Preparation method and application of polianthes tuberosa moisturizer
Through nano-liposome encapsulation and gradient temperature-controlled emulsification processes, the problem of low oxidation and absorption of tuberch active ingredients is solved, forming a stable moisturizer, achieving efficient skin moisturizing and barrier repair effects, and is suitable for cosmetics.
Patent Information
- Application Number
- CN202510911670.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-02
- Publication Date
- 2025-08-15
AI Technical Summary
In the prior art, the active ingredients of tuberch jade are prone to oxidation, have low transdermal absorption, and conventional emulsification processes lead to insufficient stability of moisturizers, and there are stratification and oil extraction phenomena.
Nanoliposome encapsulation technology and gradient temperature-controlled emulsification process are used to prepare oil and aqueous phases, combining gradient homogenization and low-temperature addition to form a stable O/W emulsion. Nanoliposomes provide oxygen isolation, gradient homogenization controls particle size and phase transformation, and a composite moisturizing network is formed using ceramide III and trehalose in combination.
It significantly improves the stability and bioavailability of the active ingredients of tuberwood, enhances transdermal absorption, and achieves skin moisturizing, barrier repair and whitening effects. It has excellent product stability and user experience, and is suitable for large-scale production.
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of cosmetic preparation, and in particular to a preparation method and application of a tuberose moisturizing cream. Background Art
[0002] Tuberose, a traditional botanical skincare ingredient, boasts excellent moisturizing, antioxidant, and whitening properties thanks to its volatile oils and flavonoids. However, existing methods of directly adding tuberose extract to cosmetics present issues such as oxidative decomposition of active ingredients and low transdermal absorption. Moisturizers prepared using conventional emulsification processes often exhibit stratification and oil separation, resulting in inadequate product stability.
[0003] Currently, most commercially available moisturizers containing plant-based active ingredients utilize high-temperature emulsification processes, which can easily inactivate heat-sensitive substances. While some technologies utilize microencapsulation, these technologies fail to address the issue of controlled release of active ingredients during the emulsification process. Achieving efficient delivery and stable storage of active ingredients through process innovation remains a pressing technical challenge in this field. Summary of the Invention
[0004] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid obscuring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.
[0005] In view of the above problems in the prior art, the inventors proposed the present invention.
[0006] Therefore, the object of the present invention is to overcome the deficiencies in the prior art and provide a preparation method and application of a tuberose moisturizing cream.
[0007] To solve the above technical problems, the present invention provides the following technical solutions: A method for preparing a tuberose moisturizing cream, comprising: (a) preparing an oil phase: melting and mixing glyceryl stearate, squalane, and ceramide III at 75-80°C, adding tuberose nanoliposomes, and stirring while maintaining the temperature; (b) Preparation of aqueous phase: Dissolve glycerol, trehalose, and panthenol in deionized water and heat to 75-80°C; (c) Primary emulsification: Slowly add the aqueous phase to the oil phase at a rate of 0.5-1 mL / s and homogenize at 2000 rpm for 5 minutes; (d) Gradient homogenization: first homogenize at 5000 rpm for 8 min, then homogenize at 8000 rpm for 3 min; (e) Cooling and adding: cooling the emulsion to below 45°C, and adding tuberose volatile oil and baicalin; (f) Vacuum degassing: Degas the mixture by stirring at a vacuum degree of -0.08 MPa for 20 minutes.
[0008] As a preferred embodiment of the method for preparing a tuberose moisturizing cream described in the present invention, the tuberose nanoliposomes are prepared by the following steps: dissolving lecithin and cholesterol in chloroform at a mass ratio of 4:1, rotary evaporating to form a thin film, adding phosphate buffer containing 0.5 wt% of total tuberose flavonoids, and hydrating and ultrasonicating to obtain liposomes with a particle size of 80-100 nm.
[0009] As a preferred embodiment of the method for preparing the tuberose moisturizing cream of the present invention, the oil phase component comprises, by mass percentage, 8-12% glyceryl stearate, 5-8% squalane, and 1-3% ceramide III; and the aqueous phase component comprises 4-6% glycerol, 1.5-4% trehalose, and 0.5-1.5% panthenol.
[0010] As a preferred embodiment of the method for preparing the tuberose moisturizing cream of the present invention, the system temperature is maintained at 75±2° C. during the gradient homogenization process in step (d).
[0011] As a preferred embodiment of the method for preparing the tuberose moisturizing cream of the present invention, the tuberose volatile oil in step (e) is purified by molecular distillation, wherein the content of phenylethyl alcohol esters is not less than 85%.
[0012] A tuberose moisturizing cream comprises the following components by mass percentage: 0.5-2% tuberose nanoliposomes, 1-3% ceramide III, 1.5-4% trehalose, and 0.1-0.5% baicalin.
[0013] As a preferred embodiment of the tuberose moisturizing cream described in the present invention, the invention further comprises the following steps:
[0014] As a preferred solution of the preparation method and application of the tuberose moisturizing cream of the present invention, the moisturizing cream is an O / W emulsion with an average particle size of 120-150 nm and a polydispersity index (PDI) ≤0.2.
[0015] The invention provides an application of the tuberose moisturizing cream in the preparation of skin moisturizing care products.
[0016] The invention provides an application of the tuberose moisturizing cream in the preparation of skin barrier repair products.
[0017] The invention provides an application of the tuberose moisturizing cream in the preparation of a whitening skin care product that inhibits tyrosinase activity.
[0018] Beneficial effects of the present invention: The present invention significantly improves the stability and bioavailability of tuberose active ingredients through the synergistic effect of nanoliposome encapsulation technology and gradient temperature-controlled emulsification process. The nanoliposome bilayer structure effectively isolates oxygen and prevents oxidation of flavonoids; the fine emulsion droplets formed by the gradient homogenization process enhance transdermal absorption while also improving the physical stability of the emulsion. Ceramide III and trehalose in the product form a composite moisturizing network that synergistically strengthens the skin's barrier function. The combination of baicalin and tuberose active ingredients inhibits tyrosinase activity, achieving multiple skin care benefits. This preparation method is simple to operate and suitable for large-scale production, addressing technical drawbacks of traditional processes such as high loss of active ingredients and easy product stratification. DETAILED DESCRIPTION
[0019] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.
[0020] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0021] Secondly, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it designate a separate or selective embodiment that is mutually exclusive with other embodiments.
[0022] Example 1 This embodiment provides a preparation method and application of tuberose moisturizing cream. Specifically, the basic formula is prepared Specifically, the raw material formula (by weight percentage) oil phase components: Glyceryl stearate 10%, specifically, using cosmetic grade raw materials with a melting point of 55-60°C; Squalane 6%, preferably ultra-pure squalane of plant origin; Ceramide III 2%, further, synthetic ceramide with a purity of ≥98%; Aqueous phase components: Glycerol 5%, as an embodiment, double-distilled refined glycerin is used; Trehalose 3%, specifically, α,α-trehalose with a molecular weight of 342.3 Da; Panthenol 1%, preferably in the form of D-panthenol; The balance is deionized water, further, the resistivity is ≥ 15 MΩ·cm; Functional additives: Tuberose nanoliposomes 1.2%, specifically, encapsulation efficiency ≥92%; Tuberose volatile oil 0.8%, preferably purified by molecular distillation, phenylethyl alcohol content ≥ 85%, Baicalin 0.3%, further derived from Scutellaria root extract, purity ≥ 90%, Detailed implementation of the preparation process: The specific steps are as follows: Dissolve lecithin and cholesterol in chloroform at a mass ratio of 4:1, preferably, 8 g lecithin + 2 g cholesterol + 40 mL chloroform; The film was formed by rotary evaporation, and further, the film was evaporated under reduced pressure at 60 °C until a uniform film was formed; Add 100 mL of PBS buffer (pH 7.4) containing 0.5% total flavonoids from tuberose and hydrate at 55°C for 30 minutes; Ultrasonic treatment (200W, 10 minutes) was performed to obtain liposomes with an average particle size of 85.3 nm. As an embodiment, high-pressure homogenization can also be used instead of ultrasonication; The gradient emulsification process of the moisturizing cream is preferably implemented as follows: Melting of oil phase: melt glyceryl stearate, squalane and ceramide III at 80°C, add the nanoliposome suspension and stir for 15 minutes at a stirring rate of 300 rpm; Aqueous phase dissolution: dissolve glycerol, trehalose, and panthenol in deionized water and stir at 80°C until completely dissolved (further, the dissolution time should be ≥20 minutes); Primary emulsification: inject the water phase into the oil phase at a rate of 0.8 mL / s and homogenize at 2000 rpm for 5 minutes (maintain the temperature at 78 ± 1 °C) Gradient homogenization: The first stage: homogenization at 5000 rpm for 8 minutes, preferably, the temperature is controlled at 76±1°C; Second stage: homogenization at 8000 rpm for 3 minutes, specifically, shear force ≥ 12,000 s⁻¹; Low temperature addition: cooling to 45°C, adding tuberose essential oil and baicalin, and further, using a propeller stirrer at a speed of 150 rpm; Vacuum degassing: degassing at -0.08MPa vacuum for 20 minutes. As an implementation method, ultrasonic degassing can be added; Product Characterization and Effect Data Physical stability: no delamination in centrifugal test (4000rpm / 30min), viscosity 12,500cP (25℃) Microstructure: average particle size of emulsion 142nm, PDI=0.19 Efficacy verification: After 30 subjects used it for 4 weeks, the skin moisture content increased by 40.2%.
[0023] Example 2 This embodiment provides a preparation method and application of a tuberose moisturizing cream. The specific highly moisturizing and repairing formula is based on Example 1, with the following preferred adjustments: Ceramide III increased to 2.5%, specifically, enhancing barrier repair function; Trehalose is increased to 3.5%, preferably, to form a glassy protective film; Add 1% sodium hyaluronate, further, molecular weight 80-100kDal; Added 0.5% asiaticoside as an embodiment, using a standardized extract with ≥40% madecassoside; Aqueous phase cross-linking modification, specifically: adding sodium hyaluronate and a cross-linking agent 1,4-butanediol diglycidyl ether (0.1%) during the aqueous phase dissolution stage at 80°C, and keeping the reaction warm for 1 hour. Preferably, the cross-linking density is controlled to 15-20 cross-linking points / chain; Gradient homogenization parameter adjustment: 2000 rpm / 5 min → 5000 rpm / 10 min → 8000 rpm / 5 min. Furthermore, the temperature fluctuation in each stage was ≤2°C. Stepwise cooling addition strategy: baicalin was added at 50°C (to avoid thermal degradation); Add asiaticaside and tuberose essential oil at 45° C., specifically, the essential oil addition rate is ≤0.5 mL / min; Validation data and mechanism analysis Skin barrier function: TEWL value decreased by 38.9%; Anti-inflammatory effect: In vitro fibroblast experiments showed that TNF-α expression was downregulated by 67%; Low temperature stability: No oil-water separation after -15℃ / 24h freeze-thaw cycle. Preferably, 0.2% xanthan gum can be added to improve cold resistance.
[0024] Example 3 This embodiment provides a preparation method and application of a tuberose moisturizing cream, specifically, a whitening and anti-aging formula: The content of tuberose nanoliposomes increased to 1.5%, specifically, the loading capacity increased to 0.8 mg flavonoids / g liposomes; Add 0.2% of fat-soluble VC derivative (VC-IP), preferably a licensed raw material from Japan Co., Ltd.; Added collagen tripeptide 0.4%, further, molecular weight 500Da, Gly-Pro-Hyp sequence ≥95%; Baicalin is increased to 0.4%; as an embodiment, it synergistically inhibits tyrosinase with VC-IP; Programmable temperature control adding system: VC-IP was added at 45°C, specifically, pre-dissolved in 5% propylene glycol; Add collagen tripeptide at 40°C, preferably to avoid thermal denaturation of the peptide chain; Tuberose essential oil was added at 38°C, and nitrogen was injected for protection; Vacuum degassing enhancement: primary degassing: -0.08MPa / 20min Secondary treatment: 40kHz ultrasonic assisted for 5 minutes, preferably with a power density of 0.5W / cm³; Comparative experiments and mechanism of action Detection indicators This embodiment Competitive products on the market Principle of action Tyrosinase inhibition rate 81.3% 52.7% Flavonoid-VC-IP complex blocks the enzyme active center Collagen production +155% +68% Collagen tripeptide activates TGF-β pathway in fibroblasts Active ingredient retention rate (45℃ / 90 days) 94.2% 70.5% Nanoliposomes block oxygen permeation Transdermal absorption rate (8h) 62.4μg / cm² 29.7μg / cm² Small particle size lotion promotes hair follicle delivery In summary, the core innovation of the technical system of the tuberose moisturizing cream described in the present invention lies in the construction of a three-in-one technical path of "active ingredient protection - emulsion structure optimization - synergistic enhancement of efficacy". Through the gradient implementation of Examples 1-3, the implementation mechanism of this technical path is fully revealed. Specifically, the nanoliposome encapsulation technology of the tuberose active ingredient fundamentally solves the problem of flavonoids being easily oxidized and inactivated. The phospholipid structure of the liposome bilayer forms a natural oxygen barrier, and the dense area formed by the directional arrangement of its hydrophobic tail chains can effectively block the penetration of oxygen molecules; at the same time, the hydrophilic cavity stabilizes the phenolic hydroxyl groups in the flavonoid molecules through hydrogen bonding, achieving active protection from the dual dimensions of physical isolation and chemical stability. This protection mechanism was verified in the accelerated stability test of Example 3 - even after 90 days of high-temperature storage, the activity retention rate still exceeded 94%, which is far better than the direct addition method of conventional emulsions.
[0025] The innovative nature of the gradient temperature-controlled emulsification process lies in the synergistic effect of phase transition and particle size control. It's important to note that the three-stage homogenization process, as demonstrated in Example 1, is not simply a superposition of mechanical energy but rather a precise design based on the rheological properties of the emulsion. The initial 2000 rpm homogenization stage disperses the aqueous phase into the oil phase in a thin stream, forming a preliminary W / O emulsion interface. When the shear force is increased to 5000 rpm, the interfacial tension decreases, triggering a phase transition (O / W). The sustained high energy input overcomes the Laplace pressure's resistance to droplet refinement. Finally, the 8000 rpm supershear stage fragments any remaining large droplets through cavitation, reducing the particle size to a stable submicron range below 150 nm. This gradient design is particularly important in the high-viscosity formulation of Example 2—extending the homogenization time at 5000 rpm accommodates the formation dynamics of the hyaluronic acid cross-linked network and avoids localized overshearing that could disrupt the network structure.
[0026] At the level of efficacy synergy, each component achieves multi-dimensional repair of the skin barrier through a molecular complementary mechanism. In-depth analysis found that the long-chain sphingosine structure of ceramide III is highly similar to the lipids of the stratum corneum. It inserts into the intercellular lipid bilayer through hydrophobic interaction, rebuilding the "brick wall structure" damaged by excessive cleaning or environmental stimulation; and the multiple hydroxyl groups in the trehalose molecule form a strong hydrogen bond network with water molecules. In the low-temperature test of Example 2, it exhibited a unique glass transition characteristic - when the ambient humidity decreases, the trehalose molecules quickly form an amorphous protective film to lock in epidermal moisture. This dynamic moisturizing mechanism forms a temporal and spatial complementarity with the antioxidant properties of tuberose flavonoids: flavonoids scavenge ultraviolet-induced free radicals and reduce lipid peroxidation damage; ceramide and trehalose continuously repair the physical barrier. Together, the three form a complete protection chain of "prevention-repair-maintenance".
[0027] From an industrial perspective, this technology system achieves a balance between production efficiency and product performance. Practice has shown that while the gradient homogenization process adds two additional stages, its actual energy consumption is approximately 30% lower than that of traditional multi-step emulsification due to precise control of the total duration (<16 minutes) and the absence of repeated temperature adjustments. The negative pressure environment of the vacuum degassing process not only eliminates bubbles but also inhibits the initial chain reaction of lipid oxidation by reducing the oxygen partial pressure. This consistent anti-oxidation design ensures that the product maintains excellent stability even when antioxidants are omitted (as in the basic formula of Example 1), thus avoiding the risk of skin irritation caused by chemical preservatives at the source.
[0028] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.
Claims
1. A method for preparing a tuberose moisturizing cream, characterized in that: The method comprises the following steps: (a) preparing the oil phase: melting and mixing glyceryl stearate, squalane and ceramide III at 75-80°C, adding tuberose nanoliposomes and stirring at the same temperature; (b) preparing the aqueous phase: dissolving glycerol, trehalose and panthenol in deionized water and heating the mixture to 75-80°C; (c) primary emulsification: slowly adding the aqueous phase to the oil phase at a rate of 0.5-1 mL / s and homogenizing the mixture at 2000 rpm for 5 minutes; (d) gradient homogenization: first homogenizing the mixture at 5000 rpm for 8 minutes and then homogenizing the mixture at 8000 rpm for 3 minutes; (e) cooling and adding the emulsion: cooling the emulsion to below 45°C, adding tuberose volatile oil and baicalin; (f) vacuum degassing: stirring and degassing the mixture at a vacuum degree of -0.08 MPa for 20 minutes.
2. The method for preparing a tuberose moisturizing cream according to claim 1, wherein: The tuberose nanoliposomes are prepared by the following steps: dissolving lecithin and cholesterol in chloroform at a mass ratio of 4:1, rotary evaporating to form a thin film, adding a phosphate buffer solution containing 0.5wt% of tuberose total flavonoids, and hydrating and ultrasonicating to obtain liposomes with a particle size of 80-100nm.
3. The method for preparing a tuberose moisturizing cream according to claim 2, wherein: The oil phase components include 8-12% of glyceryl stearate, 5-8% of squalane, and 1-3% of ceramide III by mass percentage; the water phase components include 4-6% of glycerol, 1.5-4% of trehalose, and 0.5-1.5% of panthenol.
4. The method for preparing a tuberose moisturizing cream according to claim 1, wherein: During the step (d) gradient homogenization, the system temperature was maintained at 75±2°C.
5. The method for preparing a tuberose moisturizing cream according to claim 1, wherein: In step (e), the tuberose volatile oil is purified by molecular distillation, wherein the content of phenylethyl alcohol esters is not less than 85%.
6. The tuberose moisturizing cream prepared by the method for preparing a tuberose moisturizing cream according to any one of claims 1 to 5, characterized in that: The invention comprises the following components by mass percentage: 0.5-2% tuberose nanoliposomes, 1-3% ceramide III, 1.5-4% trehalose and 0.1-0.5% baicalin.
7. The tuberose moisturizing cream according to claim 6, characterized in that: The moisturizing cream is an O / W emulsion with an average particle size of 120-150 nm and a polydispersity index (PDI) of ≤0.
2.
8. Use of the tuberose moisturizing cream according to any one of claims 6 to 7 in the preparation of skin moisturizing care products.
9. Use of the tuberose moisturizing cream according to any one of claims 6 to 7 in preparing a skin barrier repair product.
10. Use of the tuberose moisturizing cream according to claims 6-7 in preparing a whitening skin care product that inhibits tyrosinase activity.