platycladus orientalis leaves. The experimental device for supercritical fluid extraction of Platycladus orientalis leaves is as shown in the attached figure. Figure 3 As shown, the system mainly includes a CO2 cylinder, a condenser, a metering plunger pump (with adjustable flow), a co-solvent feeding pump, a circulation heater, an extraction kettle (1000 mL), two separation kettles (Separation I and Separation II), and a gas flowmeter. When extracting Platycladus orientalis leaves, the crushed Platycladus orientalis leaves are first added to the extraction kettle, and the entire system is sealed. The temperature control is turned on to ensure that the temperatures of the extraction kettle and separation kettle reach the set values, and then the CO2 system is started. The CO2 reaches the condenser (liquid state) through vaporization, filtration, and condensation. The liquid CO2 is pressurized by the metering plunger pump and heated by the heater, and enters the extraction kettle in a supercritical fluid state. After the CO2 completes the extraction in the extraction kettle, it flows through Separation Kettle I and Separation Kettle II in sequence, where the pressure is reduced to precipitate the extract. The CO2, after decompression in the separation kettle, enters the filter again and is recycled. The extract product is collected from the separation kettle at regular intervals during the extraction process.

[0043] The comparative test used 3 kg of Platycladus orientalis leaves and collected 352 g of the extract, which was a brown paste. Analysis showed that the extract contained 3.20% volatile oil, 13.65% solid oil, and 0.02% alkaloids.

[0044] Comparative Example 2:

[0045] The experimental device for extracting volatile oil from Platycladus orientalis leaves is as shown in the attached figure. Figure 4As shown. Accurately weigh 200g of Platycladus orientalis leaves and mix with distilled water at a material-to-liquid ratio of 1:8 (w / v). Place in a 5000mL round-bottom flask, add a distilled water solution containing 5% sodium chloride, and let it stand for 4 hours. Connect the experimental apparatus and add distilled water from the condenser to the scale of the measuring instrument until it overflows into the distillation flask. Heat with an electric heating mantle, maintaining a slight boiling state for varying periods of time during extraction. Extract for a total of 3 hours, then stop heating.

[0046] At the end of the experiment, 4.12 mL of essential oil was collected from the extractor, with a yield of 1.90% of volatile oil from the leaves of Platycladus orientalis. Analysis showed that the contents of flavonoids and alkaloids in the leaves of Platycladus orientalis were both less than 0.01%.

[0047] The product obtained by this process can provide another solution: a natural raw material shampoo containing Platycladus orientalis leaf extract, characterized by comprising 50 parts Platycladus orientalis leaf extract of Example 1, 3 parts Sapindus mukorossi saponins (80%), 1 part Honeysuckle extract, 1 part Ginseng extract, 1 part Polygonum multiflorum extract, 0.7 parts Cinnamon essential oil, and 0.3 parts Lavender essential oil. Traditional Chinese Medicine believes that the primary cause of hair loss lies in the kidneys. If both the liver and kidneys are deficient in Qi and blood, blood circulation throughout the body weakens, unable to transport nutrients to the top of the head, the highest point of the human body. Hair follicles on the head are deprived of nourishment and gradually atrophy, causing hair loss. This product has the effect of replenishing Qi and blood, promoting microcirculation in the head, and achieving the effects of darkening and promoting hair growth. Usage: Apply 10-20 ml of the natural shampoo to hair, stir by hand until evenly distributed throughout the hair and lathering. After three minutes, rinse with clean water. Generally, use the natural shampoo every 2-3 days. When washing your hair, you need to rub and massage it, which can not only keep your scalp clean but also invigorate the blood circulation. If you persist for more than 30 days, you will see the effect of hair growth.

[0048] Compared with supercritical extraction, although the extraction rate of this process is 5%-8% and that of supercritical extraction is 10%-12%, the extract of this process contains less oil and wax and more alkaloids. The alkaloid content increases from 0.02% in supercritical extraction to 1.8-2.2% in this process. Compared with distillation extraction, the extraction rate of this process increases from 1.2-2.5% in distillation to 5-8%, and the alkaloid content also increases from less than 0.01% in distillation to 1.8-2.2%.

[0049] The extract obtained by this process has the following advantages over the supercritical extraction process: the extract obtained by this process is a transparent liquid at room temperature, while the extract obtained by the supercritical process is a brown paste, which is not conducive to later applications.

Claims

1. A Platycladus orientalis leaf extract for natural cosmetics, characterized in that: It is a transparent solution at room temperature and has a precipitate at low temperature. Its main components are secondary metabolites that are soluble in CO2 and water, including volatile oils and alkaloids. The preparation method includes the following steps: S1: Extraction: Place the crushed Platycladus orientalis leaves in an extraction column, extract the active ingredients using subcritical CO2 in parallel at an extraction pressure of 12-15 MPa and a temperature of 40-50°C. S2: Absorption: The subcritical CO2 fluid is heated and enters the absorption tower, where it undergoes countercurrent interaction with water mist and finally enters the aqueous solution for absorption. The absorption pressure is 8 to 10 MPa and the absorption temperature is 45 to 50°C. In this step, an absorbent is added. The absorbent is a mixture of pure water and protonated active water. The weight ratio of pure water to protonated active water ranges from 8 to 10:

1. The protonated active water is a cosolvent for the alkaloids. S3: Repeat: The subcritical CO2 fluid after the countercurrent interaction of water mist is cooled, the temperature and pressure are reduced, and it reaches the recovery tank, and then pressurized to enter the extraction column to extract the effective components.

2. The Platycladus orientalis leaf extract for natural cosmetics according to claim 1, characterized in that The extract becomes transparent without precipitation after being placed at 20-45°C for 24 hours, and becomes turbid after being placed at 0-5°C for 24 hours.

3. The Platycladus orientalis leaf extract for natural cosmetics according to claim 1, characterized in that The fat content of the dry solids of the extract does not exceed 5%.

4. A natural raw material shampoo containing Platycladus orientalis leaf extract, characterized in that: The invention comprises 50 parts of the Platycladus orientalis leaf extract for natural cosmetics according to any one of claims 1 to 3, 3 parts of sapindus saponins with a content of 80%, 1 part of honeysuckle extract, 1 part of ginseng extract, 1 part of Polygonum multiflorum extract, 0.7 parts of cinnamon essential oil, and 0.3 parts of lavender essential oil, and the above components are mixed.

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