Preparation process of cinnamon extract, cinnamon extract and application thereof
Patent Information
- Application Number
- CN202611244131.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-08-17
- Publication Date
- 2026-10-30
AI Technical Summary
其中,传统水蒸气蒸馏法是肉桂提取最经典、应用最广泛的工艺,该工艺依托水蒸气携带挥发性成分馏出的原理实现有效成分分离,操作简单、无溶剂残留风险,但现有工艺普遍采用单次高温持续蒸取的单一模式,工艺设计粗放、精细化程度低,存在显著的成分损耗与杂质富集问题
[0006]基于上述问题,本发明的目的在于提供一种肉桂提取液的制备工艺、肉桂提取液及其应用,该制备工艺的活性物质提取率高,可制得高纯度、活性物质复杂的肉桂提取液,其可作为有效成分而应用于除螨喷雾(水)、抑菌喷雾(水)、祛味喷雾(水)、清凉油等领域。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of natural plant active ingredient extraction technology, and in particular to the preparation process of cinnamon extract, cinnamon extract and its applications. Background Technology
[0002] Cinnamon, the dried bark of the genus *Cinnamomum* in the Lauraceae family, is a traditional Chinese medicinal and edible ingredient. Rich in various active components such as cinnamaldehyde, cinnamic acid, coumarins, and terpenes, it possesses multiple beneficial effects including antibacterial, anti-inflammatory, antioxidant, warming and invigorating properties, and flavor enhancement. It is widely used in food flavorings, biomedicine, cosmetics, and health products. The purity, yield, and cleanliness of the active ingredients extracted from cinnamon directly determine the quality, safety, and market value of processed cinnamon products. Therefore, efficient, green, and high-purity extraction technology for cinnamon's active ingredients has always been a research hotspot in this field.
[0003] Currently, the extraction processes for the effective components of cinnamon in industry and laboratories still mainly rely on two major technologies: traditional steam distillation and organic chemical solvent extraction. Although these two conventional processes are technically mature and have strong equipment adaptability, enabling the large-scale preparation of crude cinnamon extracts, they have many unavoidable technical defects in actual production applications, which seriously restrict the industrialization and high-end application of high-purity, high-activity cinnamon extracts. Among them, traditional steam distillation is the most classic and widely used process for cinnamon extraction. This process relies on the principle that steam carries volatile components to achieve the separation of effective ingredients. It is simple to operate and has no risk of solvent residue. However, existing processes generally adopt a single high-temperature continuous distillation mode, which is crude in process design and has a low degree of refinement, resulting in significant component loss and impurity enrichment. On the one hand, during single high-temperature distillation, the temperature inside the vessel is constant and the overall temperature is relatively high. Thermosensitive active ingredients in cinnamon, such as some low-boiling-point terpenes, are prone to high-temperature oxidation, decomposition, and polymerization failure, and cannot be effectively distilled out and retained, resulting in a low overall yield of effective ingredients and a significant reduction in activity. At the same time, single distillation cannot achieve fractional distillation, and high-boiling-point effective ingredients are difficult to fully extract. A large amount of effective ingredients remain in the cinnamon residue, resulting in extremely low raw material utilization and a serious waste of high-quality medicinal and spice resources. On the other hand, single, undifferentiated high-temperature distillation will distill off non-target inert impurities in the cinnamon raw material, such as plant waxes, resins, pigments, and coarse fiber debris, along with the steam. The crude essential oil will contain a large number of mechanical impurities and high-molecular-weight inert impurities, resulting in poor purity, high impurity content, and cloudy color of the extract. Subsequent complex purification and refining processes are required, significantly increasing production energy consumption and labor costs. Moreover, the refining process will cause secondary loss of effective components, making it difficult to balance yield and purity. In addition, single high-temperature, long-duration distillation can easily cause excessive volatilization of the main component, cinnamaldehyde, and an imbalance in component ratio, destroying the natural complex aroma and pharmacological activity of the cinnamon extract, failing to meet the quality requirements of high-end fragrances and pharmaceutical preparations.
[0004] To address the insufficient purity of steam distillation, existing technologies often employ chemical organic solvent extraction to purify cinnamon raw materials. Commonly used solvents include ethanol, diethyl ether, petroleum ether, and ethyl acetate. While this process can selectively dissolve some large-molecule inert impurities and improve extract purity, it has inherent drawbacks and safety hazards, making it unsuitable for the production standards of high-end food and pharmaceutical products. Firstly, chemical solvents have limited selectivity; while dissolving the target active ingredient, they also readily dissolve large amounts of non-water-soluble impurities such as resins, colloids, and tannins from the raw material. This results in poor targeting of impurities, limited purification effects, and difficulty in obtaining high-purity monomer components. Secondly, the risk of organic solvent residue is extremely high. The crude extract requires multiple desolventizing processes, and even after conventional distillation desolventizing, trace amounts of solvent can still remain in the extract, failing to meet food and pharmaceutical safety standards and severely limiting the product's application in safety-sensitive areas such as oral health supplements, pharmaceutical preparations, and baby and maternal and infant products. Third, chemical solvent extraction processes are flammable, explosive, and highly corrosive, requiring extremely high levels of sealing and explosion-proof capabilities in production equipment. This results in significant safety risks during production, high solvent recovery and loss rates, high production costs, and substantial environmental pressure. Fourth, solvent extraction processes can easily lead to excessive loss of polar and weakly polar active ingredients in cinnamon, damaging the integrity of the active ingredient system and causing a significant decline in the pharmacological efficacy and quality of the extract.
[0005] In summary, current mainstream cinnamon extraction processes suffer from several core technological bottlenecks, including significant component loss during single distillation, high impurity content, low raw material utilization, high risk of solvent extraction residues, poor safety, and weak purification targeting. Existing single processes cannot simultaneously meet the production demands of high yield, high purity, high activity, green safety, and low cost, severely hindering the high-quality and green upgrading of the cinnamon deep processing industry. Therefore, developing a novel cinnamon active ingredient extraction process that circumvents the defects of existing processes, is suitable for large-scale production, efficiently retains heat-sensitive active ingredients, thoroughly removes impurities, and leaves no harmful residues has become a pressing technical problem for those skilled in the art. Summary of the Invention
[0006] Based on the above problems, the purpose of this invention is to provide a preparation process for cinnamon extract, cinnamon extract and its application. The preparation process has a high extraction rate of active substances and can produce a high-purity cinnamon extract with complex active substances. It can be used as an effective ingredient in mite-removing spray (water), antibacterial spray (water), deodorizing spray (water), mentholatum and other fields.
[0007] To achieve the above objectives, the first aspect of the present invention provides a process for preparing cinnamon extract, comprising the following steps: (I) Preprocessing Select cinnamon bark, remove dead branches, cut into small pieces, wash, and air-dry in a ventilated and shaded place until the moisture content is 12~18wt.%; (II) Steam distillation The distillate is placed in a sealed distillation vessel and steam from a boiler is introduced. The first stage of distillation is carried out at 40-65℃, followed by the second stage at 70-95℃, and then the third stage at 98-112℃ to obtain the distillate. (III) Static stratification After the distillate is allowed to stand at 8-15°C to separate into layers, the lower layer of cinnamon extract is taken. (IV) Filtration The cinnamon extract was first filtered through a large-pore membrane and then through a small-pore membrane to obtain the cinnamon extract.
[0008] This invention employs gradient heating steam distillation, which enables low-temperature pre-distillation, medium-temperature main extraction, and high-temperature tail-end recovery to gradually release active substances with different boiling points from the cinnamon bark layer, thereby reducing the high-temperature decomposition loss of eugenol and cinnamaldehyde. The specific mechanism is as follows.
[0009] The first stage of distillation is carried out at a low temperature of 40~65℃. This low steam temperature can gently open up the pore structure of the cortex and trigger the azeotropic distillation of low-boiling-point light active components, so that volatile aroma substances can be distilled out quickly, gently and in a short time, thus achieving pre-purification of raw materials. The low temperature will not forcibly break down oil gland cells, and will not carry out a large amount of medium-boiling-point cinnamaldehyde and eugenol, thus avoiding the premature release of main components due to high temperature damage.
[0010] Since the first stage of distillation at a low temperature of 40-65℃ has already completed the opening of pores and the evacuation of light components, the second stage of distillation at a low temperature of 70-95℃ allows steam to penetrate the cinnamon phloem oil gland tissue at a uniform, stable, and continuous rate. This ensures the smooth and uniform release of cinnamaldehyde, eugenol, and other compounds encapsulated deep within the fibers, preventing high-temperature emulsification, high-temperature polymerization, and component denaturation caused by sudden large-scale overflow. Within this temperature range, cinnamaldehyde, eugenol, and other compounds are effectively azeotropically distilled without thermal degradation.
[0011] The temperature is then increased to 98~112℃ for a third stage of distillation. The higher temperature enhances the penetration of steam, breaks the deep and stubborn oil gland encapsulation structure, and fully recovers high-boiling-point functional components such as cinnamon acetate and monoterpenoids, thereby comprehensively improving the overall activity complexity and extraction rate of cinnamon extract.
[0012] This invention employs a gradient-temperature steam distillation process—low-temperature pre-steaming, medium-temperature main extraction, and high-temperature tail-end recovery—to replace the traditional single-stage constant-temperature distillation process, thereby improving the complexity and extraction rate of active ingredients. However, the inventors discovered that if high-moisture-content cinnamon bark is used for gradient-temperature steam distillation, the raw material fibers absorb water and swell, causing pore blockage and hindering steam permeation. This leads to material agglomeration and steam short-circuiting. The gradient-temperature distillation only affects the surface layer of the raw material, making it difficult to achieve orderly fractional distillation of components with different boiling points. Simultaneously, the large amount of free water in the raw material promotes the continuous co-distillation of water-soluble impurities such as gums, tannins, and pigments, and exacerbates the hydrolysis side reactions of active ingredients, significantly reducing their extraction rate. Therefore, this problem can be effectively solved by first removing dead branches from the cinnamon bark, cutting it into small pieces, and then air-drying it to remove a large amount of free water, achieving a low moisture content of 12-18 wt.%. After a large amount of free water is removed from cinnamon bark, the fibrous tissue forms continuous porous channels, and the oil gland cells are more susceptible to structural stress due to dehydration and are more easily wetted and ruptured by water vapor. At the same time, the amount of endogenous free water in the raw material is reduced, which lowers the water activity of the system and effectively inhibits the hydrolysis, polymerization and deterioration of heat-sensitive active ingredients such as cinnamaldehyde, terpenes and coumarins under humid and hot conditions.
[0013] Furthermore, the distillate obtained after gradient-heating steam distillation is a relatively stable emulsion system. It is then allowed to stand at a low temperature of 8-15℃ to separate into layers. This low temperature weakens the stability of the oil-water emulsion system, promotes the aggregation of dispersed micro-essential oil droplets, accelerates the separation of the oil and water phases, and forms a clear interface after separation. Simultaneously, it reduces the solubility of waxes and high-molecular-weight resin impurities in the oil phase, causing these impurities to precipitate and accumulate at the phase interface, achieving preliminary impurity removal. In addition, the low-temperature environment can inhibit the oxidation and polymerization side reactions of high-content cinnamaldehyde and eugenol, reducing the deterioration and loss of active ingredients. Using purely physical purification without chemical solvent extraction significantly improves its purity. The cinnamon concentrate after standing is then filtered using a two-stage pore size gradient filter consisting of a large-pore membrane and a small-pore membrane. This process can intercept large-molecule ineffective impurities and selectively retain small-molecule antibacterial active ingredients, thus further improving its purity and preserving its antibacterial efficacy.
[0014] As one technical solution of the present invention, the cutting is carried out to a small segment with a length of 2-5cm.
[0015] As one technical solution of the present invention, the distillation time of the first stage of distillation is 2-5 hours, the distillation time of the second stage of distillation is 4-8 hours, and the distillation time of the third stage of distillation is 1-3 hours.
[0016] As one technical solution of the present invention, the static stratification time is 12~36h.
[0017] As one technical solution of the present invention, the pore size of the large-pore filter membrane is 5~20μm, and the pore size of the small-pore filter membrane is 0.2~1.0μm.
[0018] A second aspect of the present invention provides a cinnamon extract prepared by the aforementioned cinnamon extract preparation process, wherein the active substances comprise ≥96.0% by mass, and the active substances include 70.0~91.5 wt.% trans-o-methoxycinnamonaldehyde, 4.0~25.5 wt.% cinnamyl acetate, 4.0~25.5 wt.% eugenol, and 0.5~10.0 wt.% monoterpenoids. This cinnamon extract has high content of active ingredients such as trans-o-methoxycinnamonaldehyde, cinnamyl acetate, eugenol, and monoterpenoids, and can be used as an effective ingredient in products such as mite-repellent sprays (water), antibacterial sprays (water), deodorizing sprays (water), and mentholatum.
[0019] As a technical solution of the present invention, the extraction rate of trans-o-methoxycinnamoaldehyde is 30-55%, the extraction rate of cinnamoyl acetate is 15-40%, the extraction rate of eugenol is 15-40%, and the extraction rate of monoterpenoid compounds is 30-50%. A third aspect of the present invention provides the application of the aforementioned cinnamon extract in mite-removing sprays, antibacterial sprays, or deodorizing sprays.
[0020] The fourth aspect of the present invention provides the application of the aforementioned cinnamon extract in mite-removing water, antibacterial water, or deodorizing water.
[0021] The fifth aspect of the present invention provides the application of the aforementioned cinnamon extract in mentholatum. Detailed Implementation
[0022] This invention provides a cinnamon extract with an active ingredient content ≥96.0% by mass. The active ingredients include at least trans-o-methoxycinnamoaldehyde, cinnamyl acetate, eugenol, and monoterpenoids. Trans-o-methoxycinnamoaldehyde is highly effective at inhibiting bacteria and killing mites, exhibiting long-lasting inhibitory effects on household bacteria and dust mites. Cinnamyl acetate and eugenol soothe irritation, eliminate odors, and possess antioxidant properties, preventing product spoilage during storage. Terpenoids synergistically enhance the effects of trans-o-methoxycinnamoaldehyde, cinnamyl acetate, and eugenol, providing a gentle and non-irritating effect on the skin. The active ingredients comprise 70.0–91.5 wt.% trans-o-methoxycinnamoaldehyde, 4.0–25.5 wt.% cinnamyl acetate, 4.0–25.5 wt.% eugenol, and 0.5–10.0 wt.% monoterpenoids. Because this cinnamon extract contains high levels of active ingredients such as trans-o-methoxycinnamaldehyde, cinnamyl acetate, eugenol, and monoterpenoids, it can be used as an effective ingredient in products such as mite-removing sprays (water), antibacterial sprays (water), odor-removing sprays (water), and mentholatum.
[0023] As one application technology solution, this invention provides a cinnamon mite-repellent spray, the raw materials of which include 4-16 wt.% of the aforementioned cinnamon extract, 2-9 wt.% of plant-based mite-repellent adjuvants, 1-10 wt.% of atomizing solvent, and the balance being water. The plant-based mite-repellent adjuvants may be, but are not limited to, at least one selected from honeysuckle flower extract, soapberry fruit extract, artemisia leaf extract, sophora root extract, peppermint extract, purslane extract, and safflower extract. The extraction methods for each extract in the plant-based mite-repellent adjuvants can employ industry-known techniques. Using plant-based adjuvants with mite-repellent activity, such as sophora root extract and soapberry fruit extract, deep mite removal from fabrics can be effectively achieved. Combined with cinnamon extract, which has antibacterial and mite-killing effects, a cinnamon mite-repellent spray with mite-repellent, antibacterial, and air-purifying effects can be prepared for fabrics. The atomizing solvent may be, but is not limited to, at least one selected from propylene glycol and glycerol. During preparation, each raw material is accurately weighed according to the determined ratio, stirred and homogenized at room temperature, and then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into a special spray bottle, sealed, and subjected to preliminary inspections of appearance, dosage, pH value, and other items to ensure that the product quality is up to standard.
[0024] As one application technology solution, this invention provides an antibacterial spray, the raw materials of which include 3-20 wt.% of the aforementioned cinnamon extract, 1-10 wt.% of a mild antibacterial component, 1-10 wt.% of a moisturizing solvent, and the balance being water. The mild antibacterial component is a mixture of natural plant antibacterial agents and synthetic compound antibacterial agents. The natural antibacterial agent is selected from at least one of the following: black willow bark extract, tea tree oil, chitosan, eucalyptus oil, artemisia extract, stemona extract, dictamnus root bark extract, angelica root extract, chuanxiong extract, and clove extract. The extraction methods for each extract in the natural antibacterial agent can be techniques known in the industry. The synthetic antibacterial compound is selected from at least one of benzyl chloride, polyhexamethylene guanidine, benzalkonium chloride, benzalkonium bromide, imidazolidinyl urea, methylisothiazolinone, methylchloroisothiazolinone, 2-butyl-1,2-benzisothiazolin-3-one, 2-methyl-1,2-benzene, dimethyloctadecyl[3-trimethoxysilylpropyl]ammonium chloride, triclosan, triclocarban, iodopropynylcarbamate, and 1,3-dihydroxymethyl-5,5-dimethylhydantoin. The moisturizing solvent may be, but is not limited to, at least one of ethanol, ethylene glycol, 1,2-propanediol, glycerol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, 1,4-butanediol, 1,2-pentanediol, diethylene glycol, and triethylene glycol. This antibacterial spray has skin-antibacterial and gentle protective effects. During preparation, each raw material is accurately weighed according to the determined ratio, stirred and homogenized at room temperature, and then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into a special spray bottle, sealed, and subjected to preliminary inspections of appearance, dosage, pH value, and other items to ensure that the product quality is up to standard.
[0025] As one application technology solution, this invention provides a mite-removing spray, the raw materials of which include 5-15 wt.% of the aforementioned cinnamon extract, 1-10 wt.% of a plant-based mite-removing extract, 1-10 wt.% of a deodorizing agent, and the balance being water. The plant-based mite-removing extract is selected from at least one of lavender oil, rosemary leaf oil, lemon peel oil, geranium flower oil, and sophora root extract. The extraction methods for each extract of the plant-based mite-removing extract can be techniques known in the industry. Further, the mass ratio of lavender oil, rosemary leaf oil, lemon peel oil, geranium flower oil, and sophora root extract is 1:0.5-2.0:0.2-0.8:2.3-5.5:0.1-0.8. Preferably, a plant-based mite-removing extract is composed of lavender oil, rosemary leaf oil, lemon peel oil, geranium flower oil, and sophora flavescens root extract, which is mixed with cinnamon concentrate, which has antibacterial properties, and applied to the spray. This allows the spray to effectively inhibit or kill pathogenic microorganisms while also eliminating mites without irritating the human body. The deodorizing agent is selected from at least one of grapefruit peel extract, peppermint oil, and eucalyptus oil. Among these, lavender oil, rosemary leaf oil, lemon peel oil, and geranium flower oil are essential oil-based raw materials, which not only focus on space spraying and odor removal but also address mite control. Further addition of the deodorizing agent can harmonize the strong medicinal aroma of cinnamon and optimize the finished product's scent. During preparation, each raw material is accurately weighed according to the determined ratio, stirred and homogenized at room temperature, and then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into a special spray bottle, sealed, and subjected to preliminary inspections of appearance, dosage, pH value, and other items to ensure that the product quality is up to standard.
[0026] As one application technology solution, this invention provides a cinnamon cooling oil, the raw materials of which include 1-10 wt.% of the aforementioned cinnamon extract, 5-15 wt.% of menthol, 1-10 wt.% of eucalyptus oil, 60-75 wt.% of petrolatum, and 10-20 wt.% of beeswax carrier. The high content of cinnamon acetate and eugenol in the cinnamon extract can soothe irritation and remove odors. Terpenoids can synergistically enhance the effects of cinnamon acetate and eugenol, making it gentle and non-irritating to the skin, mitigating the irritation of menthol, and optimizing the product's aroma. Menthol is the core cooling functional component, stimulating the skin's cold receptors to achieve rapid mental alertness, itch relief, and cooling. Eucalyptus oil plays a supporting role in cooling, antibacterial, and nasal decongestion, while also solubilizing various volatile components. Petrolatum, as an oil carrier, can dissolve various volatile active substances, forming a protective film on the skin surface, slowing down the volatilization of active ingredients, and reducing skin irritation. Beeswax, used as a molding matrix, regulates the hardness and melting characteristics of the ointment, ensuring it remains solid at room temperature for easy application. It also inhibits component crystallization, prevents stratification and oil separation during long-term storage, and guarantees the physical stability of the system. The components work synergistically to create a gentle, refreshing, itch-relieving, and dizziness-soothing balm that is stable. In preparation, petrolatum and beeswax carrier are first melted, cooled, and then menthol is added. Eucalyptus oil and cinnamon extract are then slowly added sequentially, stirring until all oily active components are completely miscible with the oil matrix, resulting in a homogeneous and transparent system without stratification, floating oil, or flocculent precipitates. Temperature is strictly controlled throughout the process to minimize the loss of active substances from the cinnamon extract due to volatilization. After homogenization and stirring, the mixture is allowed to stand at normal pressure to remove bubbles before being quantitatively filled into containers.
[0027] As one application technology solution, this invention provides an odor-removing spray, the raw materials of which include 3-20 wt.% of the aforementioned cinnamon extract, 5-20 wt.% of plant-based odor-removing ingredients, 1-10 wt.% of a mild solvent, and the balance being water. The plant-based odor-removing ingredients are selected from at least one of green tea extract, rose extract, soapberry extract, sophora flavescens root extract, aloe vera leaf extract, sanguisorba officinalis root extract, citrus peel extract, and pine bark extract. The extraction methods for each extract in the plant-based odor-removing ingredients can employ industry-known techniques. The mild solvent is selected from 1,2-butanediol and / or 1,3-propanediol. The high content of cinnamon acetate and eugenol in the cinnamon extract can remove odors, and terpenoid compounds can synergistically enhance the aroma of the product with cinnamon acetate and eugenol. Therefore, by combining the cinnamon extract, plant-based odor-removing ingredients, mild solvent, and water of this invention, an odor-removing spray that decomposes odors and has antibacterial and fragrance-retaining properties can be obtained. During preparation, each raw material is accurately weighed according to the determined ratio, stirred and homogenized at room temperature, and then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into a special spray bottle, sealed, and subjected to preliminary inspections of appearance, dosage, pH value, and other items to ensure that the product quality is up to standard.
[0028] As one application technology solution, this invention provides an antibacterial mop water, the raw materials of which include 5-25 wt.% of the aforementioned cinnamon extract, 3-15 wt.% of surfactant, 0.5-5.0 wt.% of detergent, and the balance being water. The surfactant is selected from at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, and alkyl glycoside. The detergent is selected from at least one of sodium citrate, lauryl ether ammonium sulfate, sodium dodecyl sulfate, ammonium dodecyl sulfate, and sodium α-olefin sulfonate. The cinnamon extract contains high levels of trans-o-methoxycinnamaldehyde, cinnamyl acetate, eugenol, and monoterpenoids. Trans-o-methoxycinnamaldehyde has strong antibacterial and mite-killing effects, and a long-lasting inhibitory effect on household bacteria and dust mites. Cinnamyl acetate and eugenol can remove odors and have antioxidant effects. Terpenoids can synergistically enhance the effects of trans-o-methoxycinnamaldehyde, cinnamyl acetate, and eugenol. Therefore, the cinnamon extract, surfactant, detergent, and water of this invention can be combined to prepare a cleaning and antibacterial mop. During preparation, each raw material is accurately weighed according to a predetermined ratio, stirred and homogenized at room temperature, and then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into a dedicated spray bottle, sealed, and subjected to preliminary inspections of appearance, dosage, pH value, etc., to ensure product quality.
[0029] The preparation process of the cinnamon extract of the present invention includes the following steps: (I) Preprocessing Select cinnamon bark, remove dead branches, cut into small pieces, wash, and air-dry in a ventilated and shaded place until the moisture content is 12~18wt.%; (II) Steam distillation The distillate is placed in a sealed distillation vessel and steam from a boiler is introduced. The first stage of distillation is carried out at 40-65℃, followed by the second stage at 70-95℃, and then the third stage at 98-112℃ to obtain the distillate. (III) Static stratification After the distillate is allowed to stand at 8-15℃ to separate into layers, the lower layer of cinnamon extract is taken. (IV) Filtration The cinnamon extract was first filtered through a large-pore membrane and then through a small-pore membrane to obtain the cinnamon extract.
[0030] This preparation process involves first removing dead branches from cinnamon bark and cutting it into small segments, then air-drying it to remove a large amount of free moisture, achieving a low moisture content of 12-18 wt.%. By controlling the moisture content, the advantages of gradient-temperature steam distillation can be effectively utilized. Gradient-temperature steam distillation allows for low-temperature pre-distillation, medium-temperature main extraction, and high-temperature tail-end recovery, gradually releasing active substances with different boiling points from the cinnamon bark layer and reducing the high-temperature decomposition loss of eugenol and cinnamaldehyde. Combined with static layering at 8-15℃ and two-stage pore size gradient filtration, high extraction rates of trans-o-methoxycinnamaldehyde, cinnamyl acetate, eugenol, and monoterpenoids can be achieved. Specifically, the extraction rates of trans-o-methoxycinnamaldehyde are 30-55%, cinnamyl acetate is 15-40%, eugenol is 15-40%, and monoterpenoids are 30-50%.
[0031] Furthermore, the material is cut into small segments of 2-5 cm in length during preparation to facilitate subsequent steam distillation. The distillation time for the first stage is 2-5 hours, the second stage is 4-8 hours, and the third stage is 1-3 hours. The settling time for stratification is 12-36 hours. The pore size of the large-pore filter membrane is 5-20 μm, and the pore size of the small-pore filter membrane is 0.2-1.0 μm.
[0032] To better illustrate the purpose, technical solution, and beneficial effects of this invention, the invention will be further described below with reference to specific embodiments. It should be noted that the methods described below are further explanations of this invention and should not be construed as limiting it.
[0033] Part 1: Preparation of Cinnamon Extract Example 1 This embodiment describes a preparation process for cinnamon extract, which includes the following steps.
[0034] (I) Preprocessing The cinnamon trees selected are Xijiang cinnamon trees over 3 years old from Gaoliang Town, Deqing County. Only the middle layer of bark is used. Old bark, tender branches, and rotten materials are removed. The pieces are cut into sections of about 3cm, rinsed with running water to remove surface dirt, and air-dried in a cool and ventilated place to control the overall moisture content to 15wt.%.
[0035] (II) Steam distillation The feed is added to a sealed stainless steel distillation vessel, with the amount added at one time controlled to 60-70% of the vessel's volume. Saturated steam generated by the boiler is introduced from the bottom of the vessel. The first stage of distillation is carried out by holding the vessel at 55℃ for 4 hours, followed by the second stage of distillation by holding the vessel at 90℃ for 7 hours, and then the third stage of distillation is carried out by holding the vessel at 100℃ for 2 hours. The temperature is lowered to below 25℃ by circulating cooling water, and the distillate is collected.
[0036] (III) Static stratification After the distillate was allowed to stand at 10°C for 30 hours to separate into layers, the lower layer of cinnamon extract was collected.
[0037] (IV) Filtration The cinnamon extract was first filtered through a 10μm large-pore membrane and then through a 0.5μm small-pore membrane to obtain the cinnamon extract. The obtained cinnamon extract was analyzed for its components. The analysis revealed that the cinnamon extract contained 70.0 wt.% trans-o-methoxycinnamonaldehyde, 14.0 wt.% cinnamon acetate, 11.5 wt.% eugenol, and 2.5 wt.% monoterpenoids. Furthermore, the extraction rates of each component were determined using HPLC: trans-o-methoxycinnamonaldehyde was extracted at 50%, cinnamon acetate at 28%, eugenol at 26%, and monoterpenoids at 45%. The formula for calculating the extraction rate is as follows.
[0038] Extraction rate (%) = (Target component content in extract × Extract mass / Total target component in raw material) × 100% Example 2 This embodiment describes a preparation process for cinnamon extract, which includes the following steps.
[0039] (I) Preprocessing We select Xijiang cinnamon trees aged over 3 years from Gaoliang Town, Deqing County, and only take the middle layer of bark from the trunk. We remove old bark, tender branches, and rotten materials, cut them into sections of about 4cm, rinse the surface mud and sand with running water, and air dry them naturally in a cool and ventilated place, controlling the overall moisture content to 18wt.%.
[0040] (II) Steam distillation The feed is added to a sealed stainless steel distillation vessel, with the amount added at one time controlled to 60-70% of the vessel's volume. Saturated steam generated by the boiler is introduced from the bottom of the vessel. The first stage of distillation is carried out by holding the temperature at 65℃ for 3 hours, followed by the second stage of distillation by holding the temperature at 85℃ for 4 hours, and then the third stage of distillation by holding the temperature at 110℃ for 3 hours. The temperature is then lowered to below 25℃ by circulating cooling water, and the distillate is collected.
[0041] (III) Static stratification After the distillate was allowed to stand at 13°C for 36 hours to separate into layers, the lower layer of cinnamon extract was collected.
[0042] (IV) Filtration The cinnamon extract was first filtered through a 15μm large-pore membrane and then through a 1.0μm small-pore membrane to obtain the cinnamon extract. The obtained cinnamon extract was analyzed for its components. The analysis revealed that the cinnamon extract contained 71.0 wt.% trans-o-methoxycinnamonaldehyde, 13.0 wt.% cinnamon acetate, 11.0 wt.% eugenol, and 2.0 wt.% monoterpenoids. Furthermore, the extraction rates of each component were determined using HPLC: trans-o-methoxycinnamonaldehyde was 47%, cinnamon acetate was 25%, eugenol was 24%, and monoterpenoids were 40%. Comparative Example 1 This comparative example illustrates a preparation process for cinnamon extract, comprising the following steps.
[0043] (I) Preprocessing The cinnamon trees selected are Xijiang cinnamon trees over 3 years old from Gaoliang Town, Deqing County. Only the middle layer of bark is used. Old bark, tender branches, and rotten materials are removed. The pieces are cut into sections of about 3cm, rinsed with running water to remove surface dirt, and air-dried in a cool and ventilated place to control the overall moisture content to 30wt.%.
[0044] (II) Steam distillation The feed is added to a sealed stainless steel distillation vessel, with the amount added at one time controlled to 60-70% of the vessel's volume. Saturated steam generated by the boiler is introduced from the bottom of the vessel. The first stage of distillation is carried out by holding the vessel at 55℃ for 4 hours, followed by the second stage of distillation by holding the vessel at 90℃ for 7 hours, and then the third stage of distillation is carried out by holding the vessel at 100℃ for 2 hours. The temperature is lowered to below 25℃ by circulating cooling water, and the distillate is collected.
[0045] (III) Static stratification After the distillate was allowed to stand at 10°C for 30 hours to separate into layers, the lower layer of cinnamon extract was collected.
[0046] (IV) Filtration The cinnamon extract was first filtered through a 10μm large-pore membrane and then through a 0.5μm small-pore membrane to obtain the cinnamon extract. The obtained cinnamon extract was analyzed for its components. The analysis revealed that the cinnamon extract contained 57.0 wt.% trans-o-methoxycinnamonaldehyde, 1.0 wt.% cinnamon acetate, 2.0 wt.% eugenol, and 0.5 wt.% monoterpenoids. Furthermore, the extraction rates of each component were determined using HPLC: trans-o-methoxycinnamonaldehyde was extracted at 25%, cinnamon acetate at 4%, eugenol at 6%, and monoterpenoids at 3%. Comparative Example 2 This comparative example illustrates a preparation process for cinnamon extract, comprising the following steps.
[0047] (I) Preprocessing The cinnamon trees selected are Xijiang cinnamon trees over 3 years old from Gaoliang Town, Deqing County. Only the middle layer of bark is used. Old bark, tender branches, and rotten materials are removed. The pieces are cut into sections of about 3cm, rinsed with running water to remove surface dirt, and air-dried in a cool and ventilated place to control the overall moisture content to 15wt.%.
[0048] (II) Steam distillation Feed the material into a sealed stainless steel distillation vessel, controlling the amount of material fed at one time to 60-70% of the vessel's volume. Saturated steam generated by the boiler is introduced from the bottom of the vessel. Distillation is carried out at 100℃ for 10 hours, and then the temperature is lowered to below 25℃ by circulating cooling water. The distillate is then collected.
[0049] (III) Static stratification After the distillate was allowed to stand at 10°C for 30 hours to separate into layers, the lower layer of cinnamon extract was collected.
[0050] (IV) Filtration The cinnamon extract was first filtered through a 10μm large-pore membrane and then through a 0.5μm small-pore membrane to obtain the cinnamon extract. The obtained cinnamon extract was analyzed for its components. The analysis revealed that the cinnamon extract contained 50.0 wt.% trans-o-methoxycinnamonaldehyde, 0.5 wt.% cinnamon acetate, and 0.5 wt.% eugenol; monoterpenoids were not detected. Furthermore, the extraction rates of each component were determined using HPLC: trans-o-methoxycinnamonaldehyde was extracted at 20%, cinnamon acetate at 2%, and eugenol at 3%. Comparative Example 3 This comparative example illustrates a preparation process for cinnamon extract, comprising the following steps.
[0051] (I) Preprocessing The cinnamon trees selected are Xijiang cinnamon trees over 3 years old from Gaoliang Town, Deqing County. Only the middle layer of bark is used. Old bark, tender branches, and rotten materials are removed. The pieces are cut into sections of about 3cm, rinsed with running water to remove surface dirt, and air-dried in a cool and ventilated place to control the overall moisture content to 15wt.%.
[0052] (II) Steam distillation The feed is added to a sealed stainless steel distillation vessel, with the amount added at one time controlled to 60-70% of the vessel's volume. Saturated steam generated by the boiler is introduced from the bottom of the vessel. The first stage of distillation is carried out by holding the vessel at 55℃ for 4 hours, followed by the second stage of distillation by holding the vessel at 90℃ for 7 hours, and then the third stage of distillation is carried out by holding the vessel at 100℃ for 2 hours. The temperature is lowered to below 25℃ by circulating cooling water, and the distillate is collected.
[0053] (III) Static stratification After the distillate was allowed to stand at room temperature for 30 hours to separate into layers, the lower layer of cinnamon extract was collected.
[0054] (IV) Filtration The cinnamon extract was first filtered through a 10μm large-pore membrane and then through a 0.5μm small-pore membrane to obtain the cinnamon extract. The obtained cinnamon extract was analyzed for its components. The analysis revealed that the cinnamon extract contained 65.0 wt.% trans-o-methoxycinnamonaldehyde, 6.0 wt.% cinnamon acetate, 3.0 wt.% eugenol, and 0.5 wt.% monoterpenoids. Furthermore, the extraction rates of each component were determined using HPLC: trans-o-methoxycinnamonaldehyde was 25%, cinnamon acetate was 15%, eugenol was 12%, and monoterpenoids were 30%. Part Two: Product Applications of Cinnamon Extract Experiment 1: The cinnamon extracts from Examples 1-2 and Comparative Examples 1-3 were used to prepare cinnamon anti-mite sprays #1-5.
[0055] The raw materials for this cinnamon mite-repellent spray include 10 wt.% of cinnamon extract from Examples 1-2 and Comparative Examples 1-3, 3 wt.% of Sophora flavescens root extract, 3 wt.% of Sapindus mukorossi fruit extract, 3 wt.% of Artemisia argyi extract, 8 wt.% of propylene glycol, and the balance being water. According to the determined ratio, each raw material is accurately weighed and homogenized at room temperature. The mixture is then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into dedicated spray bottles, and the filled spray is sealed to obtain cinnamon mite-repellent sprays #1-5.
[0056] Cinnamon mite-killing sprays #1-#5 were used for mite control testing. Two hundred test mites (house dust mites, adult males and females, and nymphs) were placed in containers, and 5 mL of each spray was sprayed into the containers. The number of dead mites was obtained after 48 hours, and the mite control rate was calculated. A control group was used without any mite-killing spray. The mite control results are shown in Table 1.
[0057] Table 1. Mite-killing test results of cinnamon mite-killing sprays #1-#5
[0058] As shown in Table 1, the cinnamon extracts from Examples 1 and 2 can achieve better mite-removal effects when used in mite-removal sprays.
[0059] Experiment 2: The cinnamon extracts from Examples 1-2 and Comparative Examples 1-3 were used to prepare antibacterial sprays 1-5#.
[0060] The raw materials for this antibacterial spray include 15 wt.% of cinnamon extract from Examples 1-2 and Comparative Examples 1-3, 4 wt.% of tea tree oil, 3 wt.% of clove extract, 1 wt.% of polyhexamethylene guanidine, 6 wt.% of glycerol, and the balance being water. According to the determined ratio, each raw material is accurately weighed and homogenized at room temperature. The solution is then filtered through a precision filter to remove impurities and particles. The filtered solution is then filled into dedicated spray bottles, and the filled spray is sealed to obtain antibacterial sprays 1-5#.
[0061] Antibacterial properties were tested using antibacterial sprays #1-#5, with testing conditions referencing the standard "QB / T 2738-2023 Evaluation Method for Antibacterial and Antimicrobial Effects of Daily Chemical Products". The results are shown in Table 2.
[0062] Table 2. Test results of antibacterial performance of antibacterial sprays #1-#5
[0063] As shown in Table 2, the cinnamon extracts from Examples 1 and 2 can achieve better antibacterial effects when used in antibacterial sprays.
[0064] Finally, 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 scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, it is not limited to those listed in the embodiments. Those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.
Claims
1. A preparation process for cinnamon extract, characterized in that, Including the following steps: (I) Preprocessing Select cinnamon bark, remove dead branches, cut into small pieces, wash, and air-dry in a ventilated and shaded place until the moisture content is 12~18wt.%; (II) Steam distillation The distillate is placed in a sealed distillation vessel and steam from a boiler is introduced. The first stage of distillation is carried out at 40-65℃, followed by the second stage at 70-95℃, and then the third stage at 98-112℃ to obtain the distillate. (III) Static stratification After the distillate is allowed to stand at 8-15°C to separate into layers, the lower layer of cinnamon extract is taken. (IV) Filtration The cinnamon extract was first filtered through a large-pore membrane and then through a small-pore membrane to obtain the cinnamon extract.
2. The preparation process of cinnamon extract according to claim 1, characterized in that, The pieces are cut into segments with a length of 2-5 cm.
3. The preparation process of cinnamon extract according to claim 1, characterized in that, The distillation time for the first stage of distillation is 2-5 hours, the distillation time for the second stage of distillation is 4-8 hours, and the distillation time for the third stage of distillation is 1-3 hours.
4. The preparation process of cinnamon extract according to claim 1, characterized in that, The settling time for stratification is 12-36 hours.
5. The preparation process of cinnamon extract according to claim 1, characterized in that, The pore size of the large-pore filter membrane is 5~20μm, and the pore size of the small-pore filter membrane is 0.2~1.0μm.
6. The cinnamon extract prepared by the process according to any one of claims 1 to 5, characterized in that, The active substance comprises ≥96.0% by mass, and includes 70.0~91.5 wt.% of trans-o-methoxycinnamoaldehyde, 4.0~25.5 wt.% of cinnamoyl acetate, 4.0~25.5 wt.% of eugenol and 0.5~10.0 wt.% of monoterpenoids.
7. The cinnamon extract according to claim 6, characterized in that, The extraction rates of trans-o-methoxycinnamoaldehyde are 30-55%, cinnamoyl acetate is 15-40%, eugenol is 15-40%, and monoterpenoids are 30-50%.
8. The application of the cinnamon extract according to claim 6 or 7 in mite-removing spray, antibacterial spray or deodorizing spray.
9. The application of the cinnamon extract according to claim 6 or 7 in mite-removing water, antibacterial water, or deodorizing water.
10. The application of the cinnamon extract according to claim 6 or 7 in mentholatum.
