Herbal sleep-aiding gel and preparation process thereof

Abstract

The invention belongs to the technical field of sleep-aiding gels, and discloses a herbal sleep-aiding gel and a preparation process thereof, the gel comprises the following components: deionized water, propylene glycol, glycerol, carbomer 980 and triethanolamine; the mask is prepared from, by weight, 1.8% of lavender essential oil, chamomile extract, bitter orange flower essential oil, gamma-aminobutyric acid, melatonin, spina date seed extract, xylaria nigripes extract and phospholipid wall materials. Sodium chloride and azone; camphor and borneol; eDTA (Ethylene Diamine Tetraacetic Acid) disodium, phenoxyethanol and ethylhexylglycerin. The traditional Chinese medicine composition is suitable for people with sleep disorders such as long-term insomnia, difficulty in falling asleep, insomnia and dreaminess, easy awakening due to light sleep, restlessness and depression and the like; through the high transdermal absorption rate of a nano micro-capsule technology, in combination with a colloid double-electrode-layer structure, capacitance-like micro-current is generated, in cooperation with lavender-chamomile-bitter orange flower and other herbal essence and GABA and melatonin active ingredients, the sleep center is adjusted in a multi-channel mode, and the physical sleep-aiding scheme is a new physical sleep-aiding scheme for safely replacing a sleeping drug.

Description

Technical Field

[0001] The invention belongs to the technical field of sleep-aiding gels, and particularly relates to a herbal sleep-aiding gel and a preparation process thereof. Background Art

[0002] During the long pre-industrial era, human life closely followed the rhythms of nature, with sunrise and sunset. Life evolved to adapt to the day-night cycle brought about by the Earth's rotation, forming an internal circadian rhythm that governs and regulates various bodily systems. Light is the most important regulator of the biological clock. When light fades, the body secretes melatonin to promote sleepiness. When daylight returns, the body begins to secrete serotonin, which suppresses melatonin and dispels sleepiness. Thus, we fall asleep and wake up again. The fast pace and high pressures of modern life have many people compensating by staying up late, becoming habitual sleepers. This leads to difficulty falling asleep, sleepless nights, and poor or insufficient sleep, leaving them exhausted upon waking.

[0003] Insomnia poses serious health risks, manifesting in the following ways: Health-wise: It can cause immune and endocrine disorders, impact children's growth and development, and accelerate aging; it can also induce or aggravate colds, diabetes, obesity, stroke, cardiovascular diseases such as hypertension and coronary heart disease, and even cancer. Behavioral-wise: Fatigue, drowsiness, decreased alertness and concentration can easily lead to accidents; judgment and memory can be impaired, and learning and work abilities can be reduced. Psychologically: It can cause mood changes, irritability, and anger, and can even lead to mental and psychological disorders such as depression, anxiety, chronic pain, alcohol and drug dependence, cognitive decline, and, in severe cases, suicide.

[0004] Sleep problems have become a social focus. The "2024 Sleep Status Report" reveals that the number of patients with sleep disorders in my country has surged to 350 million, far exceeding the global average of 12%. The "2025 China Sleep Health Research Report" points out that the average nighttime sleep duration of Chinese adults is only 6.85 hours, more than half of the people fall asleep after midnight, and 26% of people sleep less than 6 hours. 39% of people wake up at night ≥ 2 times / night, and 65% of people experience at least 1-2 sleep problems per week, mainly manifested in waking up at night or early (16%), difficulty falling asleep (14%) and going to the toilet at night (13%).

[0005] The most common Western medicine treatments, such as sleeping pills, have serious toxic side effects and can cause dependence if used for a long time. Summary of the Invention

[0006] In order to overcome the above technical problems, the present invention provides a herbal sleep-aiding gel and a preparation process thereof.

[0007] The present invention adopts the following technical solutions: A herbal sleep-aiding gel, composed of the following ingredients by mass ratio: Deionized water 61.15%, propylene glycol 8.0%, glycerin 4.0%, carbomer 980 1.0%, triethanolamine (TEA) 0.75%; Lavender essential oil 1.8%, chamomile extract (10:1) 1.5%, bitter orange flower essential oil 0.7%, gamma-aminobutyric acid (GABA) 2.0%, melatonin 0.15%, jujube seed extract (5:1) 3.0%, black ginseng extract (10:1) 1.5%, phospholipid wall material 4.35%; Sodium chloride (NaCl) 1.0%, laurocapram (Azone) 2.0%; Camphor 0.8%, borneol 0.8%; Disodium EDTA 0.1%, Phenoxyethanol + Ethylhexylglycerin 0.8%.

[0008] The present invention also discloses a preparation process of a herbal sleep-aiding gel, comprising the following steps: Phase 1: Nanocapsule encapsulation: Dissolve the wall material in an appropriate amount of organic solvent; Add the core active ingredient mixture (lavender EO, chamomile Ext, bitter orange flower EO, GABA, melatonin, jujube seed Ext, and black ginseng Ext) to the wall material solution and mix or emulsify thoroughly; Use a high-pressure homogenizer or ultrasonic probe to perform nano-processing in an ice bath, controlling the pressure / power, number of cycles, and time to form nanoparticles with a particle size range of 50-200 nm; removing the organic solvent to obtain a nanocapsule suspension; The encapsulation efficiency, particle size distribution and Zeta potential were measured, and the absolute value of Zeta potential was >30 mV; Phase 2: Construction of colloidal double layer structure: Carbomer gel: After carbomer is dispersed and swelled, it is neutralized with alkali to form a three-dimensional network structure with negative charge, which serves as the basis of the double layer; Ionic environment: The added NaCl provides counterions (Na+); around the carbomer molecular chain, the negatively charged chain attracts Na+ in the solution, forming a compact layer and a diffusion layer, forming a double layer structure; By controlling the carbomer concentration, pH, and ionic strength, the rheology and Zeta potential of the gel are optimized, giving it "capacitor-like" properties; Stage 3: Pre-dispersion and dissolution Aqueous phase preparation: Weigh about 80% of the prescription amount of deionized water into the main preparation tank, add propylene glycol, glycerin, and disodium EDTA, and stir to dissolve evenly; While stirring continuously, slowly and evenly sprinkle the carbomer powder onto the liquid surface; Continue high-speed shear dispersion at 2000-4000 rpm for 15-20 minutes until the slurry is uniform, smooth, and free of visible particles. Stop stirring and let it stand for at least 30-60 minutes to allow the carbomer to fully hydrate and swell. Preparation of ion / osmotic phase: In another container, dissolve the prescribed amount of sodium chloride (NaCl) in deionized water (about 5% of the prescribed amount) and stir until completely dissolved. Add the prescribed amount of laurocapram (Azone) and stir to form a uniform microemulsion dispersion in water, and set aside; Oil phase / cooling agent dissolution: In another small container, combine camphor and borneol. Since both are solid at room temperature, add a portion of the prescribed amount of propylene glycol. Gently heat (<40°C) and stir until completely dissolved and transparent. Cool to room temperature and set aside. Stage 4: Addition of nano-microcapsules active ingredients Adding nanocapsule suspension: adding the pre-prepared and qualified nanocapsule suspension (including encapsulated lavender EO, chamomile Ext, bitter orange flower EO, GABA, melatonin, jujube seed Ext, and black ginseng Ext) to the fully swollen carbomer aqueous phase slurry; Gentle mixing: Use a paddle stirrer at 50-100 rpm for 10-15 minutes to ensure that the nanocapsules are evenly dispersed throughout the aqueous phase; Stage 5: Gelation and Neutralization Add the ion / osmotic phase: Add the prepared NaCl / Azone solution to the main preparation tank and continue stirring at low speed with a paddle stirrer for 5-10 minutes to mix thoroughly. Neutralization and gelation: Dilute the prescribed amount of triethanolamine (TEA) with the remaining deionized water; Slowly add the TEA solution to the main preparation tank under continuous paddle stirring to prevent local over-alkalinity that may cause the gel to agglomerate, turn white, or become opaque. Real-time monitoring of pH value: Use a calibrated precision pH meter with the probe immersed in the reaction solution. Target pH range: 6.3-6.5; When the pH reaches the target value of 6.5, stop adding TEA solution. At this time, the system should thicken significantly, become transparent or translucent, and form a gel matrix; Stage 6: Add remaining ingredients and homogenize Add the cooling agent solution: Add the dissolved camphor and borneol (in propylene glycol) to the neutralized gel and continue stirring with a paddle mixer at medium to low speed for 10-15 minutes to ensure uniform dispersion; Add preservatives: Add the prescribed amount of broad-spectrum preservatives and stir for 5-10 minutes until completely dissolved; Final volume adjustment: rinse the container wall with deionized water and add to the main tank, stirring until the total volume reaches 100%; Gentle homogenization: switch to the homogenizer, 1000-2000 rpm, homogenize for 1-2 minutes; Stage 5: Degassing and filling Vacuum degassing: Transfer the prepared gel to a vacuum stirring tank, start low-speed stirring and apply vacuum (-0.08 to -0.09 MPa); degas for 15-30 minutes until no obvious bubbles escape from the gel; Filling: Under the protection of normal pressure or slightly positive pressure inert gas (such as N2), the gel is filled into the push tube through a filling machine.

[0009] Compared with the prior art, the present invention has the following beneficial effects: This product is suitable for people with sleep disorders such as chronic insomnia, difficulty falling asleep, frequent insomnia, light sleep with frequent awakenings, anxiety and depression. Its ingredients are safe. Using nano-microencapsulation technology (particle size ≤ 100nm), it achieves a high transdermal absorption rate of 92%+. Combined with a colloidal double-layer structure (zeta potential -42mV), it generates a capacitive-like microcurrent. It synergizes herbal extracts such as lavender, chamomile, and bitter orange blossom with GABA and melatonin active ingredients to regulate sleep centers through multiple pathways: ① Rapidly inhibiting neural excitability (shortening sleep onset time by 53%), ② Synchronizing biological rhythms, and ③ Alleviating anxiety. Topical application to acupuncture points eliminates the liver damage and drowsiness risks associated with oral medications, making it a safe alternative to sleeping pills and a new physical sleep aid. DETAILED DESCRIPTION

[0010] The following embodiments of the present invention are described in detail. Unless otherwise specified, the raw materials and equipment used are commercially available or commonly used in the art. The methods in the embodiments, unless otherwise specified, are conventional methods in the art. The embodiments described below are exemplary and are intended only to explain the present invention and are not to be construed as limiting the present invention.

[0011] Herbal sleep aid gel, calculated by mass ratio, is composed of the following ingredients: Aqueous matrix: deionized water 61.15%, propylene glycol 8.0%, glycerol 4.0%; Gel base: Carbomer 980 1.0%, triethanolamine (TEA) 0.75%; Nanocapsule active ingredients: lavender essential oil 1.8%, chamomile extract (10:1) 1.5%, bitter orange flower essential oil 0.7%, gamma-aminobutyric acid (GABA) 2.0%, melatonin 0.15%, jujube seed extract (5:1) 3.0%, black ginseng extract (10:1) 1.5%, phospholipid wall material 4.35%; Ion / osmotic system: sodium chloride (NaCl) 1.0%, laurocapram (Azone) 2.0%; Auxiliary ingredients: camphor 0.8%, borneol 0.8%; Stabilizing / preservative system: Disodium EDTA 0.1%, Phenoxyethanol + Ethylhexylglycerin 0.8%.

[0012] Preparation process Phase 1: Nanocapsule encapsulation (GMP clean area, temperature ≤ 25°C) wall material dissolution Dissolve 4.35% phospholipid wall material (hydrogenated soybean lecithin) in food-grade anhydrous ethanol (the amount used is 3 times the volume of the wall material) and stir in a 45°C water bath until completely transparent.

[0013] Active ingredient emulsification Mix 1.8% lavender essential oil + 0.7% bitter orange flower essential oil with 0.8% molten borneol (pre-melted), add 2.0% GABA, 0.15% melatonin, 3.0% jujube seed extract, 1.5% black ginseng extract, and 1.5% chamomile extract, and homogenize and emulsify (5000 rpm, 2 min) to form a homogeneous oil phase.

[0014] High-pressure homogenization nanomaterials The oil phase was injected into the wall material solution and homogenized under high pressure (1000 bar, 5 cycles) under ice bath conditions with an outlet temperature of ≤30°C.

[0015] Solvent removal and stabilization The ethanol was completely removed by rotary evaporation (40°C / -0.09 MPa), and deionized water was added to make the total weight 15% to obtain a nanosuspension.

[0016] Real-time QC: Laser particle size analyzer to detect particle size (D50=80±10nm, PDI<0.2), Zeta potential instrument to measure charge (-35mV±5).

[0017] Stage 2: Pre-dispersion and dissolution (closed system, dust-proof) Carbomer Dispersion Key Control 49.72% deionized water (80% of the total 61.15%) was injected into the main tank, and the anchor stirring + online homogenizer (2000 rpm) was turned on.

[0018] Carbomer 980 1.0% was slowly sucked into the liquid surface vortex through a vacuum feeder (rate ≤ 0.5 kg / min) to prevent dust.

[0019] The homogenizer was increased to 4000 rpm for dispersion for 20 minutes. The slurry was translucent and free of particles. It was allowed to stand for hydration for 45 minutes.

[0020] Preparation of ion / osmotic phase In a secondary tank, 1.0% NaCl was dissolved in 3.06% water (total 5%), and 2.0% Azone was added and then ultrasonicated (40 kHz, 5 min) to form a microemulsion.

[0021] Coolant pretreatment Dissolve 0.8% camphor + remaining propylene glycol in a 35°C water bath with stirring, then cool to 25°C for later use.

[0022] Phase 3: Nanocapsule integration and gelation (precise pH control) Nanosuspension added 15% nanosuspension was pumped into the main tank, and the tank was filled with nitrogen and mixed with anchor stirring at 50 rpm for 15 min.

[0023] Ionic phase mixing Inject NaCl / Azone microemulsion, anchor stirring + online homogenization, 1000 rpm, 10 min.

[0024] Neutralization and gelation (core step) TEA 0.75% was diluted with 6.13% water (the remaining amount) to a 10% solution, and added dropwise at a flow rate of 1 mL / min via a metering pump.

[0025] Real-time pH feedback system monitoring, when approaching pH 6.4, switch to 0.2mL / min drip rate, accurately stop at pH 6.5±0.05.

[0026] After the system turns into a transparent gel, stop stirring and let it stand for 10 minutes to complete the structural reorganization.

[0027] Stage 4: Terminal homogenization and degassing (avoid light) Post-add ingredient integration The camphor / propylene glycol solution was injected and the mixture was stirred at 30 rpm for 15 min.

[0028] Add EDTA 0.1% + phenoxyethanol 0.7% + ethylhexylglycerin 0.1% and stir for 10 minutes.

[0029] Volume determination and homogenization Add deionized water to 100%, and use an online homogenizer at 1500 rpm / 2 min (pressure < 2 bar).

[0030] Vacuum degassing optimization Transfer to a double-cone vacuum tank (-0.095 MPa, 20 rpm) and degas for 25 min until the bubble diameter is less than 100 μm.

[0031] Stage 5: Filling and packaging (protect from light throughout the process) Filling control Use a stainless steel piston pump to fill into brown medical-grade co-extruded tubing (oxygen transmission rate <0.01cc / pkg / day).

[0032] Nitrogen is filled and replaced (residual oxygen content is less than 0.5%), and the pipe end is sealed by hot melt.

[0033] Real-time quality inspection Samples are taken from the first and last tubes of each batch to measure the Zeta potential (-40mV±2) and rheological properties (viscosity 15,000±500cP).

[0034]

Applying position

[0035] Note: Apply behind the ears because there are many acupoints behind the ears. You can also apply to the temples, Shenque point, Yintang point, and Neiguan point.

[0036]

Applying time

[0037] It is generally not recommended to use it after 11 pm to avoid waking up sleepy in the morning.

[0038]

Application method

[0039]

Cleaning in time

[0040] The test results of the present invention are shown in Table 1: Table 1 Although the embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to the above embodiments without departing from the principles and purpose of the present invention, and that the scope of the present invention is defined by the claims and their equivalents.

Claims

1. A herbal sleep-aiding gel, characterized in that: By mass ratio, it is composed of the following ingredients: Deionized water 61.15%, propylene glycol 8.0%, glycerin 4.0%, carbomer 980 1.0%, triethanolamine (TEA) 0.75%; Lavender essential oil 1.8%, chamomile extract (10:1) 1.5%, bitter orange flower essential oil 0.7%, gamma-aminobutyric acid (GABA) 2.0%, melatonin 0.15%, jujube seed extract (5:1) 3.0%, black ginseng extract (10:1) 1.5%, phospholipid wall material 4.35%; Sodium chloride (NaCl) 1.0%, laurocapram (Azone) 2.0%; Camphor 0.8%, borneol 0.8%; Disodium EDTA 0.1%, Phenoxyethanol + Ethylhexylglycerin 0.8%.

2. A preparation process of a herbal sleep-aiding gel, characterized in that: The following steps are involved: Phase 1: Nanocapsule encapsulation: Dissolve the wall material in an appropriate amount of organic solvent; Add the core active ingredient mixture (lavender EO, chamomile Ext, bitter orange flower EO, GABA, melatonin, jujube seed Ext, and black ginseng Ext) to the wall material solution and mix or emulsify thoroughly; Use a high-pressure homogenizer or ultrasonic probe to perform nano-processing in an ice bath, controlling the pressure / power, number of cycles, and time to form nanoparticles with a particle size range of 50-200 nm; removing the organic solvent to obtain a nanocapsule suspension; The encapsulation efficiency, particle size distribution and Zeta potential were measured, and the absolute value of Zeta potential was >30 mV; Phase 2: Construction of colloidal double layer structure: Carbomer gel: After carbomer is dispersed and swelled, it is neutralized with alkali to form a three-dimensional network structure with negative charge, which serves as the basis of the double layer; Ionic environment: Added NaCl provides counter ions (Na + Around the carbomer molecular chain, the negatively charged chain attracts Na in the solution. + , forming a compact layer and a diffusion layer, forming a double electric layer structure; By controlling the carbomer concentration, pH, and ionic strength, the rheology and Zeta potential of the gel are optimized, giving it "capacitor-like" properties. Stage 3: Pre-dispersion and dissolution Aqueous phase preparation: Weigh about 80% of the prescription amount of deionized water into the main preparation tank, add propylene glycol, glycerin, and disodium EDTA, and stir to dissolve evenly; While stirring continuously, slowly and evenly sprinkle the carbomer powder onto the liquid surface; Continue high-speed shear dispersion at 2000-4000 rpm for 15-20 minutes until the slurry is uniform, smooth, and free of visible particles. Stop stirring and let it stand for at least 30-60 minutes to allow the carbomer to fully hydrate and swell. Preparation of ion / osmotic phase: In another container, dissolve the prescribed amount of sodium chloride (NaCl) in deionized water (about 5% of the prescribed amount) and stir until completely dissolved. Add the prescribed amount of laurocapram (Azone) and stir to form a uniform microemulsion dispersion in water, and set aside; Oil phase / cooling agent dissolution: In another small container, combine camphor and borneol. Since both are solid at room temperature, add a portion of the prescribed amount of propylene glycol. Gently heat (<40°C) and stir until completely dissolved and transparent. Cool to room temperature and set aside. Stage 4: Addition of nano-microcapsules active ingredients Adding nanocapsule suspension: adding the pre-prepared and qualified nanocapsule suspension (including encapsulated lavender EO, chamomile Ext, bitter orange flower EO, GABA, melatonin, jujube seed Ext, and black ginseng Ext) to the fully swollen carbomer aqueous phase slurry; Gentle mixing: Use a paddle stirrer at 50-100 rpm for 10-15 minutes to ensure that the nanocapsules are evenly dispersed throughout the aqueous phase; Stage 5: Gelation and Neutralization Add the ion / osmotic phase: Add the prepared NaCl / Azone solution to the main preparation tank and continue stirring with a paddle stirrer at medium to low speed for 5-10 minutes to mix thoroughly; Neutralization and gelation: Dilute the prescribed amount of triethanolamine (TEA) with the remaining deionized water; Slowly add the TEA solution to the main preparation tank under continuous paddle stirring to prevent local over-alkalinity that may cause the gel to agglomerate, turn white, or become opaque. Real-time monitoring of pH value: Use a calibrated precision pH meter with the probe immersed in the reaction solution. Target pH range: 6.3-6.5; When the pH reaches the target value of 6.5, stop adding TEA solution. At this time, the system should thicken significantly, become transparent or translucent, and form a gel matrix; Stage 6: Add remaining ingredients and homogenize Add the cooling agent solution: Add the dissolved camphor and borneol (in propylene glycol) to the neutralized gel and continue stirring with a paddle mixer at medium to low speed for 10-15 minutes to ensure even dispersion. Add preservatives: Add the prescribed amount of broad-spectrum preservatives and stir for 5-10 minutes until completely dissolved; Final volume adjustment: rinse the container wall with deionized water and add to the main tank, stirring until the total volume reaches 100%; Gentle homogenization: switch to the homogenizer, 1000-2000 rpm, homogenize for 1-2 minutes; Stage 5: Degassing and filling Vacuum degassing: Transfer the prepared gel to a vacuum stirring tank, start low-speed stirring and apply vacuum (-0.08 to -0.09 MPa); degas for 15-30 minutes until no obvious bubbles escape from the gel; Filling: Under the protection of normal pressure or slightly positive pressure inert gas (such as N2), the gel is filled into the push tube through a filling machine.

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