CN113181242A - Vacuum drying method for fructus forsythiae - Google Patents
Vacuum drying method for fructus forsythiae Download PDFInfo
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- CN113181242A CN113181242A CN202110541338.8A CN202110541338A CN113181242A CN 113181242 A CN113181242 A CN 113181242A CN 202110541338 A CN202110541338 A CN 202110541338A CN 113181242 A CN113181242 A CN 113181242A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- 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)
- A61K36/63—Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
- A61K36/634—Forsythia
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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Abstract
The invention discloses a vacuum drying method for fructus forsythiae, and belongs to the technical field of traditional Chinese medicinal material processing. The method comprises the following steps: pre-freezing fresh fructus forsythiae at the temperature of-15 to-5 ℃ for 3 to 6 hours, then placing the fructus forsythiae under the condition of the vacuum degree of 5 to 90Pa, and controlling the temperature to be from-70 to-40 ℃ to 30 to 50 ℃ for twelve stages of vacuum drying treatment to obtain the vacuum-dried fructus forsythiae. The method provided by the invention can avoid pollution of fructus forsythiae in the processing process to the greatest extent, reduce harmful ingredients such as ash content, heavy metal and the like, and improve the quality of medicinal materials.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine processing, and particularly relates to a vacuum drying method for fructus forsythiae.
Background
The forsythia is long oval to oval, slightly flat, 1.5-2.5 cm long and 0.5-1.3 cm in diameter. The surface has irregular longitudinal wrinkles and a plurality of protuberant small spots, and 1 obvious longitudinal groove is respectively arranged on both sides. The top end is sharp. The base part has small fruit stalks or falls off. The green and red forsythia is mostly not cracked, the surface is green and brown, and the raised grey white spots are less; the texture is hard; most seeds are yellow green, slender and have wings on one side. The aged fructus forsythiae is cracked or split into two parts from the top, the surface is yellowish brown or reddish brown, and the inner surface is mostly yellowish brown and smooth and has a mediastinum. The texture is crisp; seeds are brown and mostly shed. Slightly fragrant smell and bitter taste. The medicine is divided into two kinds of green fructus forsythiae and old fructus forsythiae. In the harvesting process, selecting the green fructus forsythiae in the last ten days of 9 months, harvesting the green fructus forsythiae when the peel is not mature, slightly boiling the green fructus forsythiae in boiling water or steaming the green fructus forsythiae in a steamer for about 0.5h, and taking out and drying the green fructus forsythiae in the sun. The fruit of the old fructus forsythiae is completely ripe and turns yellow in 10 last ten days, and is harvested when the fruit shell cracks, dried in the sun and screened to remove seeds and impurities.
In the process of harvesting fructus forsythiae by adopting the prior art, effective components such as plant protein, microorganism, volatile oil and the like can be damaged, and according to relevant statistics, the drug effect of a fresh traditional Chinese medicine is several times to ten times that of a dry traditional Chinese medicine; traditional Chinese medicines are easily polluted in the traditional drying process, and the contents of ash, microorganisms, heavy metals and the like are easily out of standard; the traditional Chinese medicine decoction pieces are also easily influenced by factors such as transportation, storage, preservation and the like, so that not only is the clinical curative effect of the traditional Chinese medicine reduced, but also the quality of the Chinese patent medicine taking the decoction pieces as raw materials is restricted.
Disclosure of Invention
The invention aims to provide a vacuum freeze-drying method of forsythia suspense, aiming at the defects of the method, which can keep the freshness to the maximum extent, namely, the effective components and curative effect of the traditional Chinese medicinal materials to the maximum extent.
The invention aims to provide a method for vacuum drying forsythia suspense, which comprises the following steps:
pre-freezing fresh fructus forsythiae at the temperature of-15 to-5 ℃ for 3 to 6 hours, then placing the fructus forsythiae under the condition of the vacuum degree of 5 to 90Pa, and controlling the temperature to be from-70 to-40 ℃ to 30 to 50 ℃ for twelve stages of vacuum drying treatment to obtain the vacuum-dried fructus forsythiae.
Preferably, the temperature difference between two adjacent stages of the vacuum drying treatment is 5-20 ℃, and the heat preservation time of each stage is 1-3 hours.
More preferably, the temperature is increased in a step mode, and the temperature increase rate is 10-15 ℃/h.
Preferably, the vacuum degree is 55-85 Pa.
Preferably, fresh fructus forsythiae is sliced to a thickness of 2-3 mm before precooling, and the stacked thickness is less than or equal to 20mm during vacuum drying.
The second purpose of the invention is to provide the forsythia suspense prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
the method provided by the invention can be used for drying the forsythia suspense to achieve the maximum 'fresh keeping', namely the effective components and curative effect of the forsythia suspense can be retained to the maximum.
The vacuum drying technology is suitable for fresh fructus forsythiae, can avoid pollution of fructus forsythiae in the processing process to the greatest extent, reduce harmful ingredients such as ash content, heavy metal and the like, and improve the quality of medicinal materials.
Drawings
FIG. 1 is a thin layer chromatogram of dried Forsythia suspensa and control as provided in example 1 and comparative example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
In the following examples, a freeze dryer is used to wipe out a freeze dryer cold trap with a clean towel during vacuum drying (device preparation process); cutting fresh fructus forsythiae into pieces with the thickness of 2-3 mm, placing the fresh fructus forsythiae into a material tray, placing the material tray into a shelf of a material rack, respectively placing a material temperature-sensing probe into the fructus forsythiae material, carefully placing the material rack into a cold trap, and finally covering with an organic glass cover. Switching on a power supply, pressing any key to enter a main interface, clicking a key of a refrigerator on a screen, starting a refrigeration system, and starting pre-freezing of the fructus forsythiae material (material pre-freezing process); after the material is pre-frozen, setting the freeze-drying process section and section temperature, lifting a material tray, placing a cover plate on the opening of a cold well, placing a material tray on the cover plate, covering a glass cover, clicking an 'automatic operation' button, starting a vacuum pump, a vacuum gauge and a temperature control program at the same time, starting the vacuum pump, and starting freeze-drying according to the set program (freeze-drying process); and after the freeze drying is finished, stopping the machine and taking samples. And (4) closing the refrigeration, opening the inflation valve, then closing the vacuum pump, and taking out the sample (stopping the sampling process).
Example 1
A method for vacuum drying fructus forsythiae comprises the following steps:
slicing fresh fructus forsythiae to a thickness of about 2.5mm, placing in a freeze dryer, pre-freezing at-15 deg.C for 5h, setting vacuum degree in the range of 59-64 Pa, vacuum drying at-43 deg.C to 40 deg.C by stages, and automatically drying at a heating rate of 10 deg.C/h; the specific staged treatment temperature is as follows:
a first stage: keeping the temperature at 43 ℃ below zero for 2h,
and (2) second stage: keeping the temperature at minus 20 ℃ for 2h,
and (3) three stages: keeping the temperature at minus 10 ℃ for 2h,
and a fourth stage: keeping the temperature at minus 5 ℃ for 2h,
five stages: keeping the temperature at 0 ℃ for 2h,
six sections: keeping the temperature at 5 ℃ for 3h,
seven sections: keeping the temperature at 10 ℃ for 2h,
eight sections: keeping the temperature at 15 ℃ for 2h,
nine sections: keeping the temperature at 20 ℃ for 3h15min,
ten sections: keeping the temperature at 30 ℃ for 2h,
eleven sections: keeping the temperature at 35 ℃ for 2h,
twelve stages: keeping the temperature at 40 ℃ for 2 h; thus obtaining the vacuum dried forsythia.
Example 2
A method for vacuum drying fructus forsythiae comprises the following steps:
slicing fresh fructus forsythiae to a thickness of about 2.5mm, placing in a freeze dryer, pre-freezing at-10 deg.C for 5h, setting vacuum degree in the range of 62-72 Pa, vacuum drying at-43 deg.C to 40 deg.C by stages, and automatically drying at a temperature rise rate of 15 deg.C/h; the specific staged treatment temperature is as follows:
a first stage: keeping the temperature at minus 43 ℃ for 2h
And (2) second stage: keeping the temperature at-20 ℃ for 3h
And (3) three stages: keeping the temperature at-10 ℃ for 2h15min
And a fourth stage: keeping the temperature at minus 5 ℃ for 3h
Five stages: keeping the temperature at 0 ℃ for 2h
Six sections: keeping the temperature at 5 ℃ for 3h
Seven sections: keeping the temperature at 10 ℃ for 2h
Eight sections: keeping the temperature at 15 ℃ for 2h
Nine sections: keeping the temperature at 20 ℃ for 3h
Ten sections: keeping the temperature at 30 ℃ for 3h
Eleven sections: keeping the temperature at 35 ℃ for 2h
Twelve stages: keeping the temperature at 40 ℃ for 2 h; thus obtaining the vacuum dried forsythia.
Example 3
A method for vacuum drying fructus forsythiae comprises the following steps:
slicing fresh fructus forsythiae to a thickness of about 2.5mm, placing in a freeze dryer, pre-freezing at-5 deg.C for 5h, setting vacuum degree in the range of 67-82 Pa, vacuum drying at-43 deg.C to 40 deg.C by stages, and automatically drying at a heating rate of 12 deg.C/h; the specific staged treatment temperature is as follows:
a first stage: keeping the temperature at minus 43 ℃ for 2h
And (2) second stage: keeping the temperature at-20 ℃ for 3h
And (3) three stages: keeping the temperature at minus 10 ℃ for 2h
And a fourth stage: keeping the temperature at minus 5 ℃ for 3h
Five stages: keeping the temperature at 0 ℃ for 2h
Six sections: keeping the temperature at 5 ℃ for 3h
Seven sections: keeping the temperature at 10 ℃ for 2h
Eight sections: keeping the temperature at 15 ℃ for 2h
Nine sections: keeping the temperature at 20 ℃ for 3h
Ten sections: keeping the temperature at 30 ℃ for 3h
Eleven sections: keeping the temperature at 35 ℃ for 2h30min
Twelve stages: keeping the temperature at 40 ℃ for 2 h; thus obtaining the vacuum dried forsythia.
Comparative example 1
A method for drying fructus forsythiae comprises the following steps:
steaming fresh fructus forsythiae, and sun drying to obtain dried fructus forsythiae.
In order to illustrate the relevant performance of the vacuum drying method provided by the invention, only the relevant performance of the fructus forsythiae prepared in the example 1 is detected; the forsythia suspensa provided in example 1 is designated as "sample forsythia suspensa 1", and the forsythia suspensa provided in comparative example 1 is designated as "sample forsythia suspensa 2".
The inspection basis is as follows: "Chinese pharmacopoeia" 2020 edition one department
Identification thin layer chromatography
The standard specifies: spots of the same color should appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference drug and the reference solution, as shown in FIG. 1: 1 is fructus forsythiae sample 1(10 μ l), 2 is fructus forsythiae control drug (10 μ l), 3 is phillyrin control (5 μ l), and 4 is fructus forsythiae sample 2(10 μ l).
As a result:
1. the fructus forsythiae 1 sample shows spots of the same color in the chromatogram of the test solution at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution,
2. the sample fructus forsythiae 2 shows spots of the same color in the chromatogram of the test solution at the positions corresponding to the chromatogram of the reference solution and the chromatogram of the reference solution.
(II) checking for moisture
The standard specifies: should not exceed 10.0% (toluene method)
As a result:
1. the water content of the sample forsythia suspense 1 is 4.4%,
2. sample forsythia suspensa 2 has 6.4% moisture.
(III) examination of Total Ash
The standard specifies: should not exceed 4.0%
As a result:
1. the total ash content of the forsythia suspense 1 sample is 3.1%,
2. the total ash content of forsythia suspensa 2 sample is 3.7%.
(IV) extract
The standard specifies: according to the cold soaking method under the item of alcohol-soluble extract determination method (general rule 2201), 65% ethanol is used as a solvent, and the green forsythia is not less than 30.0%; the content of old fructus forsythiae should not be less than 16.0%. Wherein the green fructus forsythiae is fresh fructus forsythiae collected when the fruit is well-ripened and green, and the old fructus forsythiae is fresh fructus forsythiae collected when the fruit is well-ripened.
As a result:
1. the extract content of the forsythia suspense 1 sample is 35.5 percent,
2. the extract of forsythia suspensa 2 sample is 32.3%.
(V) measurement of content
Phillyrin standard provisions: the product contains phillyrin (C) calculated on dry basis27H34O11) Not less than 0.15%
As a result:
1. the content of phillyrin in the sample forsythia suspensa 1 is 0.90 percent,
2. the content of forsythin in the sample forsythia suspensa 2 is 0.15%.
Forsythoside a standard specifies: the product contains forsythoside A (C) calculated on dry product29H36O15) Not less than 0.25%
As a result:
1. the forsythoside A contained in the sample forsythia suspensa 1 is 8.6%,
2. the forsythoside A contained in the sample forsythia suspensa 2 was 6.1%.
(VI) heavy metals and harmful elements (Chinese pharmacopoeia 2020 edition 2321 general rule for verification of medicinal materials and decoction pieces)
The standard specifies: lead is not more than 5 mg/kg; the cadmium can not exceed 0.3 mg/kg; arsenic is not more than 2 mg/kg; the mercury can not exceed 0.2 mg/kg; the copper content is not more than 20mg/kg,
as a result:
1. sample forsythia 1 contains lead: 0.08mg/kg, cadmium 0.01mg/kg, arsenic: undetected, mercury: 0.02mg/kg, copper: 3.9mg/kg of the total weight of the composition,
2. sample forsythia 2 contains lead: 0.14mg/kg, cadmium: 0.02mg/kg, arsenic: undetected, mercury: 0.02mg/kg, copper: 4.6 mg/kg.
(VII) 33 forbidden pesticides (Chinese pharmacopoeia 2020 edition 0212 general inspection of medicinal materials and decoction pieces)
The standard specifies: no detection should be made (no quantification limit should be exceeded) as shown in table 1 below.
As a result: are all not detected
TABLE 1 limits of quantitation for 33 of forbidden pesticides in Forsythia suspensa
The method provided by the invention can maximally keep fresh by performing vacuum drying treatment in stages, avoid pollution of fructus forsythiae in the processing process, reduce harmful components such as ash content and heavy metal, and improve the quality of fructus forsythiae. Because the vacuum drying technology can furthest retain the active ingredients, color, fragrance, taste and shape of the forsythia, the picked fresh forsythia can be dried immediately without complicated manufacturing procedures of the traditional drying method, the freeze-dried fresh traditional Chinese medicine decoction pieces with the medicine effect which is several times higher than that of the dry product gradually replace the traditional decoction pieces, and the wide prospect is shown.
In conclusion, the method provided by the invention can be used for drying the traditional Chinese medicinal materials to maximally keep the freshness, namely, the effective components and the curative effect of the traditional Chinese medicinal materials can be retained to the greatest extent.
The vacuum drying technology is suitable for fresh medicinal materials, can avoid pollution of the medicinal materials in the processing process to the maximum extent, reduces harmful ingredients such as ash content and heavy metals, and improves the quality of the medicinal materials.
The vacuum drying technology can directly dry fresh medicinal materials, reduces the processes of manual arrangement, bundling, kneading, airing, drying in a drying room and the like in the traditional method, overcomes the defects of large workload, long period, low drying efficiency, high labor cost and the like in the traditional drying method, and can directly reduce the labor cost, and meanwhile, the method provided by the invention can effectively improve the drying efficiency and reduce the cost of energy consumption by controlling the total drying time to be 20-30 h.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (6)
1. A method for vacuum drying forsythia suspense is characterized by comprising the following steps:
pre-freezing fresh fructus forsythiae at the temperature of-15 to-5 ℃ for 3 to 6 hours, then placing the fructus forsythiae under the condition of the vacuum degree of 5 to 90Pa, and controlling the temperature to be from-70 to-40 ℃ to 30 to 50 ℃ for twelve stages of vacuum drying treatment to obtain the vacuum-dried fructus forsythiae.
2. The method for vacuum drying forsythia suspense according to claim 1, wherein the temperature difference between two adjacent stages of the vacuum drying treatment is 5 to 20 ℃, and the heat preservation time of each stage is 1 to 3 hours.
3. The method for vacuum drying forsythia suspensa as claimed in claim 2, wherein the temperature is raised in a stepwise manner at a rate of 10-15 ℃/h.
4. The method for vacuum drying forsythia suspensa according to claim 1, wherein the vacuum degree is 55 to 85 Pa.
5. The method for vacuum drying forsythia suspensa as claimed in claim 1, wherein fresh forsythia suspensa is sliced to a thickness of 2-3 mm before precooling, and the stacked thickness during vacuum drying is less than or equal to 20 mm.
6. Forsythia suspensa vacuum dried according to any one of claims 1 to 5.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450296A (en) * | 2013-08-29 | 2013-12-18 | 山西大学 | Method for rapidly preparing forsythin from forsythia suspense leaves |
| CN107296820A (en) * | 2017-06-29 | 2017-10-27 | 黑龙江神守药业有限公司 | A kind of no added lyophilized ginseng class medicinal material |
| CN108379352A (en) * | 2018-04-11 | 2018-08-10 | 广州市香雪制药股份有限公司 | The processing method of Fructus Forsythiae and processing Fructus Forsythiae obtained |
-
2021
- 2021-05-18 CN CN202110541338.8A patent/CN113181242A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450296A (en) * | 2013-08-29 | 2013-12-18 | 山西大学 | Method for rapidly preparing forsythin from forsythia suspense leaves |
| CN107296820A (en) * | 2017-06-29 | 2017-10-27 | 黑龙江神守药业有限公司 | A kind of no added lyophilized ginseng class medicinal material |
| CN108379352A (en) * | 2018-04-11 | 2018-08-10 | 广州市香雪制药股份有限公司 | The processing method of Fructus Forsythiae and processing Fructus Forsythiae obtained |
Non-Patent Citations (2)
| Title |
|---|
| 施怀生，等: "快速冷冻真空干燥技术保护中药材药学品质的研究", 《山西中医学院》 * |
| 赵润怀，等: "中药材产地加工过程传统与现代干燥技术方法的分析评价", 《中国现代中药》 * |
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