Angelica sinensis freeze-drying process and freeze-dried angelica sinensis

Abstract

The invention discloses an angelica sinensis freeze-drying process and freeze-dried angelica sinensis. The angelica sinensis freeze-drying process comprises the following steps: selecting fresh angelica sinensis without plant diseases and insect pests, and cleaning; the pretreated angelica sinensis is placed in a vacuum drying machine to be subjected to vacuum freeze drying, and the vacuum freeze drying control program is as follows: the constant temperature of minus 45 DEG C to minus 35 DEG C is 3-5 h, the constant temperature of minus 15 DEG C to minus 5 DEG C is 8-12 h, the constant temperature of 4 DEG C to 6 DEG C is 8-12 h, the constant temperature of 8 DEG C to 12 DEG C is 10-14 h, and the constant temperature of 22 DEG C to 28 DEG C is 10-14 h; angelica sinensis is dried through a freeze-drying process, the internal structure and effective components of angelica sinensis can be better preserved, and the stability of angelica sinensis is improved; besides, by controlling freeze-drying process parameters, the internal structure of the radix angelicae sinensis can be better reserved, structural damage and loss of effective components are prevented, and the stability of the freeze-dried radix angelicae sinensis can be better improved.

Description

TECHNICAL FIELD

[0001] The application belongs to the processing technical field of angelica sinensis, and particularly relates to a freeze-drying process of angelica sinensis and freeze-dried angelica sinensis. BACKGROUND

[0002] Angelica sinensis (Oliv.) Diels is a perennial herbaceous plant of the family Umbelliferae. The root is cylindrical, branched, yellowish brown; the stem is erect, greenish white or purplish, with longitudinal deep grooves; the leaf is pinnately lobed, purplish or greenish, ovate; the flower is white, with a dense fine pubescent pedicel, and the petal is long ovate, the style base is conical, and the flowering period is from June to July. The fruit is elliptical to ovate, with the wing edge being light purple, and the fruiting period is from July to September. It is recorded in Shennong's Herbal Classic that "the ancient people married women for the purpose of continuation of the family, and angelica sinensis is a woman's essential medicine, and has the meaning of thinking of the husband, so it is named angelica sinensis". Angelica sinensis is mainly produced in the southeast of Gansu, with the most in Minxian County and the best quality, followed by Yunnan, Sichuan, Shaanxi and Hubei provinces, and is cultivated in some provinces and regions. It likes cold and cool and grows in high-cold and humid mountainous areas. Generally, seed direct sowing and seedling transplanting are used for reproduction, and seedling transplanting is commonly used in production.

[0003] Fresh angelica sinensis needs to be dried for storage and transportation. At present, angelica sinensis is generally dried by natural air drying or drying. However, the natural air drying process is greatly affected by weather, the drying time is long, and the quality is not easy to control. The drying has a great influence on heat-sensitive components, resulting in a decrease in effective components of angelica sinensis. SUMMARY

[0004] The purpose of the present application is to provide a freeze-drying process of angelica sinensis and freeze-dried angelica sinensis to solve the problems in the background art.

[0005] To achieve the above-mentioned purpose, the present application provides the following technical scheme:

[0006] A freeze-drying process of angelica sinensis, the freeze-drying process of angelica sinensis comprising the following steps:

[0007] (a) angelica sinensis pretreatment:

[0008] Select fresh angelica sinensis without pests and diseases and wash it;

[0009] (b) vacuum freeze-drying:

[0010] Place the pretreated angelica sinensis in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0011] -45 to -35 DEG C constant temperature for 3 to 5 h, -15 to -5 DEG C constant temperature for 8 to 12 h, 4 to 6 DEG C constant temperature for 8 to 12 h, 8 to 12 DEG C constant temperature for 10 to 14 h, and 22 to 28 DEG C constant temperature for 10 to 14 h.

[0012] Preferably, the vacuum degree during the vacuum freeze-drying process is < 10 Pa.

[0013] Preferably, the vacuum degree during the vacuum freeze-drying process is 5 Pa.

[0014] Preferably, the vacuum freeze-drying control program is as follows:

[0015] -42 to -38℃ for 3 to 5 h, -12 to -8℃ for 8 to 12 h, 4 to 6℃ for 8 to 12 h, 9 to 11℃ for 10 to 14 h, and 24 to 26℃ for 10 to 14 h.

[0016] Preferably, the vacuum freeze-drying control program is as follows:

[0017] -40℃ for 4 h, -10℃ for 10 h, 5℃ for 10 h, 10℃ for 12 h, and 25℃ for 12 h.

[0018] Preferably, the cleaning comprises washing the angelica with clean water to remove dirt and impurities on the surface of the angelica.

[0019] The second aspect of the present application provides a freeze-dried angelica prepared by the above-mentioned freeze-drying process of angelica.

[0020] Compared with the prior art, the present application has the following beneficial effects:

[0021] The present application can better preserve the internal structure and effective components of angelica and improve the stability of angelica by drying angelica through a freeze-drying process. In addition, the present application can better preserve the internal structure of angelica, prevent the destruction of the structure and the loss of effective components, and better improve the stability of freeze-dried angelica by controlling the freeze-drying process parameters. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0023] A freeze-drying process of angelica, comprising the following steps:

[0024] (a) angelica pretreatment:

[0025] Select fresh angelica free of pests and diseases and clean it;

[0026] (b) vacuum freeze-drying:

[0027] The pretreated angelica is placed in a vacuum freeze dryer, and the vacuum freeze drying control program is as follows:

[0028] -45 to -35 DEG C constant temperature 3 to 5 h, -15 to -5 DEG C constant temperature 8 to 12 h, 4 to 6 DEG C constant temperature 8 to 12 h, 8 to 12 DEG C constant temperature 10 to 14 h, 22 to 28 DEG C constant temperature 10 to 14 h.

[0029] The angelica is dried by the freeze drying process, the internal structure and effective components of the angelica can be better preserved, and the stability of the angelica is improved; in addition, the internal structure of the angelica can be better preserved, the structure damage and loss of effective components are prevented, and the stability of the freeze-dried angelica is better improved by controlling the freeze drying process parameters.

[0030] In an embodiment, the vacuum degree in the vacuum freeze drying process is < 10 Pa, and specifically can be 8 Pa, 5 Pa or 1 Pa.

[0031] In an embodiment, the vacuum degree in the vacuum freeze drying process is 5 Pa.

[0032] In an embodiment, the vacuum freeze drying control program is as follows:

[0033] -42 to -38 DEG C constant temperature 3 to 5 h, -12 to -8 DEG C constant temperature 8 to 12 h, 4 to 6 DEG C constant temperature 8 to 12 h, 9 to 11 DEG C constant temperature 10 to 14 h, 24 to 26 DEG C constant temperature 10 to 14 h.

[0034] In an embodiment, the vacuum freeze drying control program is as follows:

[0035] -40 DEG C constant temperature 4 h, -10 DEG C constant temperature 10 h, 5 DEG C constant temperature 10 h, 10 DEG C constant temperature 12 h, 25 DEG C constant temperature 12 h.

[0036] In an embodiment, the cleaning includes washing the angelica with clean water to remove dirt and impurities on the surface of the angelica.

[0037] Another embodiment of the present application provides a freeze-dried angelica prepared by the above angelica freeze drying process.

[0038] The technical solutions of the present application are further described in detail through specific embodiments.

[0039] Embodiment 1

[0040] The present embodiment is an angelica freeze drying process, which comprises the following steps:

[0041] (a) angelica pretreatment:

[0042] Select fresh Angelica free of pests and wash the Angelica with clean water to remove dirt and impurities on the surface of the Angelica;

[0043] (b) vacuum freeze-drying:

[0044] The pretreated Angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0045] -35℃ constant temperature for 5h, -5℃ constant temperature for 8h, 6℃ constant temperature for 8h, 12℃ constant temperature for 10h, 28℃ constant temperature for 10h;

[0046] The vacuum degree during the vacuum freeze-drying process is 5Pa.

[0047] Example 2

[0048] The present embodiment is a freeze-drying process for Angelica, which comprises the following steps:

[0049] (a) Angelica pretreatment:

[0050] Select fresh Angelica free of pests and wash the Angelica with clean water to remove dirt and impurities on the surface of the Angelica;

[0051] (b) vacuum freeze-drying:

[0052] The pretreated Angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0053] -45℃ constant temperature for 3h, -15℃ constant temperature for 12h, 4℃ constant temperature for 12h, 8℃ constant temperature for 14h, 22℃ constant temperature for 14h;

[0054] The vacuum degree during the vacuum freeze-drying process is 1Pa.

[0055] Example 3

[0056] The present embodiment is a freeze-drying process for Angelica, which comprises the following steps:

[0057] (a) Angelica pretreatment:

[0058] Select fresh Angelica free of pests and wash the Angelica with clean water to remove dirt and impurities on the surface of the Angelica;

[0059] (b) vacuum freeze-drying:

[0060] The pretreated Angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0061] - 38°C for 5h, -8°C for 12h, 4°C for 8h, 9°C for 14h, 26°C for 10h;

[0062] The vacuum degree during the vacuum freeze-drying process is 10 Pa.

[0063] Example 4

[0064] The present example is a freeze-drying process of angelica, which comprises the following steps:

[0065] (a) angelica pretreatment:

[0066] Fresh angelica free of pests is selected and washed with clean water to remove dirt and impurities on the surface of the angelica;

[0067] (b) vacuum freeze-drying:

[0068] The pretreated angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0069] - 42°C for 3h, -12°C for 8h, 6°C for 12h, 11°C for 10h, 24°C for 14h;

[0070] The vacuum degree during the vacuum freeze-drying process is 8 Pa.

[0071] Example 5

[0072] The present example is a freeze-drying process of angelica, which comprises the following steps:

[0073] (a) angelica pretreatment:

[0074] Fresh angelica free of pests is selected and washed with clean water to remove dirt and impurities on the surface of the angelica;

[0075] (b) vacuum freeze-drying:

[0076] The pretreated angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0077] - 40°C for 4h, -10°C for 10h, 5°C for 10h, 10°C for 12h, 25°C for 12h;

[0078] The vacuum degree during the vacuum freeze-drying process is 5 Pa.

[0079] Comparative Example 1

[0080] The present example is a freeze-drying process of angelica, which comprises the following steps:

[0081] Fresh angelica is placed in a well-ventilated sunny place to dry, and is rubbed and smoothed every day. The head residues and soil are removed, and the drying time is 3-7 days.

[0082] Comparative Example 2

[0083] The present example is a kind of angelica constant temperature blast drying process, which comprises:

[0084] Fresh angelica without pests is selected and washed with clean water to remove dirt and impurities on the surface of the angelica. Then, it is placed in a 60℃ constant temperature oven for blast drying for 40 hours.

[0085] Comparative Example 3

[0086] The present example is a kind of angelica freeze-drying process, which comprises the following steps:

[0087] (a) Angelica pretreatment:

[0088] Fresh angelica without pests is selected and washed with clean water to remove dirt and impurities on the surface of the angelica.

[0089] (b) Vacuum freeze-drying:

[0090] The pretreated angelica is placed in a vacuum drying machine for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows:

[0091] -40℃ constant temperature for 4h, -10℃ constant temperature for 10h, 10℃ constant temperature for 22h, and 25℃ constant temperature for 12h.

[0092] The vacuum degree during vacuum freeze-drying is 5Pa.

[0093] Experimental Example

[0094] The angelica is dried according to the processes of Example 5 and Comparative Examples 1-3, respectively, and then the obtained angelica is detected:

[0095] Moisture determination

[0096] The moisture content of the freeze-dried angelica sample is determined according to the method in the fourth method of Toluene Method in General Rule 0823 in Chinese Pharmacopoeia (2020 Edition, Part IV).

[0097] Ash determination

[0098] The total ash content and acid-insoluble ash content of the freeze-dried angelica sample are determined according to the method in General Rule 2302. 5g of the test sample is placed in a crucible that is ignited to a constant weight, and the weight is determined. The crucible is heated slowly, and care is taken to avoid burning. When the carbon is completely carbonized, the temperature is gradually increased to 600℃, and the sample is completely ashed and reaches a constant weight. According to the weight of the residue, the content of total ash in the test sample is calculated (%).

[0099] Leaching determination

[0100] The leaching content of the freeze-dried Angelica sinensis sample is determined according to the method in the Chinese Pharmacopoeia (2020 edition, fourth part), under the method of alcohol-soluble leaching determination in General Rule 2201. About 2 g of the test sample is accurately weighed and placed in a 250 ml flask, 100 ml of 70% ethanol is accurately added, the weight is determined, and after standing for 1 hour, a reflux condenser is connected, and heating is performed until boiling, and then micro-boiling is maintained for 1 hour. After cooling, the flask is removed, tightly sealed, and weighed again, the weight loss is made up, and then shaken and filtered through a dry filter. 25 ml of the filtrate is accurately measured and placed in an evaporating dish that has been dried to a constant weight. After evaporation on a water bath, drying is performed at 105°C for 3 hours, and then the sample is cooled in a desiccator for 30 minutes, and the weight is accurately determined. The content of alcohol-soluble leaching in the test sample is calculated (%).

[0101] Volatilized oil determination

[0102] The volatilized oil content of the freeze-dried Angelica sinensis sample is determined according to the method in the Chinese Pharmacopoeia (2020 edition, fourth part), under the method of alcohol-soluble leaching determination in General Rule 2201.

[0103] Shelf life detection (inspection)

[0104] The shelf life of Angelica sinensis prepared by different drying methods is analyzed. The product is placed in a constant temperature and humidity incubator, and the quality and hygiene indicators are measured once a month. The shelf life is calculated by months. For example, if the indicators are stable for three months, the shelf life of the product is three years.

[0105] The experimental results are shown in Table 1:

[0106] Table 1

[0107] Item Example 5 Comparative Example 1 Comparative Example 2 Comparative Example 3 Moisture content 2.2 4.6 6.9 5.4 Ash content 5.0 4.8 5.2 5.3 Extractives 60.6 53.25 44.29 50.13 Volatile oil 0.89 0.64 0.66 0.72 Shelf life 5 3 3 3

[0108] From Table 1, it can be seen that:

[0109] Compared with the comparative examples, the freeze-dried Angelica sinensis prepared by the present application has higher leaching and volatilized oil, can better retain the effective components of Angelica sinensis, and has a longer shelf life.

[0110] It should be understood that, during the development of any actual implementation, numerous implementation decisions can be made, such as in any engineering or design project. Such development efforts, while possibly complex and time-consuming, would be of a routine nature of design, fabrication and manufacture for those of ordinary skill having the benefit of this disclosure, without undue experimentation.

[0111] 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 it. Although the present invention has been described in detail with reference to preferred 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 spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A freeze-drying process for Angelica sinensis, characterized in that, The freeze-drying process of Angelica sinensis includes the following steps: (a. Pretreatment of Angelica sinensis:) Select fresh angelica root free from pests and diseases and wash it. (b) Vacuum freeze drying: The pretreated Angelica sinensis was placed in a vacuum dryer for vacuum freeze-drying, wherein the vacuum freeze-drying control program is as follows: -45~-35℃ constant temperature for 3~5h, -15~-5℃ constant temperature for 8~12h, 4~6℃ constant temperature for 8~12h, 8~12℃ constant temperature for 10~14h, 22~28℃ constant temperature for 10~14h.

2. The freeze-drying process for Angelica sinensis according to claim 1, characterized in that, The vacuum degree during the vacuum freeze-drying process is <10 Pa.

3. The freeze-drying process for Angelica sinensis according to claim 1, characterized in that, The vacuum degree during the vacuum freeze-drying process is 5 Pa.

4. The freeze-drying process for Angelica sinensis according to claim 1, characterized in that, The vacuum freeze-drying control procedure is as follows: -42~-38℃ for 3~5 hours, -12~-8℃ for 8~12 hours, 4~6℃ for 8~12 hours, 9~11℃ for 10~14 hours, and 24~26℃ for 10~14 hours.

5. The freeze-drying process for Angelica sinensis according to claim 1, characterized in that, The vacuum freeze-drying control procedure is as follows: -40℃ constant temperature for 4 hours, -10℃ constant temperature for 10 hours, 5℃ constant temperature for 10 hours, 10℃ constant temperature for 12 hours, 25℃ constant temperature for 12 hours.

6. The freeze-drying process for Angelica sinensis according to claim 1, characterized in that, The cleaning process includes rinsing the angelica root with clean water to remove dirt and impurities from its surface.

7. Freeze-dried Angelica sinensis prepared by the freeze-drying process described in any one of claims 1-6.