CN111721073B - Vacuum freeze-drying rose flower process - Google Patents
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- CN111721073B CN111721073B CN202010576887.4A CN202010576887A CN111721073B CN 111721073 B CN111721073 B CN 111721073B CN 202010576887 A CN202010576887 A CN 202010576887A CN 111721073 B CN111721073 B CN 111721073B
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
- A61K36/738—Rosa (rose)
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
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Abstract
The invention discloses a vacuum freeze-drying rose flower process, which comprises the following steps: s1 picking rose flowers; s2 processing rose with color retention solution; s3 freeze-drying rose; s4 gradient heating to dry rose; s5, condensing at low temperature to collect rose hydrosol; the invention has the beneficial effects that: the color retention liquid is utilized and atomized, so that the collection and utilization of the roses are realized; the jojoba oil, the tartaric acid and the almond oil are used for keeping the stability of petal cells, and simultaneously, the three components are combined and superposed in an antioxidant way to stabilize the integral color of petals and further realize full drying; the collection and utilization are realized by utilizing three-stage heating; the collection and utilization are realized by limiting the conditions of low-temperature condensation and collection; fully drying the mixture by atomizing the color retention liquid; thorough drying was achieved by standing for 35 min.
Description
Technical Field
The invention relates to the field of food processing, in particular to a rose vacuum freeze-drying process.
Background
Roses belong to Rosales, Rosaceae deciduous shrubs, branches and stems are multi-needle-pricked, odd feathery compound leaves and 5-9 small leaves are oval and have edge-pricked, flowers of the roses are mainly used for food and essence rose oil extraction, and the rose oil is applied to industries such as cosmetics, food, fine chemical engineering and the like. Text of materia medica (text of materia medica) Zhongdao: the rose flower has the functions of clearing without turbidity, harmonizing without fierce, softening liver, waking stomach, dredging qi, activating blood circulation, dredging suffocation stagnation without the disadvantages of acridity, warmness and dryness, has the most rapid and most tame effect among qi pushing and medicine separation, is fragrant and almost has no other advantages, contains more than 300 chemical components such as fragrant alcohol, aldehyde, fatty acid, phenol and oil and fat containing essence, is frequently eaten for softening liver, waking stomach, relaxing qi, activating blood, beautifying, making people feel cool, can be used as a medicine for flowers and roots which are just opened by roses, has the functions of regulating qi, activating blood, astringing and the like, and is mainly used for treating irregular menstruation, traumatic injury, liver-qi-stomach pain, milk swelling and pain and the like. Because fresh flowers are not easy to preserve, the roses are generally dehydrated by heating or airing, main nutritional ingredients of the roses are reserved, but the color of the flower buds of the roses becomes dark due to a heating method with high temperature, meanwhile, a large amount of rose aroma molecules in the petals can be dissipated due to high temperature, and when the prepared dry roses are used for soaking water, the aroma molecules are rare, and the taste of the brewed rose tea is light.
The invention relates to a preparation method of vacuum freeze-dried rose (application number: CN201310438607.3), which is mainly characterized by comprising the following steps: a. picking rose flowers; c. vacuum freeze drying: vacuumizing to 15-25 kPa, starting refrigeration, and reducing the temperature of a cold trap of the vacuum freeze dryer to-40-65 ℃ within 2-4 hours, and keeping the temperature for 0.5-2 hours; heating the rose to 0-15 ℃ within 9-18 hours to dry the rose. Although the vacuum drying method is adopted, the damage of the bioactive effective components of the roses is extremely small, the appearance is well preserved, and the nutritional ingredients and the active substances of the roses are kept, in fact, the temperature in the heating stage is not enough to completely dry the roses, and the roses are easily softened and further damaged by being recovered to the normal temperature in the transportation stage; meanwhile, if the rose is heated directly in the heating stage, the rose fragrance substances dissipated in the heating stage cannot be effectively collected and utilized.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a vacuum freeze-drying rose flower process so as to at least achieve the aims of fully drying, collecting and utilizing.
The purpose of the invention is realized by the following technical scheme:
a rose vacuum freeze-drying process comprises the following steps:
s1, selecting fresh rose flowers, wherein the picking period is required to be not more than 24 hours, and placing the picked rose flowers in clean water for washing to obtain clean rose flowers;
s2, standing the cleaned rose flowers in the atomized color retention solution, and then placing the rose flowers in a vacuum chamber, wherein the air pressure in the vacuum chamber is controlled to be 10 kPa;
s3, reducing the temperature to-30 to-50 ℃ within 60-80min in a vacuum chamber, and keeping the temperature for 20-40min to obtain freeze-dried rose flowers;
s4, placing the freeze-dried rose flowers in a vacuum drying chamber, controlling the air pressure in the chamber to be 2kPa, heating to 45 ℃ within 6h according to a gradient heating mode, and stabilizing for 2h to obtain dried rose flowers;
and S5 collecting the gas generated in the temperature rise process in S4, and carrying out low-temperature condensation to obtain the rose hydrosol.
Preferably, in order to further achieve the purpose of full drying, the color retention solution comprises 40-50 parts of ultrapure water, 10-20 parts of tartaric acid, 5-10 parts of jojoba oil and 5-10 parts of almond oil by weight; utilize jojoba oil to act as the dispersant, bear tartaric acid and almond oil and enter into the petal cell of rose, simultaneously the good oxidation resistance of jojoba oil and almond oil combines with the oxidation resistance of tartaric acid, and then can reduce the solidification temperature of rose to a certain extent, make the rose flower can keep the stability of the petal inner cell of flower in freeze drying stage, three's oxidation resistance combination stack simultaneously, and then can make the time that anthocyanin in the rose petal discolours because of the oxidation prolong in the stage of rising the temperature, thereby make the whole colour of petal stable, and then indirect messenger's the interior liquid material ability of petal in drying stage can be gasified completely, realize the mesh of abundant drying, the original colour of stable maintenance rose simultaneously.
Preferably, for the purpose of further realizing collection and utilization, the gradient heating is as follows: in the first stage, within 0-1h, the temperature is raised to 5 ℃ according to the speed of 2 ℃/h and then is stabilized to 1 h; in the second stage, within 1-4h, the temperature is raised to 35 ℃ according to the speed of 5 ℃/h and then is stabilized to 4 h; in the third stage, the temperature is raised to 45 ℃ within 4-6h according to 8 ℃/h and then is stabilized to 6 h; utilize the intensification of three stages to each stage intensification after the stable temperature period, and then utilize the gradient intensification, make the rose fragrance oil molecule in the rose stable loss, and then can collect the rose fragrance oil gas of different temperature gradients, thereby pave for obtaining the rose hydrosol, realize the purpose of collecting the utilization.
Preferably, for the purpose of further realizing collection and utilization, the low-temperature condensation is to condense and collect gas generated in the temperature rise process in a condensation pipe under the condition of 4 ℃; the gas is rose aromatic oil molecules; through the condition of the low temperature condensation collection of injecing the rose fragrance oil gas that collects to the intensification stage, and then cooperate the intensification of three stages, provide the support of condensation for collecting the rose hydrosol, realize the purpose of collecting the utilization.
Preferably, for the purpose of further achieving sufficient drying, the atomization is to atomize the color-keeping liquid into mist-like small droplets of 2 mm; through the mode that the little liquid that becomes 2mm with the color retaining liquid atomizing is low, and then make the little liquid of color retaining liquid can be even cover the flower of rose to for the freeze drying of rose and the dry area that covers of warming up provide more stable color retaining liquid, and then the purpose of indirect realization abundant drying.
Preferably, for the purpose of further achieving sufficient drying, the standing time in S2 is 35 min; through standing for 35min, the color retention liquid is fully immersed into the petals of the roses in the vacuum atmosphere, so that the color change of the roses after the vacuum freeze drying process is slowed down, the color of the petals of the roses is kept fixed, the freezing point temperature of the freeze drying is further reduced, the oxidation of the roses in the temperature rising stage is slowed down, and the purpose of fully drying is indirectly realized.
The invention has the beneficial effects that:
1. utilize the color retention liquid to guarantee to adopt vacuum freeze drying and gradient heating's intensification mode, the colour that makes the petal of rose is stable, the range of discolouing is little, atomizing color retention liquid can fully be infected with on the petal of rose simultaneously, and gradient heating energy makes the rose sesame oil molecule in the rose effluvium, can collect through simple low temperature condensation, and then utilize color retention liquid to improve the physical characteristics of rose, make it can dry in the technology of vacuum freeze drying rose and obtain the rose, can collect the rose hydrosol again, and then realize the purpose of the collection and the utilization of rose.
2. Utilize jojoba oil to act as the dispersant, bear tartaric acid and almond oil and enter into the petal cell of rose, simultaneously the good oxidation resistance of jojoba oil and almond oil combines with the oxidation resistance of tartaric acid, and then can reduce the solidification temperature of rose to a certain extent, make the rose flower can keep the stability of the petal inner cell of flower in freeze drying stage, three's oxidation resistance combination stack simultaneously, and then can make the time that anthocyanin in the rose petal discolours because of the oxidation prolong in the stage of rising the temperature, thereby make the whole colour of petal stable, and then indirect messenger's the interior liquid material ability of petal in drying stage can be gasified completely, realize the mesh of abundant drying, the original colour of stable maintenance rose simultaneously.
3. Utilize the intensification of three stages to each stage intensification after the stable temperature period, and then utilize the gradient intensification, make the rose fragrance oil molecule in the rose stable loss, and then can collect the rose fragrance oil gas of different temperature gradients, thereby pave for obtaining the rose hydrosol, realize the purpose of collecting the utilization.
4. Through the condition of the low temperature condensation collection of injecing the rose fragrance oil gas that collects to the intensification stage, and then cooperate the intensification of three stages, provide the support of condensation for collecting the rose hydrosol, realize the purpose of collecting the utilization.
5. Through the mode that the little liquid that becomes 2mm with the color retaining liquid atomizing is low, and then make the little liquid of color retaining liquid can be even cover the flower of rose to for the freeze drying of rose and the dry area that covers of warming up provide more stable color retaining liquid, and then the purpose of indirect realization abundant drying.
6. Through standing for 35min, the color retention liquid is fully immersed into the petals of the roses in the vacuum atmosphere, so that the color change of the roses after the vacuum freeze drying process is slowed down, the color of the petals of the roses is kept fixed, the freezing point temperature of the freeze drying is further reduced, the oxidation of the roses in the temperature rising stage is slowed down, and the purpose of fully drying is indirectly realized.
Detailed Description
The technical solutions of the present invention are described in further detail below, but the scope of the present invention is not limited to the following.
Example 1
A rose vacuum freeze-drying process comprises the following steps:
s1, selecting fresh rose flowers, wherein the picking period is required to be not more than 24 hours, and placing the picked rose flowers in clean water for washing to obtain clean rose flowers;
s2, standing the cleaned rose flowers for 35min in the atomized color retention solution, and then placing the rose flowers in a vacuum chamber, wherein the air pressure in the vacuum chamber is controlled to be 10 kPa; the color retention liquid comprises 43 parts of ultrapure water, 17 parts of tartaric acid, 7 parts of jojoba oil and 7 parts of almond oil by weight; the jojoba oil is used as a dispersing agent to bear tartaric acid and almond oil to enter petal cells of the roses, meanwhile, the good oxidation resistance of the jojoba oil and the almond oil is combined with the oxidation resistance of the tartaric acid, so that the solidification temperature of the roses can be reduced to a certain extent, the stability of cells in the petals of the roses can be kept in a freeze drying stage, meanwhile, the oxidation resistance of the jojoba oil and the almond oil is combined and superposed, the time for anthocyanin in the petals of the roses to change color due to oxidation can be prolonged in a heating stage, the integral color of the petals is stable, liquid substances in the petals in a drying stage can be gasified completely indirectly, the purpose of full drying is realized, and the original color of the roses is stably maintained; the atomization is to atomize the color-preserving liquid into atomized small droplets of 2 mm; the color retention solution is atomized into a mode of small solution with the size of 2mm, so that small liquid drops of the color retention solution can uniformly cover the flowers of the roses, a more stable color retention solution coverage area is provided for freeze drying and temperature rise drying of the roses, and the aim of fully drying is indirectly fulfilled; standing for 35min, and fully soaking the color retention liquid into the petals of the roses in a vacuum atmosphere, so that the color change of the roses after a vacuum freeze drying process is slowed down, the color of the petals of the roses is kept fixed, the freezing point temperature of freeze drying is further lowered, the oxidation of the roses in a temperature rise stage is slowed down, and the purpose of fully drying is indirectly realized;
s3, reducing the temperature to-30 to-50 ℃ within 60-80min in a vacuum chamber, and keeping the temperature for 20-40min to obtain freeze-dried rose flowers;
s4, placing the freeze-dried rose flowers in a vacuum drying chamber, controlling the air pressure in the chamber to be 2kPa, heating to 45 ℃ within 6h according to a gradient heating mode, and stabilizing for 2h to obtain dried rose flowers; the gradient heating comprises the following steps: in the first stage, within 0-1h, the temperature is raised to 5 ℃ according to the speed of 2 ℃/h and then is stabilized to 1 h; in the second stage, within 1-4h, the temperature is raised to 35 ℃ according to the speed of 5 ℃/h and then is stabilized to 4 h; in the third stage, the temperature is raised to 45 ℃ within 4-6h according to 8 ℃/h and then is stabilized to 6 h; three-stage heating is utilized, the temperature is stabilized for a period of time after each stage of heating, then gradient heating is utilized to enable the rose fragrance oil molecules in the rose to stably escape, and further rose fragrance oil gas with different temperature gradients can be collected, so that rose hydrosol is obtained to be laid, and the purpose of collection and utilization is achieved;
s5, collecting gas generated in the heating process in S4, and carrying out low-temperature condensation to obtain rose hydrosol; the low-temperature condensation is to condense and collect gas generated in the temperature rise process in a condensation pipe at the temperature of minus 35 ℃; the gas is rose aromatic oil molecules; through the condition of the low temperature condensation collection of injecing the rose fragrance oil gas that collects to the intensification stage, and then cooperate the intensification of three stages, provide the support of condensation for collecting the rose hydrosol, realize the purpose of collecting the utilization.
Example 2
The components of the color retention liquid are changed into 40 parts of ultrapure water, 10 parts of tartaric acid, 5 parts of jojoba oil and 5 parts of almond oil, and the rest formula and steps are the same as those in example 1.
Example 3
The components of the color retention liquid are changed into 50 parts of ultrapure water, 20 parts of tartaric acid, 10 parts of jojoba oil and 10 parts of almond oil, and the rest formula and steps are the same as those in example 1.
Example 4
The temperature in the vacuum chamber during the freeze drying process was reduced to-30 ℃ within 60min and maintained for 20min, and the rest of the formulation and steps were the same as in example 1.
Example 5
The temperature in the vacuum chamber during the freeze drying process was reduced to-50 ℃ within 80min and maintained for 40min, and the rest of the formulation and procedure were the same as in example 1.
Comparative example 1
The cleaned rose is directly placed in a vacuum chamber without adopting a color retention solution, and the rest formula and steps are the same as those of the example 1.
Comparative example 2
The atomized color retention solution is not adopted, the color retention solution is directly used for directly washing the roses, and the rest formula and the steps are the same as those in the example 1.
Comparative example 3
The temperature is directly raised to 45 ℃ within 6h without adopting a gradient heating mode, and the rest formula and steps are the same as those of the example 1.
Comparing the color and flavor of the dried roses obtained in each example and comparative example to obtain Table 1;
TABLE 1 distribution of color and fragrance profiles for the rose products of the various examples and comparative examples
Comparing the rose hydrosol obtained after the collected gas is condensed at low temperature in the temperature rising stage of each example and comparative example, calculating the conversion efficiency (the conversion efficiency: the ratio of the weight of the rose hydrosol condensed at low temperature to the sum of the weight of the fresh rose flowers and the weight of each liquid), and obtaining the table 2;
TABLE 2 conversion efficiency tables for respective examples and comparative examples
| Categories | Conversion efficiency (%) |
| Example 1 | 88 |
| Example 2 | 85 |
| Example 3 | 86 |
| Example 4 | 81 |
| Example 5 | 80 |
| Comparative example 1 | 74 |
| Comparative example 2 | 80 |
| Comparative example 3 | 71 |
It can be seen from tables 1 and 2 that, when a color retention solution comprising 43 parts of ultrapure water, 17 parts of tartaric acid, 7 parts of jojoba oil and 7 parts of almond oil is adopted, and the color retention solution is atomized and the roses obtained by matching with a gradient heating mode are simultaneously changed into a whole color, the parts of calyx are slightly deepened and the inner and outer colors are consistent, the fragrance condition is that plant fragrance is mixed in the original fragrance of the roses, the conversion efficiency is 85%, the corresponding conversion efficiency of the weight of the cell sap is 75%, and the plant fragrance possibly exists in the blending of the jojoba oil and the almond oil in the color retention solution, and plant oil fragrance molecules capable of dissipating parts are generated in the gradient heating stage.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (1)
1. A vacuum freeze-drying rose flower process is characterized in that: the method comprises the following steps:
s1, selecting fresh rose flowers, wherein the picking period is required to be not more than 24h, and cleaning the picked rose flowers to obtain clean rose flowers;
s2, the clean rose flowers are placed in the atomized color retention solution and then placed in a vacuum chamber, and the air pressure in the vacuum chamber is controlled to be 10 kPa;
s3, reducing the temperature to-30 to-50 ℃ within 60 to 80min in a vacuum chamber, and keeping the temperature for 20 to 40min to obtain freeze-dried rose flowers;
s4, placing the freeze-dried rose flowers in a vacuum drying chamber, controlling the air pressure in the chamber to be 2kPa, heating to 45 ℃ within 18h according to a gradient heating mode, and stabilizing for 2h to obtain dried rose flowers;
s5, collecting gas generated in the heating process in S4, and carrying out low-temperature condensation to obtain rose hydrosol;
s6 storing the rose obtained in S4 and the rose hydrosol of S5 in a low-temperature storehouse respectively;
the color retention liquid comprises, by weight, 40-50 parts of ultrapure water, 10-20 parts of tartaric acid, 5-10 parts of jojoba essential oil and 5-10 parts of almond oil;
the gradient heating comprises the following steps: in the first stage, within 0-1h, the temperature is raised to 5 ℃ according to the speed of 2 ℃/h and then is stabilized to 1 h; in the second stage, within 1-4h, the temperature is raised to 35 ℃ according to the speed of 5 ℃/h and then is stabilized to 4 h; in the third stage, the temperature is raised to 45 ℃ within 4-6h according to 8 ℃/h and then is stabilized to 6 h;
the low-temperature condensation is to condense and collect gas generated in the temperature rise process in a condensation pipe at the temperature of minus 35 ℃;
the gas is rose aromatic oil molecules;
the atomization is to atomize the color-preserving liquid into atomized small droplets of 2 mm;
the standing time in the S2 is 35 min;
the low-temperature storehouse is a storage storehouse with the temperature of minus 25 ℃.
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| CN112471304B (en) * | 2020-12-22 | 2023-03-03 | 海南中椹生物科技有限公司 | Scenting method of scented tea |
| CN114009541B (en) * | 2021-11-03 | 2024-02-13 | 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） | Passion fruit tea and processing method thereof |
| CN114432734A (en) * | 2022-01-21 | 2022-05-06 | 云南八街王大爹农业科技有限公司 | Yunnan red double-petal rose bud water and preparation method thereof |
| CN114794457A (en) * | 2022-01-29 | 2022-07-29 | 上海应用技术大学 | Drying method of convenient instant rose petals |
| CN115530158A (en) * | 2022-10-27 | 2022-12-30 | 濮阳市食品药品检验检测中心 | Method for making plant specimen with high-efficiency color retention |
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| US4312134A (en) * | 1980-08-04 | 1982-01-26 | Strausser Robert W | Method of freeze-drying flower arrangements |
| CN105168958B (en) * | 2015-09-08 | 2019-01-01 | 安徽省国臻堂生物科技股份有限公司 | Dendrobium nobile dried frozen aquatic products and preparation method thereof |
| CN205273009U (en) * | 2016-01-13 | 2016-06-01 | 哈尔滨商业大学 | Protect look, soften and dry processing apparatus flower |
| CN106244324A (en) * | 2016-08-16 | 2016-12-21 | 文县恒水玫瑰开发有限公司 | A kind of Flos Rosae Rugosae quintessence oil extracts and purification process |
| CN107234920A (en) * | 2017-05-06 | 2017-10-10 | 云南万融花卉有限公司 | A kind of manufacture craft of rose immortality flower |
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