Valerian extract, preparation method and application of valerian extract in sleep aiding product

Abstract

The invention provides a valerian extract, a preparation method and application of the valerian extract in sleep-aiding products, and belongs to the technical field of plant extracts and sleep-aiding products. The valerian extract is prepared by performing pretreatment, low-temperature enzymolysis, segmented extraction and ultrafiltration purification on valerian rhizomes. The prepared valerian extract is applied to a water-based sniffing type sleep-aiding product, and the water-based sniffing type sleep-aiding product is obtained by taking the valerian extract as a core active component and compounding the valerian extract with other sleep-aiding components. According to the preparation method disclosed by the invention, the retention rate and the purity of valerian are remarkably improved, and the obtained water-based sniffing type sleep-aiding product does not need to be smeared or pressed and can play a role only through natural sniffing. The preparation process has the advantages of clear parameters, easily available raw materials and conventional equipment, can be directly applied to industrial production, and has the advantages of good product stability, long shelf life and wide market application prospect.

Description

Technical Field

[0001] This invention belongs to the technical field of plant extracts and sleep aid products, and particularly relates to a valerian extract, its preparation method, and its application in sleep aid products. Background Technology

[0002] Valerian, a traditional sleep-aiding plant, contains core active ingredients valerate and acevalerate, which can exert sedative and sleep-aiding effects by regulating the activity of γ-aminobutyric acid (GABA) receptors in the central nervous system. However, existing valerian extract preparation processes have significant drawbacks: conventional methods use high-temperature enzymatic hydrolysis at 45-55℃ or direct hot water extraction, which causes heat-sensitive valerate to degrade due to high temperatures (the degradation rate can reach 30%-50%). Furthermore, the extract contains a large amount of impurities such as cellulose and tannins, which not only reduces the purity of the extract but also affects its compatibility with other sleep-aiding ingredients (such as essential oils and plant extracts), resulting in poor product stability and unsatisfactory sleep-aiding effects.

[0003] Meanwhile, current commercially available sleep aids (such as sleep creams and sprays) suffer from problems such as cumbersome application (requiring application and pressing), reliance on chemical preservatives (such as phenoxyethanol), and low purity of essential oils (e.g., lavender essential oil has excessive camphor content, which can easily cause nerve excitation). Especially in inhaled sleep aids, the volatility of chemical preservatives may irritate the respiratory tract, while low-purity active ingredients are unlikely to effectively promote sleep through the olfactory pathway, failing to meet the needs of sensitive groups (such as pregnant women and the elderly).

[0004] Therefore, developing a preparation process for valerian extract that can efficiently retain valerin and has low impurities, and combining it with high-purity natural sleep-aiding ingredients, along with a natural antibacterial system to construct a safe and convenient water-based inhalation sleep aid product, has become a technological direction that the industry urgently needs to break through. Summary of the Invention

[0005] To address the aforementioned problems in the prior art, this invention provides a valerian extract, its preparation method, and its application in sleep aid products. Through an innovative process of low-temperature enzymatic hydrolysis-segmented extraction-ultrafiltration purification, the problems of valerin degradation and numerous impurities in existing processes are solved. Furthermore, by applying this highly active valerian extract to a water-based inhaled sleep aid product, it combines natural sleep-aiding and antibacterial components to achieve the dual effects of highly effective sleep aid and safety without irritation.

[0006] To achieve the above objectives, the present invention provides the following technical solution: One of the technical solutions of the present invention: This invention provides a method for preparing valerian extract, comprising the following steps: (1) Valerian root and rhizome are dried and pulverized to obtain valerian root and rhizome powder; (2) Add water, compound enzyme and calcium chloride to the valerian root and stem powder, adjust the pH value, and carry out enzymatic hydrolysis under stirring to obtain enzymatic hydrolysate; (3) The valerian extract is obtained by fractional extraction and ultrafiltration purification of the enzymatic hydrolysate.

[0007] Further, the pulverization described in step (1) is performed to pass through an 80-100 mesh sieve.

[0008] Further, the mass ratio of valerian root powder to water in step (2) is 1:(8-12). The amount of the compound enzyme added is 0.2%-0.5% of the mass of the valerian root and stem powder, preferably 0.3%; The amount of calcium chloride added is 0.05%-0.1% of the mass of the valerian root and stem powder, preferably 0.08%.

[0009] Furthermore, the compound enzyme is cellulase and pectinase in a mass ratio of 1:2, with an enzyme activity ≥5000 U / g.

[0010] Furthermore, the pH value mentioned in step (2) is 4.5-5.0; The stirring speed is 150-200 r / min, preferably 180 r / min; The enzymatic hydrolysis is performed at a temperature of 35-40 °C for 1.5-2.0 h, preferably at a temperature of 38 °C for 1.8 h.

[0011] Further, the segmented extraction in step (3) is as follows: water is added to the enzymatic hydrolysate until the solid-liquid ratio of the enzymatic hydrolysate is 1 g: 8 mL, and the mixture is extracted at 50-55 ℃ for 1 h, and filtered to obtain the first extract; water is added to the filter residue, and the mixture is extracted again at 70-75 ℃ for 1 h, and filtered to obtain the second extract; the first extract and the second extract are combined to obtain the crude extract. The ultrafiltration purification is performed as follows: the crude extract is pretreated with a 0.22 μm microporous membrane, and then ultrafiltration is carried out with an ultrafiltration membrane with a molecular weight cutoff of 3000 Da at 0.1-0.15 MPa and 30-35 °C. The permeate is collected and concentrated under reduced pressure to obtain the valerian extract.

[0012] Furthermore, the mass ratio of filter residue to water in the segmented extraction is 1:8.

[0013] Furthermore, the vacuum concentration is carried out until the relative density of the permeate is 1.05-1.10 (25 °C), and the valerin content in the valerian extract after vacuum concentration is 18%-20%. The ultrafiltration pressure is further preferably 0.12 MPa, and the temperature is 32 °C.

[0014] The second technical solution of the present invention: The present invention also provides a valerian extract prepared by a method for preparing valerian extract.

[0015] Furthermore, the valerian extract contains ≥15% valerin, ≤0.5% tannins, and ≤10 CFU / mL total bacterial count.

[0016] The third technical solution of the present invention: This invention also provides an application of valerian extract in a sleep aid product, which is a water-based inhalation sleep aid product that helps shorten the time to fall asleep and prolong the time of deep sleep through the olfactory pathway.

[0017] Furthermore, the water-based inhaled sleep aid product uses valerian extract as its core active ingredient and includes the following components: Valerian extract 0.8%-2.0%, agarwood essential oil 0.1%-0.5%, lavender essential oil 0.2%-0.8%, bitter orange extract 0.5%-1.5%, orange peel extract 0.3%-1.0%, vanilla extract 0.3%-0.9%, sandalwood extract 0.2%-0.6%, honeysuckle extract 0.3%-0.5%, rosemary extract 0.2%-0.4%, PEG-40 hydrogenated castor oil 2.0%-5.0%, glycerin 1.0%-3.0%, propylene glycol 1.5%-4.0%, hydroxyethyl cellulose 0-2%, sodium alginate 0-1.5%, calcium sulfate 0-0.5%, with the balance being purified water.

[0018] Furthermore, the water-based inhalation sleep aid product comprises the following components by weight: valerian extract 1.5%, agarwood essential oil 0.3%, lavender essential oil 0.5%, bitter orange extract 1.0%, orange peel extract 0.6%, vanilla extract 0.6%, sandalwood extract 0.4%, honeysuckle extract 0.4%, rosemary extract 0.3%, PEG-40 hydrogenated castor oil 3.5%, glycerin 2.0%, propylene glycol 2.5%, hydroxyethyl cellulose 0.5%, sodium alginate 1.0%, calcium sulfate 0.3%, and the balance being purified water.

[0019] Furthermore, the lavender essential oil was purified by molecular distillation under the conditions of 60-65 °C and 0.1 Pa. After purification, the lavender essential oil contained ≥55% linalool and ≤0.5% camphor. The honeysuckle extract contains ≥5% chlorogenic acid. The rosemary extract contains ≥3% rosmarinicol.

[0020] Furthermore, the preparation process of the bitter orange flower extract, orange peel extract, vanilla extract, and sandalwood extract is as follows: after pulverizing the plant raw materials, add 8-12 times the mass of water, reflux extract at 80-90 ℃ for 2-3 times, each time for 1-1.5 h, combine the extracts and concentrate to a relative density of 1.05-1.10 (25 ℃), and filter through a 0.22 μm microporous membrane.

[0021] Furthermore, the preparation method of the water-based inhalation sleep aid product includes the following steps: (1) The PEG-40 hydrogenated castor oil, glycerin and propylene glycol were added to water and stirred at 40 °C to dissolve them, thus obtaining a mixed solvent; (2) Add the valerian extract, agarwood essential oil, lavender essential oil, bitter orange extract, orange peel extract, vanilla extract, sandalwood extract, honeysuckle extract, and rosemary extract to the mixed solvent, mix evenly, then add water again, stir for 10-15 min, and homogenize at 4000 r / min for 5-8 min to obtain a homogenized liquid. (3) The homogenized liquid is filtered through a 0.22 μm microporous membrane, then pasteurized at 60-65 °C for 30 min, and cooled to obtain the water-based inhalation sleep aid product.

[0022] Furthermore, the amount of water added in step (1) is 50%-60%; Stir at 200 r / min until completely dissolved.

[0023] Furthermore, in step (2), the mixed solvent is stirred for 15-20 min at 40 °C after each component is added during the preparation process, preferably 18 min, at a speed of 200 r / min, to ensure that each component is evenly dispersed. The amount of water added is the remainder of the remaining formula after all ingredients have been added; The homogenization time is preferably 6 minutes.

[0024] Furthermore, in step (3), the pH value of the product after sterilization is controlled at 6.0-6.5; After cooling, the product is filled into containers equipped with microporous diffusers or vent valves.

[0025] The beneficial effects of this invention compared to the prior art are as follows: This invention shortens the time to fall asleep, prolongs the time of deep sleep, reduces the number of times you wake up at night, and significantly improves sleep efficiency.

[0026] The method for preparing valerian extract of this invention, focusing on three key technical aspects—low-temperature enzymatic hydrolysis, fractional extraction, and ultrafiltration purification—leads to the following innovations: (1) Low-temperature enzymatic hydrolysis enhancement technology To address the problem of valerin degradation caused by conventional high-temperature enzymatic hydrolysis, this invention achieves low-temperature, high-efficiency enzymatic hydrolysis through two key designs: Enzyme activator addition: Calcium chloride is introduced as an activator for the compound enzyme (cellulase: pectinase = 1:2). Calcium ions can bind to the active site of the enzyme molecule, improve the catalytic efficiency of the enzyme at low temperature (35-40 ℃), and make the enzyme activity retention rate ≥90%, which solves the industry pain point of low enzymatic hydrolysis efficiency at low temperature. Dynamic stirring optimization: Dynamic stirring at 150-200 r / min ensures full contact between the enzyme solution and valerian root powder, avoiding uneven enzymatic hydrolysis caused by excessively high local enzyme concentration. This shortens the hydrolysis time from the conventional 4-6 h to 1.5-2.0 h, while also reducing the growth of miscellaneous bacteria (total colony count ≤10 CFU / mL). No additional sterilization is required to meet subsequent application requirements.

[0027] HPLC analysis of the valerian extract prepared by this invention revealed that the low-temperature enzymatic hydrolysis process can increase the valerin release rate from 40% in conventional processes to 85%, while controlling the degradation rate within 5%-8%.

[0028] (2) Segmented temperature control and directional extraction strategy This invention utilizes the differences in solubility of different active ingredients in valerian to design a two-stage extraction process: First stage (35-40 ℃): Targeted extraction of heat-sensitive valerin. At this temperature, valerin has high solubility and is not easily degraded, and the proportion of valerin in the extract is ≥80%. The second stage (70-75 ℃): secondary extraction of the filter residue to obtain auxiliary active ingredients such as flavonoids (e.g., quercetin) and polysaccharides. These ingredients can enhance the sleep-aiding synergistic effect of valerin, and the medium temperature conditions can prevent the large-scale dissolution of impurities such as cellulose and tannins.

[0029] Compared with conventional single high-temperature extraction (80-90 ℃), the total yield of active ingredients in the valerian extract of this invention is increased by 45%, and the tannin content is reduced from the conventional 5%-8% to ≤0.5%, significantly improving the purity of the extract.

[0030] (3) This invention employs an ultrafiltration membrane purification and quality improvement process. An ultrafiltration membrane with a molecular weight cutoff of 3000 Da is used to purify the crude extract, precisely removing impurities such as cellulose and large molecular weight proteins with a molecular weight greater than 3000 Da, while retaining small molecule active ingredients such as valerin (molecular weight approximately 354 Da) and flavonoids (molecular weight approximately 300-400 Da). After purification, the purity of valerin increases from 5%-8% in conventional processes to 15%-20%, and the extract exhibits high clarity, showing no stratification when mixed with essential oils and other plant extracts, laying the foundation for subsequent preparation of water-based products.

[0031] This invention employs an innovative low-temperature enzymatic hydrolysis, segmented extraction, and ultrafiltration purification process. By activating enzyme activity with calcium chloride, performing segmented temperature-controlled directional extraction, and using ultrafiltration membranes for precise purification, it solves the problems of valerin degradation (degradation rate reduced from 30%-50% to 5%-8%), high impurity levels (tannin content reduced from 5%-8% to ≤0.5%), and poor solubility in conventional processes. This increases the purity of valerin to 15%-20%, laying a core raw material foundation for the development of highly effective sleep aid products.

[0032] (4) Innovative compound formulation of water-based inhalation sleep aid products This invention uses valerian extract as the core to prepare a water-based inhaled sleep aid product. It is then combined with various natural sleep-aiding and antibacterial ingredients to form a synergistic water-based inhaled product. The innovations are as follows: This invention synergistically combines sleep-aiding ingredients. The core sleep-aiding combination consists of valerian extract (valerin), agarwood essential oil (linalool), and lavender essential oil (linalool). These three ingredients work synergistically through a dual mechanism of regulating GABA receptor activity and inhibiting sympathetic nerve excitation. Animal experiments show that this reduces the time it takes for rats to fall asleep by 20%-25% compared to the valerian extract-only group. The auxiliary sleep-aiding ingredients are: bitter orange extract (limonene), orange peel extract (hesperidin), vanilla extract (coumarin), and sandalwood extract (santalol). These four extracts work synergistically to further relieve nervous tension, reduce the number of nighttime awakenings, and their refreshing aroma improves the product's inhalation experience, increasing user acceptance. This invention also controls the purity of the essential oils: lavender essential oil is purified by molecular distillation (60-65 ℃, 0.1 Pa) to remove camphor (content ≤0.5%), avoiding its nerve excitation, while simultaneously increasing the linalool content to ≥55%, enhancing the sleep-aiding effect.

[0033] This invention constructs a natural antibacterial system by introducing honeysuckle extract (chlorogenic acid ≥5%) and rosemary extract (rosmarinic acid ≥3%) to replace traditional chemical preservatives. Synergistic antibacterial effect: The minimum inhibitory concentrations (MICs) of chlorogenic acid against Escherichia coli and Staphylococcus aureus are 0.2% and 0.15%, respectively, while the MIC of rosmarinic acid against mold is 0.3%. When the two are combined in a 4:3 ratio, the antibacterial spectrum covers both bacteria and mold, ensuring a total bacterial count ≤50 CFU / mL and no skin irritation (skin irritation index PII=0). Furthermore, chlorogenic acid enhances the sleep-aiding effect of valerin, and rosmarinic acid delays essential oil oxidation and reduces the formation of aldehyde oxidation products, allowing the product to retain ≥90% of its sleep-aiding activity after 6 months of storage at 40 ℃ and 75% RH.

[0034] This invention constructs a stable water-based system: using PEG-40 hydrogenated castor oil as an emulsifier, combined with glycerin and propylene glycol as cosolvents and stabilizers; wherein PEG-40 hydrogenated castor oil can emulsify fat-soluble essential oils (agarwood essential oil, lavender essential oil) into tiny droplets of 10-100 nm, which are uniformly dispersed in the water matrix, avoiding stratification; glycerin and propylene glycol can enhance the moisturizing properties of the system, reduce the rapid loss of volatile components, and make the product's inhalation effect last for 8-12 hours, meeting the needs of nighttime sleep use.

[0035] The water-based inhalation sleep aid product prepared by this invention, with valerian extract as the core active ingredient, achieves the triple goals of safety, high efficiency, and convenience. Safety: It utilizes honeysuckle and rosemary extracts to construct a natural antibacterial system, completely replacing chemical preservatives. Toxicological verification shows no skin or respiratory irritation, meeting the needs of sensitive groups such as pregnant women and the elderly. High efficiency: The highly active valerian extract, combined with high-purity essential oils and auxiliary plant extracts, works synergistically to regulate the central nervous system through the olfactory pathway, shortening sleep onset time by 54% and extending deep sleep time by 100%, resulting in a significantly better sleep aid effect than existing products. Convenience: No application or pressing is required; it works simply through natural inhalation, making it suitable for various scenarios such as home, travel, and office use, with a low barrier to entry.

[0036] The preparation process parameters of this invention are clear, the raw materials are readily available, the equipment is conventional, it can be directly applied to industrial production, and the product has good stability and long shelf life, and has broad market application prospects. Detailed Implementation

[0037] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0038] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0039] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0040] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be obvious to those skilled in the art. This specification and embodiments are merely exemplary.

[0041] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0042] All raw materials used in the following embodiments of the present invention can be purchased commercially.

[0043] In the embodiments of the present invention, the room temperature is 23±2℃.

[0044] Example 1 A method for preparing valerian extract includes the following steps: (1) Raw material pretreatment: Valerian root and stem are dried and pulverized to pass through an 80-mesh sieve to obtain valerian root and stem powder.

[0045] (2) Low-temperature enzymatic hydrolysis: Take 100 g of the above valerian root and stem powder, add 800 mL of purified water, then add 0.5 g of compound enzyme (cellulase: pectinase = 1:2) and 0.1 g of calcium chloride, adjust the pH value to 4.5, and enzymatically hydrolyze under stirring at 150 r / min, at a temperature of 40 ℃ for 1.5 h to obtain the enzymatic hydrolysate.

[0046] (3) Segmented extraction: Add purified water to the above enzymatic hydrolysate until the solid-liquid ratio of the enzymatic hydrolysate is 1 g: 8 mL, then extract at 50 ℃ for 1 h, filter to obtain the first extract, add 800 mL of purified water to the filter residue, extract again at 75 ℃ for 1 h, filter to obtain the second extract, combine the two extracts to obtain the crude extract.

[0047] (4) Ultrafiltration purification: After pretreatment of the above crude extract with a 0.22 μm microporous membrane, ultrafiltration was carried out at 0.1 MPa and 35 °C using an ultrafiltration membrane with a molecular weight cutoff of 3000 Da. The permeate was collected and concentrated under reduced pressure to a relative density of 1.05 (25 °C) to obtain valerian extract.

[0048] The above-mentioned valerian extract was tested and the results showed that the valerin content was 18.5%, the tannin content was 0.5%, and the total bacterial count was <10 CFU / mL.

[0049] Example 2 A method for preparing valerian extract includes the following steps: (1) Raw material pretreatment: Valerian root and stem are dried and pulverized to pass through a 90-mesh sieve to obtain valerian root and stem powder.

[0050] (2) Low-temperature enzymatic hydrolysis: Take 100 g of the above valerian root and stem powder, add 1200 mL of purified water, then add 0.2 g of compound enzyme (cellulase: pectinase = 1:2) and 0.05 g of calcium chloride, adjust the pH value to 5.0, and enzymatically hydrolyze under stirring at 200 r / min. The enzymatic hydrolysis temperature is 35 ℃ and the time is 2.0 h to obtain the enzymatic hydrolysate.

[0051] (3) Segmented extraction: Add purified water to the above enzymatic hydrolysate until the solid-liquid ratio of the enzymatic hydrolysate is 1 g: 8 mL, then extract at 55 ℃ for 1 h, filter to obtain the first extract, add 800 mL of purified water to the filter residue, extract again at 70 ℃ for 1 h, filter to obtain the second extract, combine the two extracts to obtain the crude extract.

[0052] (4) Ultrafiltration purification: After pretreatment of the crude extract with a 0.22 μm microporous membrane, ultrafiltration was carried out with a 3000 Da molecular weight cutoff membrane at 0.15 MPa and 30 °C. The permeate was collected and concentrated under reduced pressure to a relative density of 1.10 (25 °C) to obtain valerian extract.

[0053] The above-mentioned valerian extract was tested and the results showed that the valerin content was 17.2%, the tannin content was 0.4%, and the total bacterial count was <10 CFU / mL.

[0054] Example 3 A method for preparing valerian extract includes the following steps: (1) Raw material pretreatment: Valerian root and stem are dried and pulverized to pass through a 100-mesh sieve to obtain valerian root and stem powder.

[0055] (2) Low-temperature enzymatic hydrolysis: Take 100 g of the above valerian root and stem powder, add 1000 mL of purified water, then add 0.3 g of compound enzyme (cellulase: pectinase = 1:2) and 0.08 g of calcium chloride, adjust the pH value to 4.8, and enzymatically hydrolyze under stirring at 180 r / min. The enzymatic hydrolysis temperature is 38 ℃ and the time is 1.8 h to obtain the enzymatic hydrolysate.

[0056] (3) Segmented extraction: Add purified water to the above enzymatic hydrolysate until the solid-liquid ratio of the enzymatic hydrolysate is 1 g: 8 mL, then extract at 52 ℃ for 1 h, filter to obtain the first extract, add 800 mL of purified water to the filter residue, extract again at 72 ℃ for 1 h, filter to obtain the second extract, combine the two extracts to obtain the crude extract.

[0057] (4) Ultrafiltration purification: After pretreatment of the above crude extract with a 0.22 μm microporous membrane, ultrafiltration was carried out using an ultrafiltration membrane with a molecular weight cutoff of 3000 Da at 0.12 MPa and 32 °C. The permeate was collected and concentrated under reduced pressure to a relative density of 1.08 (25 °C) to obtain valerian extract.

[0058] The above valerian extract was tested and the results showed that the valerin content was 19.2%, the tannin content was 0.3%, and the total bacterial count was <10 CFU / mL.

[0059] Application Examples A method for preparing a water-based inhalation sleep aid product includes the following steps: (1) Formula (based on 1000 g): Weigh 15 g of valerian extract, 3 g of agarwood essential oil, 5 g of lavender essential oil (obtained by molecular distillation at 63 °C and 0.1 Pa, with 58% linalool and 0.4% camphor), 10 g of bitter orange extract, 6 g of orange peel extract, 6 g of vanilla extract, 4 g of sandalwood extract, 4 g of honeysuckle extract (6% chlorogenic acid), 3 g of rosemary extract (4% rosmarinic acid), 35 g of PEG-40 hydrogenated castor oil, 20 g of glycerin, 25 g of propylene glycol, 5 g of hydroxyethyl cellulose, 3 g of sodium alginate, 4 g of calcium sulfate, and 852 g of purified water.

[0060] (2) Add the above-mentioned PEG-40 hydrogenated castor oil, glycerin and propylene glycol to 500 g of purified water, place it in a 40°C constant temperature water bath, stir at 200 r / min for 15 min until completely dissolved to form a clear and transparent mixed solvent.

[0061] (3) Under continuous stirring (200 r / min), valerian extract was first added to the above mixed solvent and stirred at 40 ℃ for 18 min until completely dispersed; then agarwood essential oil, lavender essential oil, bitter orange extract, orange peel extract, vanilla extract, sandalwood extract, honeysuckle extract and rosemary extract were added in sequence. After each ingredient was added, stirring was maintained at 40 ℃ for 18 min to ensure that the ingredients were evenly mixed and that there were no visible oil droplets or precipitates, thus obtaining a mixed solution.

[0062] (4) Add the remaining 367 g of purified water to the above mixed solution, stir for 12 min, transfer the mixture to a high-speed homogenizer, homogenize at 4000 r / min for 6 min to obtain a uniform light yellow-green transparent homogenized solution.

[0063] (5) The above homogenized liquid is filtered through a 0.22 μm microporous membrane to remove any possible residual micro-impurities; then the filtrate is pasteurized in a 62 ℃ constant temperature water bath for 30 min; after sterilization, it is naturally cooled to room temperature and the pH value is measured to be 6.2. Finally, it is filled into a glass bottle with a microporous diffusion device (micropore diameter 0.5 mm to ensure slow release of volatile components) to obtain a water-based inhalation sleep aid product.

[0064] 1. Performance testing of valerian extract The valerian extract prepared in Example 3 was tested for key indicators, namely, the valerin content, tannin content, total bacterial count, and solubility (water at 25 °C). The test results, comparison values ​​with conventional processes, and improvement rates are shown in Table 1.

[0065] Table 1

[0066] The content of valerin and tannin was determined by high performance liquid chromatography (HPLC, column: C18 column, mobile phase: methanol: 0.1% phosphoric acid water = 60: 40, detection wavelength 254 nm); the total bacterial count was determined by plate counting method according to GB 4789.2-2022.

[0067] As shown in Table 1, the present invention can increase the valerin content of the product, reduce the tannin content, reduce the total bacterial count, and produce a product without precipitates, thus significantly improving product quality.

[0068] 2. Stability testing of water-based inhalation sleep aid products The prepared water-based inhalation sleep aid product with valerian extract as the core active ingredient was stored in an accelerated testing chamber at 40 ℃ and 75% relative humidity for 6 months. The appearance, valerin retention rate, lavender essential oil retention rate and total bacterial count were tested periodically. The results are shown in Table 2.

[0069] Table 2

[0070] As can be seen from Table 2, the water-based inhalation sleep aid product prepared by this invention, with valerian extract as the core active ingredient, remains stable under accelerated storage conditions, has a high retention rate of active ingredients, meets the requirements for microbial indicators, and has a shelf life of up to 24 months.

[0071] 3. Safety performance testing of water-based inhalation sleep aid products The prepared water-based inhaled sleep aid product with valerian extract as the core active ingredient was subjected to safety performance testing, namely heavy metal testing, microbial testing, and toxicological verification.

[0072] For heavy metal detection, inductively coupled plasma mass spectrometry (ICP-MS) was used. The results showed that lead was not detected (<1.5 mg / kg), mercury was not detected (<0.002 mg / kg), arsenic (<0.01 mg / kg), and cadmium was detected (<0.18 mg / kg), all of which were far below the limit standards (the limit standards are lead ≤10 mg / kg, mercury ≤1 mg / kg, arsenic ≤2 mg / kg, and cadmium ≤5 mg / kg). Microbiological testing: The water-based inhalation sleep aid product prepared in the application examples was tested according to the "Cosmetic Safety Technical Specifications" (2015 edition). The results showed that the total bacterial count was <10 CFU / mL, the total number of molds and yeasts was <10 CFU / mL, and Escherichia coli, Staphylococcus aureus, and Pseudomonas aeruginosa were not detected. Toxicological validation: Inhalation toxicology and skin irritation tests were conducted. The results of the acute inhalation toxicity test (rat) were: LD50 > 5000 mg / m³ 3 It is practically non-toxic; multiple skin irritation tests (rabbit): skin irritation index (PII) = 0, no irritation; respiratory irritation test (guinea pig): after continuous inhalation for 7 days, there were no respiratory irritation symptoms such as coughing and wheezing, and no pathological changes were found in lung tissue sections.

[0073] 4. Functional verification of water-based inhalation sleep aid products Sixty volunteers aged 18-60 with sleep disorders (meeting the diagnostic criteria of the "Guidelines for the Diagnosis and Treatment of Insomnia in Chinese Adults": sleep onset time > 30 minutes, nighttime awakenings ≥ 2 times, total sleep duration < 6.5 hours) were randomly divided into an experimental group (30 participants) and a control group (30 participants) for a 28-day controlled trial. (1) Objective sleep indicators (PSG monitoring) PSG monitoring was performed on volunteers, and the results are shown in Table 3.

[0074] Table 3

[0075] As shown in Table 3, the water-based inhaled sleep aid product prepared using valerian extract as the core active ingredient can significantly shorten the time to fall asleep, prolong the deep sleep time, reduce the number of nighttime awakenings, and significantly improve sleep efficiency.

[0076] (2) Subjective sleep quality (PSQI score) Subjective sleep quality was monitored in volunteers. The experimental group placed the water-based inhalation sleep aid product prepared according to this invention, with valerian extract as the core active ingredient, near their pillow (30-50 cm from their head) before bedtime each night, using it through natural inhalation for 8 hours each time. The control group used a blank water-based product (containing only PEG-40 hydrogenated castor oil, glycerin, propylene glycol, and water) without any active ingredients, using the same method as the experimental group. Sleep indicators were recorded using a polysomnography (PSG) system during the experiment, and subjective sleep quality was evaluated using the Pittsburgh Sleep Quality Index (PSQI).

[0077] The results showed that the PSQI score in the experimental group decreased from 14.2±2.5 before treatment to 5.3±1.8 after treatment, while that in the control group decreased from 13.8±2.3 to 12.1±2.1. The improvement effect in the experimental group was significantly better than that in the control group (P<0.01), and no volunteers experienced adverse reactions such as dizziness or nausea during the trial.

[0078] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing valerian extract, characterized in that, Includes the following steps: (1) Valerian root and rhizome are dried and pulverized to obtain valerian root and rhizome powder; (2) Add water, compound enzyme and calcium chloride to the valerian root and stem powder, adjust the pH value, and carry out enzymatic hydrolysis under stirring to obtain enzymatic hydrolysate; (3) The valerian extract is obtained by fractional extraction and ultrafiltration purification of the enzymatic hydrolysate.

2. The method for preparing valerian extract according to claim 1, characterized in that, The material described in step (1) is pulverized to pass through an 80-100 mesh sieve.

3. The method for preparing valerian extract according to claim 1, characterized in that, The mass ratio of valerian root powder to water in step (2) is 1:(8-12). The amount of the compound enzyme added is 0.2%-0.5% of the mass of the valerian root and stem powder; The amount of calcium chloride added is 0.05%-0.1% of the mass of the valerian root and stem powder.

4. The method for preparing valerian extract according to claim 3, characterized in that, The compound enzyme is composed of cellulase and pectinase in a mass ratio of 1:2, with an enzyme activity ≥5000 U / g.

5. The method for preparing valerian extract according to claim 1, characterized in that, The pH value mentioned in step (2) is 4.5-5.0; The stirring speed is 150-200 r / min; The enzymatic hydrolysis is performed at a temperature of 35-40 °C for 1.5-2.0 h.

6. The method for preparing valerian extract according to claim 1, characterized in that, The segmented extraction in step (3) is as follows: water is added to the enzymatic hydrolysate until the solid-liquid ratio of the enzymatic hydrolysate is 1 g: 8 mL, and the mixture is extracted at 50-55 ℃ for 1 h. The first extract is obtained by filtration. Water is added to the filter residue, and the mixture is extracted again at 70-75 ℃ for 1 h. The second extract is obtained by filtration. The first extract and the second extract are combined to obtain the crude extract. The ultrafiltration purification is performed as follows: the crude extract is pretreated with a 0.22 μm microporous membrane, and then ultrafiltration is carried out with an ultrafiltration membrane with a molecular weight cutoff of 3000 Da at 0.1-0.15 MPa and 30-35 °C. The permeate is collected and concentrated under reduced pressure to obtain the valerian extract.

7. A valerian extract prepared by the method of any one of claims 1-6.

8. The application of the valerian extract as described in claim 7 in a sleep aid product, characterized in that, The sleep aid product is a water-based inhalation sleep aid product.

9. The application according to claim 8, characterized in that, The water-based inhalation sleep aid product uses the valerian extract as described in claim 7 as its core active ingredient and includes the following components by mass: Valerian extract 0.8%-2.0%, agarwood essential oil 0.1%-0.5%, lavender essential oil 0.2%-0.8%, bitter orange extract 0.5%-1.5%, orange peel extract 0.3%-1.0%, vanilla extract 0.3%-0.9%, sandalwood extract 0.2%-0.6%, honeysuckle extract 0.3%-0.5%, rosemary extract 0.2%-0.4%, PEG-40 hydrogenated castor oil 2.0%-5.0%, glycerin 1.0%-3.0%, propylene glycol 1.5%-4.0%, hydroxyethyl cellulose 0-2%, sodium alginate 0-1.5%, calcium sulfate 0-0.5%, with the balance being purified water.

10. The application according to claim 9, characterized in that, The preparation method of the water-based inhalation sleep aid product includes the following steps: (1) Add the PEG-40 hydrogenated castor oil, glycerin and propylene glycol to water with a mass of 50%-60%, and stir to dissolve at 40 °C to obtain a mixed solvent; (2) Add the valerian extract, agarwood essential oil, lavender essential oil, bitter orange extract, orange peel extract, vanilla extract, sandalwood extract, honeysuckle extract, and rosemary extract to the mixed solvent, mix evenly, then add water again, stir for 10-15 min, and homogenize at 4000 r / min for 5-8 min to obtain a homogenized liquid. (3) The homogenized liquid is filtered through a 0.22 μm microporous membrane, then pasteurized at 60-65 °C for 30 min, and cooled to obtain the water-based inhalation sleep aid product.

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