CN109528797A - Have effects that the preparation method of clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice and elephants-foot broken wall medicine materical crude slice prepared therefrom - Google Patents

Have effects that the preparation method of clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice and elephants-foot broken wall medicine materical crude slice prepared therefrom Download PDF

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CN109528797A
CN109528797A CN201811589007.6A CN201811589007A CN109528797A CN 109528797 A CN109528797 A CN 109528797A CN 201811589007 A CN201811589007 A CN 201811589007A CN 109528797 A CN109528797 A CN 109528797A
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elephants
foot
broken wall
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廖年生
胡贤德
杨健平
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Jiangxi Gan Long Pharmaceutical Co Ltd
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    • A61P7/10Antioedematous agents; Diuretics
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • 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
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    • 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 present invention relates to Chinese medicine wall cell disruption medicine materical crude slice technical fields, disclose a kind of preparation method with clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice and elephants-foot broken wall medicine materical crude slice prepared therefrom.Method includes the following steps: (1) then impregnates dry elephants-foot medicinal material precomminution with ethanol water;(2) it filters, obtained filter cake is freeze-dried;(3) then -10 DEG C~0 DEG C at a temperature of place 1-3 hours;(4) the elephants-foot particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment;(5) the elephants-foot particle that step (4) obtains is pulverized;(6) gained micropowders are mixed with ethanol water, is then pelletized and is freeze-dried.The higher elephants-foot broken wall medicine materical crude slice of broken wall ratio can be made using method of the present invention.

Description

The preparation method for having effects that clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice And elephants-foot broken wall medicine materical crude slice prepared therefrom
Technical field
The present invention relates to Chinese medicine wall cell disruption medicine materical crude slice technical fields, and in particular to one kind has effects that clearing heat and detoxicating and inducing diuresis to remove edema Elephants-foot broken wall medicine materical crude slice preparation method and elephants-foot broken wall medicine materical crude slice prepared therefrom.
Background technique
Chinese medicine wall cell disruption medicine materical crude slice be with modern superfine communication technique by traditional medicine materical crude slice be process it is a kind of in powder form The prepared slices of Chinese crude drugs being used as medicine.Chinese medicine wall cell disruption medicine materical crude slice is that full ingredient is used as medicine, and medical substance basis is constant, meets the intension of the prepared slices of Chinese crude drugs, The nature and flavor of medicine materical crude slice and channel tropism after broken wall, function keep consistent with the tradition property of medicine materical crude slice with curing mainly etc., and broken wall medicine materical crude slice can be straight It connects to brew and take, can be taken together with the dregs of a decoction.But medicine materical crude slice manufacturing enterprise applies not broken wall medicine materical crude slice technology at home at present Extensively, real industry standard is not formed yet.Therefore, a kind of preparation method of Chinese medicine wall cell disruption medicine materical crude slice is researched and developed, sufficiently The advantage that the full ingredient of Chinese medicine wall cell disruption medicine materical crude slice is used as medicine is played, whole effective components of traditional Chinese medicine are retained by broken wall, and then more sharp In absorption of the user to effective component, is extracted with alleviating after existing Chinese medicine particle adds water to be concentrated, Chinese medicine part can only be extracted The problem of effective component, becomes very necessary and urgent.
Elephants-foot (Elephantopus scaber L.) is composite family, and Elephantopus, upright draft is born on meadow, is produced In provinces and regions such as Zhejiang, Jiangxi, Fujian, Taiwan, Hunan, Guangdong, Guangxi, Guizhou and Yunnan, have clearing heat and detoxicating, inducing diuresis to remove edema Effect is mainly used for treating flu, acute tonsillitis, sphagitis, eye conjunctivitis, Japanese Type-B encephalitis, pertussis, acute The diseases such as icteric hepatitis, cirrhotic ascites, urgency/chronic nephritis, furuncle, eczema.However, there is presently no about elephants-foot broken wall The report of medicine materical crude slice and its preparation process.
Summary of the invention
The object of the present invention is to provide a kind of systems with clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice Preparation Method and elephants-foot broken wall medicine materical crude slice prepared therefrom.
Have effects that the clearing heat and detoxicating preparation method with the elephants-foot broken wall medicine materical crude slice of inducing diuresis to remove edema the present invention provides a kind of, Method includes the following steps:
(1) it is the particle of 10-100 mesh by dry elephants-foot medicinal material precomminution to granularity, then uses 30-60 weight % Ethanol water impregnate, wherein the condition of immersion include: temperature be 40-60 DEG C, the time be 1-3 hours;
(2) it filters, obtained filter cake is freeze-dried, wherein the condition of freeze-drying includes: that temperature is -10 DEG C~-50 DEG C, vacuum degree 5-50Pa;
(3) then -10 DEG C~0 DEG C at a temperature of place 1-3 hours;
(4) the elephants-foot particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment It include: temperature is 10-40 DEG C, time 10-60min, the power of microwave is 5-20kW, vacuum degree 5-50Pa;
(5) the elephants-foot particle that step (4) obtains is pulverized, obtaining granularity is 40 microns below ultra tiny Powder;
(6) micropowders are mixed with the ethanol water of 60-80 weight %, is then pelletized and freezed and is dry It is dry, wherein the mixing mass ratio of the micropowders and the ethanol water is 1:0.3-1.
Preferably, in step (1), the concentration of the ethanol water is 40-50 weight %.
Preferably, in step (4), it is 5-30 microns that the process of the ultramicro grinding, which crushes the elephants-foot particle, Micropowders.
Preferably, in step (6), the concentration of the ethanol water is 65-75 weight %.
Preferably, in step (6), the mixing mass ratio of the micropowders and the ethanol water is 1:0.5- 0.7。
The present invention also provides the elephants-foot broken wall medicine materical crude slice prepared by the above method.
The beneficial effects of the present invention are:
According to the preparation method of elephants-foot broken wall medicine materical crude slice of the present invention, elephants-foot medicinal material is subjected to precomminution first, Then it successively impregnated, be freeze-dried, stored frozen and microwave treatment, a whole set for the treatment of process in this way can be to elephants-foot Cell wall carry out embrittlement, then by pulverize can easily make elephants-foot breaking-wall cell, to obtain broken wall ratio Higher elephants-foot broken wall medicine materical crude slice.
Moreover, the product composition consistency of the elephants-foot broken wall medicine materical crude slice prepared according to the method described in the present invention is preferable, matter Amount is stablized, is controllable, is conducive to modern big industrialized development significantly.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more New numberical range, these numberical ranges should be considered as specific open herein.
The preparation method of elephants-foot broken wall medicine materical crude slice of the present invention the following steps are included:
(1) it is the particle of 10-100 mesh by dry elephants-foot medicinal material precomminution to granularity, then uses 30-60 weight % Ethanol water impregnate, wherein the condition of immersion include: temperature be 40-60 DEG C, the time be 1-3 hours;
(2) it filters, obtained filter cake is freeze-dried, wherein the condition of freeze-drying includes: that temperature is -10 DEG C~-50 DEG C, vacuum degree 5-50Pa;
(3) then -10 DEG C~0 DEG C at a temperature of place 1-3 hours;
(4) the elephants-foot particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment It include: temperature is 10-40 DEG C, time 10-60min, the power of microwave is 5-20kW, vacuum degree 5-50Pa;
(5) the elephants-foot particle that step (4) obtains is pulverized, obtaining granularity is 40 microns below ultra tiny Powder;
(6) micropowders are mixed with the ethanol water of 60-80 weight %, is then pelletized and freezed and is dry It is dry, wherein the mixing mass ratio of the micropowders and the ethanol water is 1:0.3-1.
In method of the present invention, after precomminution, the particle that is obtained after the elephants-foot pulverizing medicinal materials It specifically, such as can be 10 mesh, 20 mesh, 30 mesh, 40 mesh, 50 mesh, 60 mesh, 70 mesh, 80 mesh, 90 mesh having a size of 10-100 mesh Or 100 mesh.By carrying out precomminution to the elephants-foot medicinal material, the specific surface area of elephants-foot medicinal material is improved, to be more advantageous to The embrittlement of the processes to elephants-foot cell wall such as subsequent immersion, freezing and microwave treatment.In the present invention, the precomminution Process is implemented using the grinding device of this field routine, and details are not described herein.
In method of the present invention, the concentration that gallbladder grass particle impregnate the ethanol water used over the ground can Think 30-60 weight %, specifically, such as can be 30 weight %, 35 weight %, 40 weight %, 45 weight %, 50 weights Measure %, 55 weight % or 60 weight %.In the preferred case, the concentration of the ethanol water is 40-50 weight %.In this hair In bright, using the ethanol water of above-mentioned concentration, gallbladder grass particle is impregnated over the ground, is conducive to carry out elephants-foot cell wall crisp Change, to help to obtain the elephants-foot broken wall medicine materical crude slice of high sporoderm-broken rate.
In method of the present invention, the condition of immersion may include: that temperature is 40-60 DEG C of (such as 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or 60 DEG C), the time be 1-3 hours (such as 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours).In the present invention In, by impregnating elephants-foot particle at a relatively high temperature, freezing processing is then carried out at very low temperature, So that elephants-foot cell is exposed under the larger temperature difference, be conducive to carry out embrittlement to elephants-foot cell wall in this way, to be conducive to Obtain the elephants-foot broken wall medicine materical crude slice of high sporoderm-broken rate.
In method of the present invention, during the immersion, the volume of elephants-foot particle and ethanol water Than that can be 1:2-10, preferably 1:3-8, more preferably 1:3-5.
In method of the present invention, the condition of freeze-drying may include: that temperature is -10 DEG C~-50 DEG C (such as -10 DEG C, -15 DEG C, -20 DEG C, -25 DEG C, -30 DEG C, -35 DEG C, -40 DEG C, -45 DEG C or -50 DEG C), vacuum degree be 5-50Pa (such as 5Pa, 10Pa, 20Pa, 30Pa, 40Pa or 50Pa).Herein, vacuum degree refers to absolute pressure.
In method of the present invention, filtering can use the strainer filtering of this field routine.In specific embodiment party In formula, the strainer can be the stainless steel cloth that mesh size is 200 mesh.
In method of the present invention, the condition of microwave treatment may include: that temperature is 10-40 DEG C, preferably 20-30 ℃;Time is 10-60min, preferably 20-40min;The power of microwave is 5-20kW, preferably 10-20kW;Vacuum degree is 5- 50Pa, preferably 10-20Pa.
In method of the present invention, it is preferable that the process of the ultramicro grinding, which crushes the elephants-foot particle, is The micropowders of 40 microns or less (preferably 5-40 microns, more preferably 5-30 microns).Equipment used in pulverizing can Wall-broken grinder is thought, such as CW5-100QA broken wall micronizer.
In step (6), the concentration of the ethanol water can be 60-80 weight %, specifically, such as can be 60 Weight %, 65 weight %, 70 weight %, 75 weight % or 80 weight %.
In step (6), the mixing mass ratio of the micropowders and the ethanol water is 1:0.3-1, preferably 1:0.5-0.7。
The present invention also provides the elephants-foot broken wall medicine materical crude slice prepared by the above method.
The present invention will be described in detail by way of examples below.
Embodiment 1
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of elephants-foot particle The ethanol solution of 45 long-pending weight % impregnates 2 hours at 50 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 25 DEG C, time 30min, and the power of microwave is 15kW, vacuum degree 15Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with ethanol water that concentration is 70 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A1。
Embodiment 2
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 3 times of bodies of elephants-foot particle The ethanol solution of 60 long-pending weight % impregnates 3 hours at 40 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 20 DEG C, time 40min, and the power of microwave is 10kW, vacuum degree 10Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with ethanol water that concentration is 60 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A2。
Embodiment 3
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 40 mesh, is subsequently added into 5 times of bodies of elephants-foot particle The ethanol solution of 40 long-pending weight % impregnates 1 hour at 60 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 30 DEG C, time 20min, and the power of microwave is 20kW, vacuum degree 20Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.5 is mixed with weight ratio with ethanol water that concentration is 80 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A3。
Embodiment 4
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 100 mesh, is subsequently added into 4 times of elephants-foot particle The ethanol solution of 34 weight % of volume impregnates 3 hours at 42 DEG C, with the stainless steel wire net filtration of 200 mesh, by what is obtained Filter cake is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 25 DEG C, time 30min, and the power of microwave is 15kW, vacuum degree 15Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with ethanol water that concentration is 70 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A4。
Embodiment 5
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 60 mesh, is subsequently added into 3 times of bodies of elephants-foot particle The ethanol solution of 30 long-pending weight % impregnates 3 hours at 44 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 20 DEG C, time 40min, and the power of microwave is 10kW, vacuum degree 10Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with ethanol water that concentration is 60 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A5。
Embodiment 6
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 5 times of bodies of elephants-foot particle The ethanol solution of 32 long-pending weight % impregnates 3 hours at 45 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 30 DEG C, time 20min, and the power of microwave is 20kW, vacuum degree 20Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.5 is mixed with weight ratio with ethanol water that concentration is 80 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A6。
Embodiment 7
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of elephants-foot particle The ethanol solution of 36 long-pending weight % impregnates 3 hours at 46 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 25 DEG C, time 30min, and the power of microwave is 15kW, vacuum degree 15Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with ethanol water that concentration is 70 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A7。
Embodiment 8
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 3 times of bodies of elephants-foot particle The ethanol solution of 38 long-pending weight % impregnates 3 hours at 48 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 20 DEG C, time 40min, and the power of microwave is 10kW, vacuum degree 10Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with ethanol water that concentration is 60 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A8。
Embodiment 9
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 40 mesh, is subsequently added into 5 times of bodies of elephants-foot particle The ethanol solution of 42 long-pending weight % impregnates 3 hours at 51 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 30 DEG C, time 20min, and the power of microwave is 20kW, vacuum degree 20Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.5 is mixed with weight ratio with ethanol water that concentration is 80 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A9。
Embodiment 10
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of elephants-foot particle The ethanol solution of 44 long-pending weight % impregnates 3 hours at 52 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 25 DEG C, time 30min, and the power of microwave is 15kW, vacuum degree 15Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with ethanol water that concentration is 70 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A10。
Embodiment 11
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 3 times of bodies of elephants-foot particle The ethanol solution of 46 long-pending weight % impregnates 3 hours at 54 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 20 DEG C, time 40min, and the power of microwave is 10kW, vacuum degree 10Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with ethanol water that concentration is 60 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A11。
Embodiment 12
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 40 mesh, is subsequently added into 5 times of bodies of elephants-foot particle The ethanol solution of 48 long-pending weight % impregnates 3 hours at 56 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 30 DEG C, time 20min, and the power of microwave is 20kW, vacuum degree 20Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.5 is mixed with weight ratio with ethanol water that concentration is 80 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A12。
Embodiment 13
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of elephants-foot particle The ethanol solution of 52 long-pending weight % impregnates 3 hours at 57 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 25 DEG C, time 30min, and the power of microwave is 15kW, vacuum degree 15Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with ethanol water that concentration is 70 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A13。
Embodiment 14
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 3 times of bodies of elephants-foot particle The ethanol solution of 54 long-pending weight % impregnates 3 hours at 58 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 20 DEG C, time 40min, and the power of microwave is 10kW, vacuum degree 10Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with ethanol water that concentration is 60 weight % by the micropowders It closes, then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample be made A14。
Embodiment 15
(1) 2.0kg elephants-foot medicinal material is taken, precomminution to granularity is the particle of 40 mesh, is subsequently added into 5 times of bodies of elephants-foot particle The ethanol solution of 56 long-pending weight % impregnates 3 hours at 60 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter that will be obtained Cake is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after elephants-foot particle drying.
(2) the elephants-foot particle that step (1) obtains is placed under vacuum condition and carries out microwave treatment, the condition of microwave treatment Are as follows: temperature is 30 DEG C, time 20min, and the power of microwave is 20kW, vacuum degree 20Pa.
(3) it is pulverized, is obtained with the elephants-foot particle that CW5-100QA broken wall micronizer obtains step (2) The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.5 is mixed with weight ratio with the ethanol water that concentration is 80 weight % by the micropowders, Then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that elephants-foot broken wall medicine materical crude slice sample A15 be made.
Comparative example 1
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 1, the difference is that not implementing ethanol water immersion Process, so that elephants-foot broken wall medicine materical crude slice sample D1 be made.
Comparative example 2
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 1, the difference is that being replaced with the mode of natural air drying cold Be lyophilized it is dry, thus be made elephants-foot broken wall medicine materical crude slice sample D2.
Comparative example 3
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 1, the difference is that after freeze without cold Freeze storage, but directly carry out microwave treatment, so that elephants-foot broken wall medicine materical crude slice sample D3 be made.
Comparative example 4
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 2, the difference is that not implementing ethanol water immersion Process, so that elephants-foot broken wall medicine materical crude slice sample D4 be made.
Comparative example 5
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 2, the difference is that being replaced with the mode of natural air drying cold Be lyophilized it is dry, thus be made elephants-foot broken wall medicine materical crude slice sample D5.
Comparative example 6
Elephants-foot broken wall medicine materical crude slice is prepared according to the method for embodiment 2, the difference is that after freeze without cold Freeze storage, but directly carry out microwave treatment, so that elephants-foot broken wall medicine materical crude slice sample D6 be made.
Test case
The non-broken cells limit of elephants-foot broken wall medicine materical crude slice is tested with the following method: taking elephants-foot broken wall medicine materical crude slice 0.1g adds chloraldurate aqueous solution (volume ratio of chloraldurate test solution and water is 1:1) 10ml to be placed on glass slide, and load is set In microscopically observation, under 10 × 10 times of visuals field, greater than 100 microns and the powder number of complete cell is 0-5.Test As a result as shown in table 1 below.
Table 1
Can be seen that by the result of table 1 can be made broken wall ratio higher ground gallbladder using method of the present invention Careless broken wall medicine materical crude slice.
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to Protection scope of the present invention.

Claims (6)

1. a kind of preparation method with clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice, which is characterized in that packet Include following steps:
(1) it is the particle of 10-100 mesh by dry elephants-foot medicinal material precomminution to granularity, then uses the ethyl alcohol of 30-60 weight % Aqueous solution soaking, wherein the condition of immersion includes: that temperature is 40-60 DEG C, and the time is 1-3 hours;
(2) it filtering, obtained filter cake is freeze-dried, wherein the condition of freeze-drying includes: that temperature is -10 DEG C~-50 DEG C, Vacuum degree is 5-50Pa;
(3) then -10 DEG C~0 DEG C at a temperature of place 1-3 hours;
(4) the elephants-foot particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, the condition packet of microwave treatment Include: temperature is 10-40 DEG C, time 10-60min, and the power of microwave is 5-20kW, vacuum degree 5-50Pa;
(5) the elephants-foot particle that step (4) obtains is pulverized, obtaining granularity is 40 microns of micropowders below;
(6) micropowders are mixed with the ethanol water of 60-80 weight %, are then pelletized and is freeze-dried, In, the mixing mass ratio of the micropowders and the ethanol water is 1:0.3-1.
2. the method according to claim 1, wherein in step (1), the concentration of the ethanol water is 40-50 weight %.
3. method according to claim 1 or 2, which is characterized in that in step (4), the process of the ultramicro grinding will The micropowders that it is 5-30 microns that the elephants-foot particle, which crushes,.
4. method according to claim 1 or 2, which is characterized in that in step (6), the concentration of the ethanol water For 65-75 weight %.
5. method according to claim 1 or 2, which is characterized in that in step (6), the micropowders and the second The mixing mass ratio of alcohol solution is 1:0.5-0.7.
6. the elephants-foot broken wall medicine materical crude slice of the preparation of the method as described in any one of claim 1-5.
CN201811589007.6A 2018-12-25 2018-12-25 Have effects that the preparation method of clearing heat and detoxicating and inducing diuresis to remove edema elephants-foot broken wall medicine materical crude slice and elephants-foot broken wall medicine materical crude slice prepared therefrom Withdrawn CN109528797A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101768554A (en) * 2008-12-31 2010-07-07 胡如军 Technological method for breaking cell walls of ganoderma lucidum spore powder
CN102846698A (en) * 2012-08-20 2013-01-02 浙江中医药大学中药饮片有限公司 Wall-broken radix tetrastigme oral decoction pieces
CN107019718A (en) * 2017-03-15 2017-08-08 天马(安徽)国药科技股份有限公司 A kind of preparation method of Radix Codonopsis broken wall medicine materical crude slice

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101768554A (en) * 2008-12-31 2010-07-07 胡如军 Technological method for breaking cell walls of ganoderma lucidum spore powder
CN102846698A (en) * 2012-08-20 2013-01-02 浙江中医药大学中药饮片有限公司 Wall-broken radix tetrastigme oral decoction pieces
CN107019718A (en) * 2017-03-15 2017-08-08 天马(安徽)国药科技股份有限公司 A kind of preparation method of Radix Codonopsis broken wall medicine materical crude slice

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Application publication date: 20190329