Powdered essence containing rose extract concentrate and preparation method thereof
By using extraction solvents such as malt syrup and soaking alkali liquid, combined with pretreatment of water-in-oil system and coating agent, the problems of impure flavor and poor fragrance retention in the prior art are solved, and more efficient and more stable aroma ingredient extraction and retention are achieved.
Patent Information
- Application Number
- CN202411798786.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-03-14
- Estimated Expiration
- 2044-12-09
AI Technical Summary
The prior art is difficult to effectively extract and stabilize the aroma components in roses, resulting in the impure flavor of rose powder essence and poor fragrance retaining effect.
The mixture of malt syrup, water and organic solvents is used for heating and reflux extraction, combined with alkaline liquid soaking and aeration treatment, and further protect and stabilize the active ingredients in the rose extract concentrate through pretreatment of the water-in-oil system and coating agent.
It improves the extraction efficiency and stability of aroma components in the rose extract concentrate, ensures that the flavor of powder essence is better and pure, and extends the fragrance time.
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Abstract
Description
Technical Field
[0001] The present application relates to the field of plant extraction, and more specifically, to a powder essence containing rose extract concentrate and a preparation method thereof. Background Art
[0002] Rose is an important medicinal and aromatic plant in my country. Rose mainly contains vitamin C, carotene, thiamine, riboflavin, bitter substances, tannins, and minerals such as potassium, sodium, calcium, and magnesium. The vitamin C content in some roses is 50 times that of lemons. It can enhance the body's ability to produce collagen, resist the invasion of free radicals, and protect the skin from ultraviolet damage. Rose is warm in nature, sweet in taste, spicy and slightly bitter. It can help the body's positive energy flow, promote blood circulation, and have the effect of removing blood stasis and regulating menstruation. The volatile oil contained in rose has the effect of promoting bile secretion and can help the stomach digest. Rose extract concentrate has rich aromatic components including alcohols, aldehydes, ketones and other compounds. These components have unique aroma and biological activity, and have high medicinal value and edible value.
[0003] Rose extract concentrate is usually extracted from rose petals by steam distillation or other extraction techniques. It contains a variety of active ingredients in rose petals such as volatile oils, flavonoids, phenolic compounds, etc. with antioxidant, anti-inflammatory, moisturizing and other active ingredients. It is used in the preparation of rose powder flavor, and then used in food flavors to add rose aroma to obtain rose food flavor. It is used as a food additive and can also be used in other fields such as beverages to add rose flavor, which is of great significance.
[0004] Therefore, how to use rose as raw material to obtain rose extract concentrate and then make rose powder flavor with better flavor is of great significance for the application of flavors. Summary of the invention
[0005] In order to obtain rose extract concentrate using rose as raw material and then prepare rose powder essence with better flavor, the present application provides a powder essence containing rose extract concentrate and a preparation method thereof.
[0006] In the first aspect, the present application provides a powder essence containing rose extract concentrate, which adopts the following technical solution:
[0007] A powder essence containing rose extract concentrate, comprising the following raw materials in parts by weight:
[0008] 200-500 parts of rose extract concentrate, 1500-3000 parts of water, 700-1600 parts of corn starch, 300-500 parts of modified starch, 0.3-0.8 parts of citric acid, 0.1-0.5 parts of sodium tripolyphosphate, 0.1-0.5 parts of sodium hexametaphosphate, 1-3 parts of potassium sorbate and 1-5 parts of rose fragrance base;
[0009] The rose extract concentrate is prepared by the following method:
[0010] 1) Wash and dry fresh and dried roses, then crush and sieve to obtain rose pollen;
[0011] 2) Mix maltose syrup, water and organic solvent in a mass ratio of 1: (0.4-0.6): (0.4-0.6) to obtain an extraction solvent;
[0012] 3) Using the rose pollen in step 1) as raw material, the solvent extracted in step 2) is heated under reflux for 2-3 hours, extracted 3-5 times and filtered, the filtrates are combined, filtered, concentrated to be alcohol-free, and cooled to obtain a rose extract concentrate;
[0013] In the preparation process of rose extract concentrate, before step 3), firstly, the rose pollen in step 1) is soaked in sodium carbonate alkali solution, and sodium chloride is added after soaking for 40-60 minutes, and then carbon dioxide gas is introduced for aeration treatment, and after filtering and washing, extract A and pre-treated raw material A are obtained, and then step 3) is performed using pre-treated raw material A as a raw material, and the extraction solvent in step 2) is heated and refluxed for 60-90 minutes, and when the filtrate is combined in step 3), it is also combined with the obtained extract A, and then filtered and concentrated to obtain rose extract concentrate;
[0014] The rose extract concentrate is added after the following pretreatment:
[0015] Firstly, propylene glycol fatty acid ester, sucrose fatty acid ester and edible oil are mixed to prepare a mixed solution A;
[0016] Add the rose extract concentrate to the stirred mixed solution A, stir and mix at 65-75° C. for 40-60 min, homogenize, and then cool to obtain a primary mixture;
[0017] Mixing hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose with water to prepare a mixed solution B;
[0018] The primary mixture is added to the stirred mixed solution B, and then homogenized and spray-dried to obtain a rose extract concentrated powder;
[0019] The rose fragrance base comprises the following raw materials in parts by weight:
[0020] 8.0-8.6 parts of phenylethyl alcohol, 3.8-4.4 parts of vanillyl alcohol, 2.2-2.8 parts of geraniol, 0.06-0.12 parts of linalool, 1.8-2.4 parts of nerol, 0.7-0.76 parts of phenylethyl acetate, 2.0-2.6 parts of benzyl acetate, 0.3-0.36 parts of vanillyl acetate, 0.06-0.12 parts of ethyl phenylacetate, 0.1 -0.16 parts of citral, 0.1-0.16 parts of cinnamyl alcohol, 0.12-0.18 parts of artificial konjac oil, 0.06-0.12 parts of rose alcohol, 0.06-0.12 parts of diphenyl ether, 0.06-0.12 parts of eugenol, 0.02-0.08 parts of phenylacetaldehyde, 81.3-81.9 parts of propylene glycol, and 0.06-0.12 parts of ionone.
[0021] By adopting the above technical scheme, the present application adopts rose extract concentrate as the main aroma component of the essence, and the present application adopts a mixed solution of maltose syrup, water and an organic solvent as an extraction solvent to heat and reflux the rose to extract the aroma components in the rose, such as geraniol, citronellol and other volatile oils, polyphenols and flavonoids and other active ingredients, while maintaining their stability. In particular, the addition of maltose syrup is conducive to the dissolution and extraction of the active ingredients in the rose, and as a stabilizer, it can protect the active ingredients in the rose extract, especially in the subsequent preparation, processing and storage process, oxidation, degradation, etc., resulting in the loss of active ingredients, thereby making the final rose-flavored powder essence more pure in flavor.
[0022] On this basis, corn starch and modified starch are added in the present application as excipients and adhesives to improve the stability and dispersant of the powder flavor, citric acid, sodium tripolyphosphate and sodium hexametaphosphate are used as flavoring agents and stabilizers to adjust the pH value and stability of the powder flavor product, potassium sorbate is used as a preservative to extend its shelf life, and rose fragrance base is used to enhance and stabilize the rose aroma, which interacts with the rose extract concentrate to form a unique rose aroma. Finally, the present application obtains a powder flavor with a rich and pure rose flavor, which is more convenient to store and use and has broad application prospects.
[0023] In the present application, fresh roses are first soaked in alkaline solution. Flavonoids have a high solubility in alkaline solution. Soaking in alkaline solution allows flavonoid glycosides to be fully dissolved in the alkaline solution, thereby extracting more flavonoids. Then, aeration treatment is performed to use the impact force and vibration formed by the bubble formation and rupture process to act on the cell wall of the rose, causing microscopic mechanical stress, which helps to destroy the cell wall structure, thereby releasing the internal active substances. In addition, the rise and rupture of the bubbles help the fluidity of the soaking solution, help soften the cell wall, make the cell wall more easily penetrate into the cell, make it easy to rupture and promote the dissolution of the active ingredients. In addition, a large number of microbubbles generated during the gas aeration process can penetrate deeply into the cell wall to produce a more concentrated destructive effect. The above-mentioned multiple mechanisms act on the rose cell wall, effectively promote its rupture and the release of the internal active ingredients, improve the extraction of the active ingredients, and more importantly, reduce the subsequent heating reflux extraction time, thereby reducing the damage of the active substances to the high temperature, retaining more active ingredients while not reducing the extraction rate, and finally having better rose fragrance and nutrients.
[0024] Moreover, carbon dioxide is selected as the gas introduced in the present application. On the one hand, it prevents oxygen from reacting with the active ingredients in the rose to form an oxidation reaction, which leads to the oxidation inactivation of the active ingredients. On the other hand, it may be due to the reversible reaction of sodium carbonate with carbon dioxide and water to form sodium bicarbonate. The pH value in the system is constantly adjusted, and the active ingredients are continuously dissolved during the process. Moreover, it also has an effect on the osmotic pressure. Combined with the effect of sodium chloride on the permeability of the cell wall, more flavonoid active ingredients are dissolved, and the rose extract finally obtained has a richer rose aroma and contains more nutrients.
[0025] When the rose extract concentrate is directly added in the present application, due to the subsequent steps of heating, melting and spray drying in the preparation of powder essence, the active ingredients such as citronellol in the rose extract concentrate are easily oxidized and degraded under high temperature, affecting the pure flavor of its rose aroma. Therefore, the rose extract concentrate is pretreated in the present application, and is first added to an oily system containing propylene glycol fatty acid ester and sucrose fatty acid ester to achieve the preparation of an oil-in-water system. Propylene glycol fatty acid ester and sucrose fatty acid ester serve as thermal stabilizers to prevent the rose extract concentrate from oxidative degradation at high temperature and retain more active ingredients. Moreover, its encapsulation structure can also protect the active ingredients in the rose extract concentrate and prevent its aroma from evaporating. Then, it is encapsulated by hydroxypropyl β-cyclodextrin, microcrystalline cellulose and carboxymethyl cellulose. β-cyclodextrin has a lipophilic cavity structure and a hydrophilic shell. The addition of microcrystalline cellulose can further improve the thermal stability of the rose extract concentrated powder, and the lipophilic side of hydroxypropyl β-cyclodextrin can achieve the coating of the oil-in-water structure, thereby solving the subsequent water dispersion performance of the rose extract concentrated powder, improving the compatibility with other adjuvants, and dispersing more evenly in the powder flavor system. The carboxyl functional group in sodium carboxymethyl cellulose can form a chemical bond with the hydroxyl groups in hydroxypropyl β-cyclodextrin and microcrystalline cellulose, thereby improving the coating performance of the rose extract concentrated powder and further improving its subsequent thermal stability. In addition, sodium carboxymethyl cellulose and microcrystalline cellulose can also be used as suspending agents to improve the uniform dispersion of the subsequent rose extract concentrated powder in the powder flavor raw material system, prevent its sedimentation or agglomeration, and contribute to the uniform distribution of the final rose extract concentrate in the powder flavor.
[0026] Finally, the rose extract concentrate is subjected to the above pretreatment, which not only improves the encapsulation protection of the active ingredients in the rose extract concentrate, reduces the volatilization, oxidation or degradation of the aroma components at high temperature in subsequent operations, retains more effective ingredients, but also facilitates the uniform dispersion of the aroma components in the powder flavor raw material system. The powder flavor finally obtained has better uniformity and stability, and better fragrance retention effect.
[0027] Optionally, the organic solvent is one or two of ethanol, ether, acetone, ethyl acetate, and propylene glycol.
[0028] By adopting the above technical solution, the extraction solvent prepared with the above organic solvent has a better effect on the final extraction of active ingredients from roses.
[0029] Optionally, during the pretreatment of the rose extract concentrate, aluminum monostearate is added together with propylene glycol fatty acid ester, and the mass ratio of aluminum monostearate to propylene glycol fatty acid ester is 1:(1.5-2).
[0030] By adopting the above technical scheme, aluminum monostearate is used as a typical thixotropic gel formed in vegetable oil. In the present application, it is added to the oil phase mixed liquid A. In addition, the aluminum monostearate has the characteristics of high viscosity at low temperature and disappearance of viscosity at high temperature. Therefore, when the rose extract concentrate is added to the mixed liquid A in the present application, it has a certain fluidity due to its thixotropy. When the oil phase is wrapped to form an oil-in-water system, aluminum monostearate forms a gel system in the oil phase, thereby achieving the suspension of the rose extract concentrated powder in water to prevent sedimentation. The viscosity disappears during the subsequent high-temperature treatment, which is helpful for the mixing and dispersion of the rose extract concentrated powder with other raw materials and improves the uniform distribution of the active ingredients in the rose extract concentrate.
[0031] Optionally, during the pretreatment of rose extract concentrate, the mass ratio of propylene glycol fatty acid ester, sucrose fatty acid ester and edible oil is 1:(0.6-0.8):(2-3), the mass ratio of rose extract concentrate to mixed solution A is 1:(1.2-1.5), and the mass ratio of hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose is 1:(2-3):(1-1.2), the amount of water added is 3-4 times the mass of hydroxypropyl β-cyclodextrin, and the mass ratio of the primary mixture to mixed solution B is 1:(1.2-1.5).
[0032] By adopting the above technical scheme, the dissolution rate of the final rose extract concentrated powder in the water system is controlled by the addition amount of the above raw materials, especially the final addition amount of microcrystalline cellulose, thereby improving its compatibility with the powder flavor system while retaining the existence of the oil phase film, thereby improving the subsequent protection and fragrance retention effects.
[0033] Optionally, the specific operation of aeration treatment is: first, introduce carbon dioxide gas at a ventilation flow rate of 20-25L / min, the aeration time is 5-10min, then introduce carbon dioxide gas at a ventilation flow rate of 10-15 L / min, the aeration time is 15-25min, then stop aeration for 10-20min and repeat the above operation, and cycle 3-5 times.
[0034] By adopting the above technical scheme, in the present application, by adjusting the aeration flow rate, on the one hand, the effect on the cell wall is adjusted, and on the other hand, there is a dynamic adjustment process for the system pH, so that more effective ingredients can be dissolved. First, high-flow gas aeration is used, and the strong bubble impact and vibration directly act on the cell wall, quickly destroying its structure, thereby achieving an efficient wall-breaking effect. The microbubbles generated in the low-flow gas aeration stage penetrate into the cell gap, continuously destroy the residual cell wall structure, optimize the dissolution environment, and further release the active ingredients. Then stopping the aeration helps to disperse the active ingredients, and at the same time adjusts the environment to improve the dissolution and extraction of the effective ingredients, so that the subsequent heating reflux time is lower and more effective ingredients are dissolved, reducing the damage of high temperature to the active ingredients, and the final extract has more effective ingredients.
[0035] Optionally, the rose pollen is immersed in sodium carbonate alkali solution, and the alkali solution is added to a pH value of 7.5-8.5, and the amount of sodium chloride added is 2-5wt% of the amount of rose pollen added.
[0036] In a second aspect, the present application provides a method for preparing a powder essence containing a rose extract concentrate, using the following technical solution:
[0037] A method for preparing a powder flavor containing rose extract concentrate comprises the following steps: heating and melting the rose extract concentrate, water, corn starch, modified starch, citric acid, sodium tripolyphosphate, sodium hexametaphosphate and potassium sorbate, adding rose concentrate after mixing evenly, then adding rose fragrance base and carmine solution, stirring evenly and homogenizing, and then spray drying to obtain the powder flavor.
[0038] In summary, this application has the following beneficial effects:
[0039] 1. In the present application, rose extract concentrate is used as the main aroma component of the flavor, and a mixed solution of maltose syrup, water and an organic solvent is used as an extraction solvent to heat and reflux the rose to effectively extract aroma components in the rose, such as volatile oils such as geraniol and citronellol, polyphenols and flavonoids and other active ingredients, while maintaining their stability. In particular, the addition of maltose syrup is conducive to the dissolution and extraction of active ingredients in the rose, and as a stabilizer, it can protect the active ingredients in the rose extract, especially in the subsequent preparation, processing and storage process, oxidation, degradation, etc., resulting in the loss of active ingredients, so that the flavor of the final rose-flavored powdered flavor is more pure;
[0040] 2. In the present application, the rose extract concentrate is pretreated and first added to an oily system containing propylene glycol fatty acid ester and sucrose fatty acid ester to prepare an oil-in-water system. Propylene glycol fatty acid ester and sucrose fatty acid ester are used as heat stabilizers to prevent the rose extract concentrate from oxidative degradation at high temperature, retaining more active ingredients, and their encapsulation structure can also protect the active ingredients in the rose extract concentrate to prevent the evaporation of its aroma. Then, it is encapsulated by hydroxypropyl β-cyclodextrin, microcrystalline cellulose and carboxymethyl cellulose, which not only improves the encapsulation protection of the active ingredients in the rose extract concentrate, but also reduces the volatilization, oxidation or degradation of the aroma components at high temperature in subsequent operations, retains more effective ingredients, and is conducive to its uniform dispersion in the powder flavor raw material system. The powder flavor finally obtained has better uniformity and stability, and better fragrance retention effect;
[0041] 3. In the present application, on the one hand, the rose extract concentrate is pretreated, and on the other hand, the rose extraction process in the preparation process of the rose extract concentrate is improved to reduce the high-temperature extraction time and reduce the loss of active substances. In this way, the final powder flavor contains more active ingredients, and the final powder flavor contains more aroma components, has a purer and richer rose aroma, and has a longer lasting fragrance. DETAILED DESCRIPTION
[0042] The present application is further described in detail below in conjunction with the examples. It is particularly noted that if no specific conditions are specified in the following examples, the experiments are carried out according to conventional conditions or the conditions recommended by the manufacturer. Unless otherwise specified, the raw materials used in the following examples can be obtained from common commercial sources.
[0043] In the process of preparing powder flavor in the present application, whether it is the influence of heating temperature in the process of raw material mixing or the subsequent high-temperature treatment of spray drying, the active ingredients in the rose extract concentrate will volatilize, oxidize or degrade at high temperature, resulting in loss, affecting the subsequent active substances and flavor. In the present application, on the one hand, by pretreating the rose extract concentrate, on the other hand, by improving the rose extraction process in the preparation of the rose extract concentrate, the high-temperature extraction time is reduced and the loss of active substances is reduced. In this way, the final powder flavor has more active ingredients, and the final powder flavor has more aroma components, has a purer and richer rose aroma, and has a longer lasting fragrance time.
[0044] The carmine solution in the following examples is a 2 wt % carmine solution prepared by dissolving carmine in water;
[0045] The modified starch is the modified starch produced by Shandong Gushuo Biotechnology Co., Ltd.
[0046] The roses in the following embodiments are fresh and dried double rose petals.
[0047] The following preparation examples 1-3 are preparation examples of rose floral fragrance base.
[0048] Preparation Example 1
[0049] A method for preparing a rose fragrance base comprises the following steps:
[0050] Mix 8.4 g of phenylethanol, 4 g of vanillyl alcohol, 2.5 g of geraniol, 0.08 g of linalool, 2 g of nerol, 0.73 g of phenylethyl acetate, 2.4 g of benzyl acetate, 0.34 g of vanillyl acetate, 0.08 g of ethyl phenylacetate, 0.12 g of citral, 0.12 g of cinnamyl alcohol, 0.14 g of artificial konjac oil, 0.1 g of rose alcohol, 0.1 g of diphenyl ether, 0.1 g of eugenol, 0.05 g of phenylacetaldehyde, 81.6 g of propylene glycol and 0.08 g of ionone, place the mixture in a 60°C water bath for 5.5 h, and fully dissolve and mix to obtain rose fragrance base.
[0051] Preparation Example 2
[0052] A method for preparing a rose fragrance base comprises the following steps:
[0053] Mix 8.0 g of phenylethanol, 3.8 g of vanillyl alcohol (citronellol), 2.2 g of geraniol, 0.06 g of linalool, 1.8 g of nerol, 0.7 g of phenylethyl acetate, 2.0 g of benzyl acetate, 0.3 g of vanillyl acetate, 0.06 g of ethyl phenylacetate, 0.1 g of citral, 0.1 g of cinnamyl alcohol, 0.12 g of artificial konjac oil, 0.06 g of rose alcohol, 0.06 g of diphenyl ether, 0.06 g of eugenol, 0.02 g of phenylacetaldehyde, 81.3 g of propylene glycol and 0.06 g of ionone, place in a 60°C water bath for 5 hours, and fully dissolve and mix to obtain rose floral base.
[0054] Preparation Example 3
[0055] A method for preparing a rose fragrance base comprises the following steps:
[0056] Mix 8.6 g of phenylethyl alcohol, 4.4 g of vanillyl alcohol, 2.8 g of geraniol, 0.12 g of linalool, 2.4 g of nerol, 0.76 g of phenylethyl acetate, 2.6 g of benzyl acetate, 0.36 g of vanillyl acetate, 0.12 g of ethyl phenylacetate, 0.16 g of citral, 0.16 g of cinnamyl alcohol, 0.18 g of artificial konjac oil, 0.12 g of rose alcohol, 0.12 g of diphenyl ether, 0.12 g of eugenol, 0.08 g of phenylacetaldehyde, 81.9 g of propylene glycol and 0.12 g of ionone, place in a 60°C water bath for 6 hours, and fully dissolve and mix to obtain rose floral base.
[0057] Example 1
[0058] A method for preparing a powder essence containing rose extract comprises the following steps:
[0059] S1, preparing rose extract concentrate, specifically comprising the following steps:
[0060] 1) Wash and dry fresh and dried roses, then crush and sieve to obtain rose pollen, and take 500g of rose pollen for later use;
[0061] 2) Take 500 g of maltose syrup, mix maltose syrup, water and ethanol in a mass ratio of 1:0.5:0.5 to obtain an extraction solvent;
[0062] 3) Using the rose pollen in step 1) as raw material, the solvent extracted in step 2) is heated under reflux for 2.5 hours, extracted three times in total and then filtered, the filtrates are combined, and then centrifuged in a high-speed centrifuge to remove fine impurities to obtain a clear liquid, and then the obtained clear liquid is vacuum-concentrated in a multi-effect concentrator, the temperature is controlled at 55°C, the speed is 16r / min, and vacuum-concentrated at -0.09Mpa until there is no alcohol, and cooled to obtain a rose extract concentrate;
[0063] S2, take 2200g water, 1200g corn starch, 400g modified starch, 0.6g citric acid, 0.3g sodium tripolyphosphate, 0.3g sodium hexametaphosphate, 1.8g potassium sorbate, heat and melt, mix well, add 200g rose extract concentrate, then add 3g rose fragrance base in Preparation Example 1 and 2ml2% carmine solution, stir well, treat in a high-speed shearing machine at a speed of 800r / min for 25min, then pass through a homogenizer twice and spray dry, the inlet temperature of the spray dryer is 160°C, the outlet temperature is 80°C, and the speed is 18r / min, to obtain a powder flavor containing rose extract with a water content of 3%.
[0064] Example 2
[0065] A method for preparing a powder essence containing rose extract comprises the following steps:
[0066] S1, preparing rose extract concentrate, specifically comprising the following steps:
[0067] 1) Wash and dry fresh and dried roses, then crush and sieve to obtain rose pollen, and take 500g of rose pollen for later use;
[0068] 2) Take 500 g of maltose syrup, and mix maltose syrup, water and ethanol in a mass ratio of 1:0.4:0.4 to obtain an extraction solvent;
[0069] 3) Using the rose pollen in step 1) as the raw material, the solvent extracted in step 2) is heated under reflux for 2 hours, extracted 5 times in total and then filtered, the filtrates are combined, and then centrifuged in a high-speed centrifuge to remove fine impurities to obtain a clear liquid, and then the obtained clear liquid is vacuum-concentrated in a multi-effect concentrator, the temperature is controlled at 55°C, the speed is 16r / min, and vacuum-concentrated at -0.08Mpa until there is no alcohol, and cooled to obtain a rose extract concentrate;
[0070] S2, take 1500g water, 700g corn starch, 300g modified starch, 0.3g citric acid, 0.1g sodium tripolyphosphate, 0.1g sodium hexametaphosphate, 1g potassium sorbate, heat and melt, mix well, add 200g rose extract concentrate, then add 1g rose fragrance base in Preparation Example 2 and 2ml2% carmine solution, stir well, treat in a high-speed shearing machine at a speed of 800r / min for 25min, then pass through a homogenizer twice and spray dry, the inlet temperature of the spray dryer is 160°C, the outlet temperature is 80°C, and the speed is 18r / min, to obtain a powder flavor containing rose extract with a water content of 3%.
[0071] Example 3
[0072] A method for preparing a powder essence containing rose extract comprises the following steps:
[0073] S1, preparing rose extract concentrate, specifically comprising the following steps:
[0074] 1) Wash and dry fresh and dried roses, then crush and sieve to obtain rose pollen, and take 500g of rose pollen for later use;
[0075] 2) Take 500 g of maltose syrup, mix maltose syrup, water and ethanol in a mass ratio of 1:0.6:0.6 to obtain an extraction solvent;
[0076] 3) Using the rose pollen in step 1) as raw material, the solvent extracted in step 2) is heated under reflux for 3 hours, extracted three times in total and then filtered, the filtrates are combined, and then centrifuged in a high-speed centrifuge to remove fine impurities to obtain a clear liquid, and then the obtained clear liquid is vacuum-concentrated in a multi-effect concentrator, the temperature is controlled at 55°C, the speed is 16r / min, and vacuum-concentrated to alcohol-free under (-0.1)Mpa conditions, and cooled to obtain a rose extract concentrate;
[0077] S2, take 3000g water, 1600g corn starch, 500g modified starch, 0.8g citric acid, 0.5g sodium tripolyphosphate, 0.5g sodium hexametaphosphate, 3g potassium sorbate, heat and melt, mix well, add 500g rose extract concentrate, then add 5g rose fragrance base in Preparation Example 3 and 2ml of 2% carmine solution, stir well, treat in a high-speed shearing machine at a speed of 800r / min for 25min, then pass through a homogenizer twice and spray dry, the inlet temperature of the spray dryer is 160°C, the outlet temperature is 80°C, and the speed is 18r / min, to obtain a powder flavor containing rose extract with a water content of 3%.
[0078] Example 4
[0079] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that the rose extract concentrate is pretreated as follows before being added in step S2:
[0080] Propylene glycol fatty acid ester, sucrose fatty acid ester and rapeseed oil are mixed in a ratio of 1:0.7:2.5 to prepare a mixed solution A;
[0081] 200 g of the rose extract concentrate prepared in Preparation Example 1 was added to the mixed solution A under stirring, and the mixture was stirred and mixed at 70° C. for 50 min, and then homogenized. The mixture was then cooled to obtain a primary mixture, and the mass ratio of the rose extract concentrate to the mixed solution A was 1:1.3;
[0082] Mixing hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose with water to prepare a mixed solution B, wherein the added mass ratio of hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose is 1:2.5:1.1, and the added amount of water is 3 times the mass of hydroxypropyl β-cyclodextrin;
[0083] The primary mixture is added to the stirred mixed solution B, the mass ratio of the primary mixture to the mixed solution B is 1:1.3, and then the mixture is homogenized and spray-dried to obtain a rose extract concentrated powder, and then the rose extract concentrated powder is added to the mixed solution containing corn starch.
[0084] Example 5
[0085] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that the rose extract concentrate is pretreated as follows before being added in step S2:
[0086] Propylene glycol fatty acid ester, sucrose fatty acid ester and rapeseed oil are mixed in a ratio of 1:0.6:2 to prepare a mixed solution A;
[0087] 200 g of the rose extract concentrate prepared in Preparation Example 1 was added to the mixed solution A under stirring, and the mixture was stirred at 65° C. for 60 min and then homogenized, and then cooled to obtain a primary mixture, wherein the mass ratio of the rose extract concentrate to the mixed solution A was 1:1.2;
[0088] Mixing hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose with water to prepare a mixed solution B, wherein the mass ratio of hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose is 1:2:1, and the amount of water added is 3-4 times the mass of hydroxypropyl β-cyclodextrin;
[0089] The primary mixture is added to the stirred mixed solution B, the mass ratio of the primary mixture to the mixed solution B is 1:1.2, and then the mixture is homogenized and spray-dried to obtain a rose extract concentrated powder, and then the rose extract concentrated powder is added to the mixed solution containing corn starch.
[0090] Example 6
[0091] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that the rose extract concentrate is pretreated as follows before being added in step S2:
[0092] Propylene glycol fatty acid ester, sucrose fatty acid ester and rapeseed oil are mixed in a ratio of 1:0.8:3 to prepare a mixed solution A;
[0093] 200 g of the rose extract concentrate prepared in Preparation Example 1 was added to the mixed solution A under stirring, and the mixture was stirred and mixed at 75° C. for 40 min, and then homogenized, and then cooled to obtain a primary mixture, wherein the mass ratio of the rose extract concentrate to the mixed solution A was 1:1.5;
[0094] Mixing hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose with water to prepare a mixed solution B, wherein the added mass ratio of hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose is 1:3:1.2, and the added amount of water is 3-4 times the mass of hydroxypropyl β-cyclodextrin;
[0095] The primary mixture is added to the stirred mixed solution B, the mass ratio of the primary mixture to the mixed solution B is 1:1.5, and then the mixture is homogenized and spray-dried to obtain a rose extract concentrated powder, and then the rose extract concentrated powder is added to the mixed solution containing corn starch.
[0096] Example 7
[0097] A powder essence containing rose extract concentrate is prepared according to the method of Example 4, except that: when the rose extract concentrate is pretreated, aluminum monostearate is added together with propylene glycol fatty acid ester, and the mass ratio of aluminum monostearate to propylene glycol fatty acid ester is 1:1.8.
[0098] Example 8
[0099] A powder essence containing rose extract concentrate is prepared according to the method of Example 4, except that: when the rose extract concentrate is pretreated, aluminum monostearate is added together with propylene glycol fatty acid ester, and the mass ratio of aluminum monostearate to propylene glycol fatty acid ester is 1:1.5.
[0100] Example 9
[0101] A powder essence containing rose extract concentrate is prepared according to the method of Example 4, except that: when the rose extract concentrate is pretreated, aluminum monostearate is added together with propylene glycol fatty acid ester, and the mass ratio of aluminum monostearate to propylene glycol fatty acid ester is 1:2.
[0102] Example 10
[0103] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that: in the preparation process of the rose extract concentrate, the operation of step 3) is as follows:
[0104] First, the rose pollen in step 1) is soaked in sodium carbonate alkali solution with a pH value of 8, the alkali solution submerges the rose pollen, and sodium chloride is added after soaking for 50 minutes, the amount of sodium chloride added is 3wt% of the amount of rose pollen added, and then carbon dioxide gas is introduced for aeration treatment. The specific operation of aeration treatment is: first, carbon dioxide gas is introduced at an aeration flow rate of 22L / min, and the aeration time is 8min, and then carbon dioxide gas is introduced at an aeration flow rate of 12L / min, and the aeration time is 20min, and then the aeration is stopped for 15min and the above operation is repeated, and the cycle is repeated 4 times. After filtering and washing, extract A and pre-treated raw material A are obtained, and then step 3) in Example 1 is performed using pre-treated raw material A as a raw material, and the extraction solvent in step 2) is heated to reflux for extraction, heated to reflux for 70min, extracted 3 times in total, and then filtered, and then the filtrate is combined with the extract A and subsequent filtering, centrifugation, and concentration operations are performed.
[0105] Embodiment 11
[0106] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that: in the preparation process of the rose extract concentrate, the operation of step 3) is as follows:
[0107] First, the rose pollen in step 1) is soaked in sodium carbonate alkali solution with a pH value of 7.5, and the alkali solution is immersed in the rose pollen. After soaking for 40 minutes, sodium chloride is added, and the amount of sodium chloride added is 2wt% of the amount of rose pollen added. Then, carbon dioxide gas is introduced for aeration treatment. The specific operation of aeration treatment is: first, carbon dioxide gas is introduced at a ventilation flow rate of 20L / min, and the aeration time is 5min, and then carbon dioxide gas is introduced at a ventilation flow rate of 10L / min, and the aeration time is 15min, and then the aeration is stopped for 10min and the above operation is repeated, and the cycle is repeated 3 times. After filtering and washing, extract A and pre-treated raw material A are obtained, and then the pre-treated raw material A is used as the raw material in step 3) in Example 1, and the extraction solvent in step 2) is heated and refluxed for extraction, heated and refluxed for 90min, extracted 3 times in total, filtered, and then the filtrate and extract A are combined and then the subsequent filtration, centrifugation and concentration operations are performed.
[0108] Example 12
[0109] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that: in the preparation process of the rose extract concentrate, the operation of step 3) is as follows:
[0110] First, the rose pollen in step 1) is soaked in sodium carbonate alkali solution with a pH value of 8.5, and the alkali solution is immersed in the rose pollen. After soaking for 60 minutes, sodium chloride is added, and the amount of sodium chloride added is 5wt% of the amount of rose pollen added. Then, carbon dioxide gas is introduced for aeration treatment. The specific operation of aeration treatment is: first, carbon dioxide gas is introduced at a ventilation flow rate of 25L / min, and the aeration time is 10min, and then carbon dioxide gas is introduced at a ventilation flow rate of 15L / min, and the aeration time is 25min, and then the aeration is stopped for 20min and the above operation is repeated, and the cycle is repeated 5 times. After filtering and washing, extract A and pre-treated raw material A are obtained. Then, according to step 3) in Example 1, the pre-treated raw material A is used as a raw material, and the extraction solvent in step 2) is heated and refluxed for extraction, heated and refluxed for 60min, extracted 3 times in total, filtered, and then the filtrate and extract A are combined and then the subsequent filtration, centrifugation and concentration operations are performed.
[0111] Embodiment 13
[0112] A powder essence containing rose extract concentrate is prepared according to the method of Example 4, except that during the pretreatment of the rose extract concentrate, an equal amount of sucrose fatty acid ester is replaced by propylene glycol fatty acid ester.
[0113] Embodiment 14
[0114] A powder essence containing rose extract concentrate is prepared according to the method of Example 10, except that no aeration treatment is performed.
[0115] Embodiment 15
[0116] A powder essence containing rose extract concentrate is prepared according to the method of Example 10, except that carbon dioxide gas is directly introduced into the aeration process at a flow rate of 20 L / min, and after aeration for 150 minutes, the extract A and the pretreated raw material A are obtained by filtering and washing.
[0117] Comparative Example 1
[0118] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that maltose syrup is not added in step 2).
[0119] Comparative Example 2
[0120] A powder essence containing rose extract concentrate is prepared according to the method in Example 1, except that no rose fragrance base is added to the raw materials.
[0121] Performance Testing
[0122] First, the rose extract concentrate obtained in Examples 1-3, Examples 10-12, Example 14 and Comparative Example 1 was tested for sugar content. The test results are shown in Table 1 below.
[0123] Table 1:
[0124]
[0125] Referring to the test results in Table 1 above, the rose extract concentrate obtained by the scheme in the embodiment of the present application has a higher sugar content when extracting roses. The sugar content measures the soluble solid content in the extract. The higher the sugar content, the higher the content of sugar, polyphenols and other active ingredients. Combining the test results of Example 1 with those of Examples 10-12, it can be seen that after the rose pollen is soaked in alkali and pretreated with aeration, the extraction effect of the active ingredient is better, and the extracted concentrate has a higher sugar content. Combining the test results of Example 12, when the rose pollen is only soaked without aeration pretreatment, its sugar content is reduced, and the extraction effect of the active substances in the rose is reduced. Combining the test results of Example 15, when the aeration treatment is not staged flow regulation, its extraction effect is also reduced. Combining the test results in Comparative Example 1, when maltose syrup is not added to the extraction solvent, its sugar content is significantly reduced. On the one hand, maltose syrup can provide a certain sugar content, and on the other hand, the extraction effect of the active ingredients in the rose pollen is also reduced.
[0126] In addition, the loss of citronellol content and phenylethanol content in the powder flavors prepared in the examples and comparative examples of the present application was statistically analyzed. Specifically, the citronellol content and phenylethanol content (mg / g) in the rose extract concentrate added in step S2 of the embodiment were detected, the amount of phenylethanol and citronellol in the raw material was calculated, and then the phenylethanol and citronellol in the final powder flavor were detected (removed), and then the added amount in the rose fragrance base was removed, and then the loss rate in the process (loss amount / amount in the rose extract concentrate) was statistically analyzed. The statistical results are shown in Table 2 below.
[0127] Table 2:
[0128]
[0129] Combined with the test results in Table 2 above, combined with the test results of Example 1 and Example 4, it can be seen that the rose extract concentrate is coated and then added to significantly reduce the loss of flavor substances in the rose extract. Combined with the test results of Examples 7-9, the addition of aluminum monostearate can further reduce the loss. Combined with the test results of Example 1 and Example 13, when sucrose fatty acid esters are not added, the loss is large. Sucrose fatty acid esters help to form an oil-in-water coating rate and improve its protective effect. Referring to the test results of Comparative Example 1, when maltose syrup is not added to the extraction solvent, the loss of citronellol is greater, and it is also found that the extraction amount of citronellol is significantly reduced, and there is also a certain loss of flavor substances during the heating reflux extraction process.
[0130] The powder flavors obtained in the examples and comparative examples of the present application were subjected to an aroma evaluation test, and 50 professional tasters evaluated and scored the aromas. The average value of the final scoring results was calculated. The evaluation criteria and evaluation results are shown in Tables 3 and 4 below, respectively.
[0131] Table 3:
[0132]
[0133] Table 4:
[0134]
[0135] Combined with the test results in Table 3 and Table 4 above, referring to the test results of Example 1 and Examples 4-6, the rose extract concentrate was pretreated and then added, and the subsequent loss was less, and the pink powder essence was obtained with a strong floral fragrance, lasting fragrance, and aftertaste. Combined with the test results of Examples 7-9, the addition of aluminum monostearate further improved the protection of active flavor substances. Combined with the test results of Examples 10-12, when aeration treatment was performed during the extraction process, more flavor substances were obtained while reducing the heat extraction time, and the final evaluation result was higher. Combined with the test results of Example 13, when the extract concentrate was pretreated, no addition was made. When sucrose fatty acid ester is added, its protective effect is reduced, and the final flavor evaluation is also reduced. Combined with the test results of Example 14 and Example 15, when the rose pollen is pretreated without aeration treatment or flow regulation pretreatment, the extraction effect of active substances is reduced, and the final evaluation effect is reduced. Referring to the test results of Comparative Example 1, when maltose syrup is not added, the evaluation result is reduced. As a stabilizer, it helps to stabilize the flavor substances. Referring to the test results of Comparative Example 2, it can be seen that when the powder flavor is combined with rose extract concentrate and then with additional flavor substances, the final effect is better.
[0136] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.
Claims
1. A powder essence containing rose extract concentrate, characterized in that: It includes the following raw materials in parts by weight: 200-500 parts of rose extract concentrate, 1500-3000 parts of water, 700-1600 parts of corn starch, 300-500 parts of modified starch, 0.3-0.8 parts of citric acid, 0.1-0.5 parts of sodium tripolyphosphate, 0.1-0.5 parts of sodium hexametaphosphate, 1-3 parts of potassium sorbate and 1-5 parts of rose fragrance base; The rose extract concentrate is prepared by the following method: 1) Wash and dry fresh and dried roses, then crush and sieve to obtain rose pollen; 2) Mix maltose syrup, water and organic solvent in a mass ratio of 1: (0.4-0.6): (0.4-0.6) to obtain an extraction solvent; 3) Using the rose pollen in step 1) as raw material, the solvent extracted in step 2) is heated under reflux for 2-3 hours, extracted 3-5 times and filtered, the filtrates are combined, filtered, concentrated to be alcohol-free, and cooled to obtain a rose extract concentrate; In the preparation process of rose extract concentrate, before step 3), firstly, the rose pollen in step 1) is soaked in sodium carbonate alkali solution, and sodium chloride is added after soaking for 40-60 minutes, and then carbon dioxide gas is introduced for aeration treatment, and after filtering and washing, extract A and pre-treated raw material A are obtained, and then step 3) is performed using pre-treated raw material A as a raw material, and the extraction solvent in step 2) is heated and refluxed for 60-90 minutes, and when the filtrate is combined in step 3), it is also combined with the obtained extract A, and then filtered and concentrated to obtain rose extract concentrate; The rose extract concentrate is added after the following pretreatment: Firstly, propylene glycol fatty acid ester, sucrose fatty acid ester and edible oil are mixed to prepare a mixed solution A; Add the rose extract concentrate to the stirred mixed solution A, stir and mix at 65-75° C. for 40-60 minutes, homogenize, and then cool to obtain a primary mixture; Mixing hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose with water to prepare a mixed solution B; The primary mixture is added to the stirred mixed solution B, and then homogenized and spray-dried to obtain a rose extract concentrated powder; The rose fragrance base comprises the following raw materials in parts by weight: 8.0-8.6 parts of phenylethyl alcohol, 3.8-4.4 parts of vanillyl alcohol, 2.2-2.8 parts of geraniol, 0.06-0.12 parts of linalool, 1.8-2.4 parts of nerol, 0.7-0.76 parts of phenylethyl acetate, 2.0-2.6 parts of benzyl acetate, 0.3-0.36 parts of vanillyl acetate, 0.06-0.12 parts of ethyl phenylacetate, 0.1 -0.16 parts of citral, 0.1-0.16 parts of cinnamyl alcohol, 0.12-0.18 parts of artificial konjac oil, 0.06-0.12 parts of rose alcohol, 0.06-0.12 parts of diphenyl ether, 0.06-0.12 parts of eugenol, 0.02-0.08 parts of phenylacetaldehyde, 81.3-81.9 parts of propylene glycol, and 0.06-0.12 parts of ionone.
2. The powder essence containing rose extract concentrate according to claim 1, characterized in that: The organic solvent is selected from one or two of ethanol, ether, acetone, ethyl acetate and propylene glycol.
3. The powder essence containing rose extract concentrate according to claim 1, characterized in that: When the rose extract concentrate is pretreated, aluminum monostearate is added together with propylene glycol fatty acid ester, and the added mass ratio of aluminum monostearate to propylene glycol fatty acid ester is 1:(1.5-2).
4. The powder essence containing rose extract concentrate according to claim 1, characterized in that: During the pretreatment of rose extract concentrate, the mass ratio of propylene glycol fatty acid ester, sucrose fatty acid ester and edible oil is 1: (0.6-0.8): (2-3), the mass ratio of rose extract concentrate to mixed solution A is 1: (1.2-1.5), and the mass ratio of hydroxypropyl β-cyclodextrin, microcrystalline cellulose and sodium carboxymethyl cellulose is 1: (2-3): (1-1.2), the amount of water added is 3-4 times the mass of hydroxypropyl β-cyclodextrin, and the mass ratio of the initial mixture to mixed solution B is 1: (1.2-1.5).
5. The powder essence containing rose extract concentrate according to claim 1, characterized in that: The specific operation of aeration treatment is: first, introduce carbon dioxide gas at a ventilation flow rate of 20-25L / min, and the aeration time is 5-10min, then introduce carbon dioxide gas at a ventilation flow rate of 10-15 L / min, and the aeration time is 15-25min, then stop aeration for 10-20min and repeat the above operation, and cycle 3-5 times.
6. A method for preparing a powder essence containing a rose extract concentrate as claimed in any one of claims 1 to 5, characterized in that: The following steps are involved: Heat and melt rose extract concentrate, water, corn starch, modified starch, citric acid, sodium tripolyphosphate, sodium hexametaphosphate and potassium sorbate, mix well, add rose concentrate, then add rose fragrance base and carmine solution, stir well and homogenize, and then spray dry to obtain powder essence.
Citation Information
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