CN111265569A - Preparation method of cistanche superfine powder - Google Patents

Preparation method of cistanche superfine powder Download PDF

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CN111265569A
CN111265569A CN201911005772.3A CN201911005772A CN111265569A CN 111265569 A CN111265569 A CN 111265569A CN 201911005772 A CN201911005772 A CN 201911005772A CN 111265569 A CN111265569 A CN 111265569A
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drying
cistanche
preparation
superfine powder
temperature
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宋玉霞
聂峰杰
陈学军
张丽
甘晓燕
巩檑
丁学兵
刘璇
杨文静
陈虎
陈虞超
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Agricultural Biotechnology Research Center Of Ningxia Academy Of Agriculture And Forestry Sciences (ningxia Key Laboratory Of Agricultural Biotechnology)
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/64Orobanchaceae (Broom-rape family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting

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Abstract

The invention provides a preparation method of cistanche superfine powder, which relates to the technical field of traditional Chinese medicinal material processing, and comprises the following steps: 1) carrying out vacuum microwave drying on the cistanche slices to obtain first dried slices; the temperature of the vacuum microwave drying is 50-60 ℃; 2) drying the first drying sheet obtained in the step 1) in an air circulation drying environment to obtain a second drying sheet; the water content of the second drying sheet is 1-5%; 3) micronizing the obtained second dried tablet to obtain superfine powder; the particle size of the superfine powder is less than 20 mu m. The preparation method of the cistanche superfine powder provided by the invention adopts a vacuum low-temperature microwave drying technology, so that polysaccharide of a cistanche dried product is not oxidized, cells are loosened and not shrunk in a vacuum environment, the active ingredients of cistanche are retained to the maximum extent, and the problems that moisture in the cells is difficult to remove in normal-temperature drying of cistanche and polysaccharide is easily oxidized and cells are shrunk in a high-temperature drying process are solved.

Description

Preparation method of cistanche superfine powder
Technical Field
The invention relates to the technical field of traditional Chinese medicine processing, and in particular relates to a preparation method of cistanche superfine powder.
Background
Cistanche salsa is a perennial parasitic herbaceous plant and mainly parasitizes at the roots of arenaceous plants such as haloxylon ammodendron and the like. Cistanchis herba takes succulent stem with scaly leaves as medicine, and the main components of acteoside and echinacoside are phenylethanoid glycosides compounds, and has pharmacological effects of improving organism immunity, enhancing physical strength, relieving fatigue, resisting tumor, improving sexual dysfunction, loosening bowel to relieve constipation, protecting liver, improving memory dysfunction, preventing senile dementia, improving brain circulation, promoting nerve cell growth and repair, resisting atherosclerosis, etc.
The polysaccharide content of the cistanche deserticola can reach 58.4 percent; the water content can reach more than 80%, wherein 70% of water exists among cells, and 30% of water exists in polysaccharide bodies in the cells. The processing of the cistanche deserticola in the prior art adopts a normal temperature drying method and a high temperature drying method. The normal temperature drying method can only remove intercellular water, and is difficult to remove intracellular water. The high-temperature drying method can remove intracellular water to cause severe shrinkage of cells and oxidation of polysaccharide in cistanche cells, so that dried cistanche is black and hard, effective components are lost and the cistanche is difficult to process.
Disclosure of Invention
In view of the above, the present invention is directed to a method for preparing cistanche ultra-fine powder. The preparation method of the cistanche superfine powder provided by the invention adopts a vacuum low-temperature microwave drying technology, so that polysaccharide of a cistanche dried product is not oxidized, cells are loosened and not shrunk in a vacuum environment, the active ingredients of cistanche are retained to the maximum extent, and the problems that moisture in the cells is difficult to remove in normal-temperature drying of cistanche and polysaccharide is easily oxidized and cells are shrunk in a high-temperature drying process are solved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of cistanche superfine powder, which comprises the following steps:
1) carrying out vacuum microwave drying on the cistanche slices to obtain first dried slices; the temperature of the vacuum microwave drying is 50-60 ℃;
2) placing the first drying sheet obtained in the step 1) in an air circulation drying environment for drying to obtain a second drying sheet; the water content of the second drying sheet is 1-5%;
3) micronizing the second drying sheet obtained in the step 2) to obtain superfine powder; the particle size of the superfine powder is less than 20 mu m.
Preferably, the thickness of the cistanche slice in the step 1) is 0.1-0.4 cm.
Preferably, the vacuum degree of the vacuum microwave drying in the step 1) is-10 Pa to-6 Pa.
Preferably, the power of the vacuum microwave drying in the step 1) is 18-20 KW.
Preferably, the time of vacuum microwave drying in the step 1) is 15-20 min.
Preferably, the conditions of the stroke cycle drying environment of step 2) include: the air of the wind circulation is air; the temperature of the air circulation drying is 50-60 ℃; the air circulation drying time is 1-4 h.
Preferably, the micronization in the step 3) adopts a vibrating water-cooling micronization method.
Preferably, the superfine grinding time is 6-10 min.
The invention has the beneficial effects that: the invention provides a preparation method of cistanche superfine powder. The method provided by the invention adopts a vacuum low-temperature microwave drying technology, so that polysaccharides of the dried cistanche deserticola are not oxidized, cells are loosened and not shrunk in a vacuum environment, the active ingredients of the cistanche deserticola are retained to the maximum extent, and the problems that the moisture in the cells is difficult to remove in normal-temperature drying of the cistanche deserticola and the polysaccharides are easily oxidized and the cells are shrunk in a high-temperature drying process are solved. The invention adopts the vibrating water-cooling superfine powder grinding machine, avoids the adhesion of cistanche powder caused by the temperature rise in the grinding process, breaks the cell wall to the micron-sized range after superfine grinding, fully exposes the effective components in the cell, greatly improves the release speed and the release amount of the medicine, and can promote the dissolution and the absorption of the effective components. The cistanche superfine powder prepared by the preparation method has the powder yield of 98 percent, the retention rate of verbascoside and echinacoside in the cistanche superfine powder of 98 percent and the dissolution rate of 96 percent.
Drawings
FIG. 1 is a microscopic characteristic diagram of cistanche powder prepared at different micronization times under a scanning electron microscope; wherein A is micronization for 2 min; b is 4 min; c is 6 min; d is 8 min; e is 10 min; f is 12 min.
Detailed Description
The invention provides a preparation method of cistanche superfine powder, which comprises the following steps:
1) carrying out vacuum microwave drying on the cistanche slices to obtain first dried slices; the temperature of the vacuum microwave drying is 50-60 ℃;
2) placing the first drying sheet obtained in the step 1) in an air circulation drying environment for drying to obtain a second drying sheet; the water content of the second drying sheet is 1-5%;
3) micronizing the second drying sheet obtained in the step 2) to obtain superfine powder; the particle size of the superfine powder is less than 20 mu m.
The cistanche deserticola slice is subjected to vacuum microwave drying to obtain a first dried slice; the temperature of the vacuum microwave drying is 50-60 ℃, and is preferably 55 ℃.
In the present invention, the thickness of the cistanche slice is preferably 0.1 to 0.4cm, more preferably 0.15 to 0.35cm, and most preferably 0.2 to 0.3 cm. In the present invention, the cistanche slice is preferably prepared by slicing fresh cistanche using a ceramic knife. In the present invention, the fresh cistanche deserticola is preferably unearthed and unopened cistanche deserticola. In the invention, before the cistanche is sliced, the cistanche is preferably soaked and cleaned in clear water, and scales are removed.
In the invention, the vacuum degree of the vacuum microwave drying is preferably-10 to-6 Pa, and more preferably-9 to-8 Pa; the power of the vacuum microwave drying is preferably 18-20 KW, and more preferably 19 KW; the time for vacuum microwave drying is preferably 15-20 min, and more preferably 18 min.
In the present invention, the water content of the first drying sheet is preferably 10% or less.
The obtained first drying sheet is placed in an air circulation drying environment for drying to obtain a second drying sheet; the water content of the second drying sheet is 1-5%, and preferably 2-3%.
In the present invention, the conditions of the air circulation drying environment preferably include: the air of the wind circulation is air; the temperature of the air circulation drying is 50-60 ℃, and the optimal temperature is 55 ℃; the time of the air circulation drying is 1-4 h, preferably 2-3 h.
In the invention, the water content of the second drying sheet is 1-5%, preferably 3-4%.
The obtained second drying sheet is subjected to superfine grinding to obtain superfine powder; the particle size of the superfine powder is less than 20 mu m.
In the present invention, the ultrafine pulverization is preferably carried out by a method of water-cooling ultrafine pulverization with a vibration type. In the invention, the time for superfine grinding is preferably 6-10 min, and more preferably 8 min.
In the present invention, it is preferable that the fine cistanche powder is canned in an environment having a humidity of 20% or less and then hermetically stored.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the cistanche superfine powder comprises the following steps:
A. selecting materials: selecting fresh cistanche deserticola which is not unearthed and not bloomed, screening and classifying, putting into a freezing disc, covering all the fresh cistanche deserticola with clear sand, putting on a goods shelf of a refrigeration house, and adjusting the temperature of the refrigeration house to 0-5 ℃ for storage;
B. cleaning: soaking herba cistanches in a water pool for initial washing, then peeling and removing squama Manis, completely removing sand at the root of squama Manis with a small spoon, putting in clear water, brushing with a brush, draining water, and slicing;
C. slicing: transversely cutting cleaned Cistanchis herba into 0.2cm slices, spreading the slices on a special magnetic disk of a microwave oven, aligning, pressing up and down, and placing into the microwave oven;
D. vacuum microwave drying: adjusting the temperature to 55 ℃, adjusting the pressure to-9 to-8 Pa, and drying for 18min to obtain a first drying sheet;
E. secondary drying: placing the first drying sheet after microwave drying in an air circulation drying box for secondary drying until the water content of the material is 2.3% to obtain a second drying sheet;
F. powdering: and (4) pulverizing the second dried slices into powder for 8min by using a vibrating water-cooling ultramicro pulverizing machine, wherein the fineness of the powder is more than 400 meshes, so as to obtain the cistanche superfine powder.
Example 2
Color, taste, water content, verbascoside content and echinacoside content of different cistanche (fresh cistanche, primary dried cistanche slice, secondary dried cistanche slice and cistanche ultra-fine powder) in the preparation process of example 1 were measured respectively, and the results are shown in table 1.
The determination method comprises the following steps: according to the content determination method of echinacoside and verbascoside in Chinese pharmacopoeia, a high performance liquid chromatography method is adopted for determination.
TABLE 1 data for determining color, taste, water content, verbascoside content and echinacoside content of different cistanches during preparation
Figure BDA0002242724850000041
Figure BDA0002242724850000051
The results in Table 1 show that the cistanche superfine powder prepared by the preparation method has golden color and luster, sweet and slightly bitter taste, the content of verbascoside reaches 20.5366ug/g, and the content of echinacoside reaches 55.8962 ug/g.
Example 3
The average particle size, the powder yield, the retention rate and the dissolution rate of verbascoside and echinacoside of the cistanche powder in example 1 were measured, and the color and the taste of the powder after brewing are shown in table 2.
Table 2 data relating to cistanche powder of example 1
Figure BDA0002242724850000052
Comparative example 1
The preparation method of the cistanche powder comprises the following steps:
cutting cleaned Cistanchis herba into 0.2cm slices, vacuum drying at low temperature to water content of 8%, pulverizing for 8min with vibration type water-cooling ultramicro pulverizing machine, and determining by high performance liquid chromatography according to determination method of echinacoside and verbascoside in Chinese pharmacopoeia. The average particle diameter, powder yield, retention rate and dissolution rate of verbascoside and echinacoside of the obtained cistanche powder, and the color and the taste of the powder after brewing are shown in Table 3.
Table 3 data relating to cistanche powder of comparative example 1
Figure BDA0002242724850000053
Figure BDA0002242724850000061
From the results of the example 3 and the comparative example 1, the cistanche superfine powder prepared by the preparation method disclosed by the invention is golden yellow in color, fragrant, sweet and slightly bitter in taste, the powder yield reaches 98%, the retention rates of verbascoside and echinacoside respectively reach 98%, and the dissolution rates respectively reach 96%.
Example 4
The preparation method of the cistanche deserticola submicron powder is the same as that of the embodiment 1 except that the powdering time is 6 min.
Example 5
The preparation method of the cistanche deserticola submicron powder is the same as that of the embodiment 1 except that the powdering time is 10 min.
Comparative example 2
The preparation method of the cistanche deserticola submicron powder is the same as that of the embodiment 1 except that the powdering time is 2 min.
Comparative example 3
The preparation method of the cistanche deserticola submicron powder is the same as that of the embodiment 1 except that the powdering time is 4 min.
Comparative example 4
The preparation method of the cistanche deserticola submicron powder is the same as that of the embodiment 1 except that the powdering time is 12 min.
The average particle size, the powder yield, the caking time, the retention rate and the dissolution rate of verbascoside and echinacoside of cistanche powder prepared in examples 1, 4-5 and comparative examples 2-4 are shown in Table 4. The surface microscopic characteristic diagram of the cistanche powder prepared in the examples 1, 3-4 and the comparative examples 2-4 after being stored for 120 days is shown in figure 1.
TABLE 4 data relating to cistanche powder prepared in examples 1, 4 to 5 and comparative examples 2 to 4
Figure BDA0002242724850000062
Figure BDA0002242724850000071
From the results, the average particle size of the cistanche superfine powder prepared by the preparation method is 15-30 um, the powder yield reaches 92-98%, the preservation time reaches 120-180 d, the verbascoside retention rate reaches 98%, the verbascoside dissolution rate reaches 90-96%, the echinacoside retention rate reaches 98%, and the echinacoside dissolution rate reaches 91-96%. Compared with comparative examples 2 and 3, the average particle size is small, the powder yield is high, and the dissolution rates of the verbascoside and the echinacoside are high; the storage time was longer than that of comparative example 4.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (8)

1. The preparation method of the cistanche ultrafine powder is characterized by comprising the following steps:
1) carrying out vacuum microwave drying on the cistanche slices to obtain first dried slices; the temperature of the vacuum microwave drying is 50-60 ℃;
2) placing the first drying sheet obtained in the step 1) in an air circulation drying environment for drying to obtain a second drying sheet; the water content of the second drying sheet is 1-5%;
3) micronizing the second drying sheet obtained in the step 2) to obtain superfine powder; the particle size of the superfine powder is less than 20 mu m.
2. The preparation method according to claim 1, wherein the thickness of the cistanche slice in the step 1) is 0.1-0.4 cm.
3. The method according to claim 1, wherein the vacuum degree of the vacuum microwave drying in the step 1) is-10 to-6 Pa.
4. The preparation method of claim 1, wherein the power of the vacuum microwave drying in the step 1) is 18-20 KW.
5. The preparation method according to claim 1, wherein the time of the vacuum microwave drying in the step 1) is 15-20 min.
6. The method of claim 1, wherein the conditions of the dry environment of the stroke cycle of step 2) include: the air of the wind circulation is air; the temperature of the air circulation drying is 50-60 ℃; the air circulation drying time is 1-4 h.
7. The method according to claim 1, wherein the micronization in step 3) is carried out by vibration type water-cooling micronization.
8. The method according to claim 7, wherein the duration of the ultrafine pulverization is 6 to 10 min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112369600A (en) * 2020-11-12 2021-02-19 宁夏农林科学院农业生物技术研究中心(宁夏农业生物技术重点实验室) Chewable tablet containing cistanche and preparation method thereof
CN113082086A (en) * 2021-05-08 2021-07-09 冯美灵 Processing method of traditional Chinese medicine decoction pieces

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CN106031749A (en) * 2015-03-18 2016-10-19 民勤县天盛农业科技有限公司 Drying fresh-keeping processing method for cistanche deserticola
CN104997849A (en) * 2015-06-25 2015-10-28 孟令刚 Cistanche extraction process and forms and food prepared by using the process
CN105011159A (en) * 2015-06-25 2015-11-04 孟令刚 Herba cistanches powder making process and preparation and food prepared by utilizing the powder making process

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112369600A (en) * 2020-11-12 2021-02-19 宁夏农林科学院农业生物技术研究中心(宁夏农业生物技术重点实验室) Chewable tablet containing cistanche and preparation method thereof
CN113082086A (en) * 2021-05-08 2021-07-09 冯美灵 Processing method of traditional Chinese medicine decoction pieces

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