CN109602801A - Have effects that the preparation method of the five fingers mandarin orange broken wall medicine materical crude slice of liver-smoothing, qi-regulating protecting the stomach and relieve the pain and the five fingers mandarin orange broken wall medicine materical crude slice prepared therefrom - Google Patents
Have effects that the preparation method of the five fingers mandarin orange broken wall medicine materical crude slice of liver-smoothing, qi-regulating protecting the stomach and relieve the pain and the five fingers mandarin orange broken wall medicine materical crude slice prepared therefrom Download PDFInfo
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Abstract
The present invention relates to Chinese medicine wall cell disruption medicine materical crude slice technical field, disclose a kind of the five fingers mandarin orange broken wall medicine materical crude slice with liver-smoothing, qi-regulating protecting the stomach and relieve the pain preparation method and the five fingers mandarin orange broken wall medicine materical crude slice prepared therefrom.Method includes the following steps: (1) is by dry the five fingers mandarin orange medicinal material precomminution；(2) the five fingers mandarin orange herb in granule form made is impregnated in ethanol water；(3) filter, by obtained filter cake be freeze-dried, then -10 DEG C~0 DEG C at a temperature of place 1-3 hours；(4) the five fingers mandarin orange particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, then pulverized, obtaining granularity is 40 microns of micropowders below；(5) micropowders that step (4) obtains are mixed with 60-80 weight % ethanol water with mass ratio for 1:0.3-1, is then pelletized and is dried.The higher the five fingers mandarin orange broken wall medicine materical crude slice of broken wall ratio can be made using method of the present invention.
Description
Technical field
The present invention relates to Chinese medicine wall cell disruption medicine materical crude slice technical field, and in particular to a kind of to have effects that liver-smoothing, qi-regulating protecting the stomach and relieve the pain
The preparation method of the five fingers mandarin orange broken wall medicine materical crude slice and the five fingers mandarin orange 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.
The five fingers mandarin orange mainly originates in the ground such as Jiangsu, Zhejiang, Jiangxi, Hubei, Hunan, Sichuan, Guangxi.Its main active is
Cineole containing 1,8-, sabinene, firpene, amphene, carypohyllene and Diterpenes, sesquiterpenoid and class compound difficult to understand etc..With easypro liver
The effect of regulating qi-flowing for harmonizing stomach relieves pain.However, there is presently no the reports about the five fingers mandarin orange broken wall medicine materical crude slice and its preparation process.
Summary of the invention
The object of the present invention is to provide a kind of preparations of the five fingers mandarin orange broken wall medicine materical crude slice with liver-smoothing, qi-regulating protecting the stomach and relieve the pain
Method and the five fingers mandarin orange broken wall medicine materical crude slice prepared therefrom.
The present invention provides a kind of preparation methods of the five fingers mandarin orange broken wall medicine materical crude slice with liver-smoothing, qi-regulating protecting the stomach and relieve the pain, should
Method the following steps are included:
It (1) is the particle of 10-100 mesh by dry the five fingers mandarin orange medicinal material precomminution to granularity；
(2) the five fingers mandarin orange herb in granule form made impregnates 1- at 50-80 DEG C in the ethanol water of 30-60 weight %
3 hours；
(3) it filters, obtained filter cake is carried out under conditions of temperature is -10 DEG C~-50 DEG C, vacuum degree is 5-50Pa cold
Be lyophilized it is dry, then -10 DEG C~0 DEG C at a temperature of place 1-3 hours；
(4) the five fingers mandarin orange particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, then carry out Ultramicro-powder
Broken, obtaining granularity is 40 microns of micropowders below；
(5) micropowders for obtaining step (4) and 60-80 weight % ethanol water are mixed for 1:0.3-1 with mass ratio
It closes, is then pelletized and dried.
The present invention also provides the five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice of the present invention, the five fingers mandarin orange 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 the five fingers mandarin orange
Cell wall carry out embrittlement, then by pulverize can easily make the five fingers mandarin orange breaking-wall cell, to obtain broken wall ratio
Higher the five fingers mandarin orange broken wall medicine materical crude slice.
Moreover, the product composition consistency of the five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice of the present invention the following steps are included:
It (1) is the particle of 10-100 mesh by dry the five fingers mandarin orange medicinal material precomminution to granularity；
(2) the five fingers mandarin orange herb in granule form made impregnates 1- at 50-80 DEG C in the ethanol water of 30-60 weight %
3 hours；
(3) it filters, obtained filter cake is carried out under conditions of temperature is -10 DEG C~-50 DEG C, vacuum degree is 5-50Pa cold
Be lyophilized it is dry, then -10 DEG C~0 DEG C at a temperature of place 1-3 hours；
(4) the five fingers mandarin orange particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, then carry out Ultramicro-powder
Broken, obtaining granularity is 40 microns of micropowders below；
(5) micropowders for obtaining step (4) and 60-80 weight % ethanol water are mixed for 1:0.3-1 with mass ratio
It closes, is then pelletized and dried.
In step (1), after precomminution, the size of the particle obtained after the five fingers mandarin orange pulverizing medicinal materials is 10-
100 mesh specifically, such as can be 10 mesh, 20 mesh, 30 mesh, 40 mesh, 50 mesh, 60 mesh, 70 mesh, 80 mesh, 90 mesh or 100 mesh.It is logical
Cross to the five fingers mandarin orange medicinal material carry out precomminution, improve the five fingers mandarin orange medicinal material specific surface area, thus be more advantageous to it is subsequent impregnate,
The embrittlement of the processes to the five fingers mandarin orange cell wall such as freezing and microwave treatment.In the present invention, the process of the precomminution is using this
The grinding device of field routine is implemented, and details are not described herein.
In step (2), the concentration for carrying out impregnating the ethanol water used to the five fingers mandarin orange particle can be 30-60
Weight % specifically, such as can be 30 weight %, 35 weight %, 40 weight %, 45 weight %, 50 weight %, 55 weight %
Or 60 weight %.In the preferred case, the concentration of the ethanol water is 40-50 weight %.In the present invention, use is above-mentioned
The ethanol water of concentration impregnates the five fingers mandarin orange particle, is conducive to carry out embrittlement to the five fingers mandarin orange cell wall, to be conducive to
Obtain the five fingers mandarin orange broken wall medicine materical crude slice of high sporoderm-broken rate.
In step (2), the condition of immersion may include: that temperature is 50-80 DEG C (such as 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C),
Time is 1-3 hours (such as 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours).In the present invention, by making the five fingers mandarin orange
Grain is impregnated at a relatively high temperature, freezing processing is then carried out at very low temperature, so that the five fingers mandarin orange cell is sudden and violent
It is exposed under the larger temperature difference, is conducive to carry out embrittlement to the five fingers mandarin orange cell wall in this way, to help to obtain the five of high sporoderm-broken rate
Refer to mandarin orange broken wall medicine materical crude slice.
In step (2), during the immersion, the volume ratio of the five fingers mandarin orange particle and ethanol water can be 1:
2-10, preferably 1:3-8, more preferably 1:3-5.
In step (3), the condition of freeze-drying may include: temperature be -10 DEG C~-50 DEG C (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 step (3), filtering can use the strainer filtering of this field routine.In a particular embodiment, described
Strainer can be the stainless steel cloth that mesh size is 200 mesh.
In step (4), the condition of microwave treatment may include: that temperature is 10-40 DEG C, preferably 20-30 DEG C；Time is
10-60min, preferably 20-40min；The power of microwave is 5-20kW, preferably 10-20kW；Vacuum degree is 5-50Pa, preferably
For 10-20Pa.
In step (4), it is preferable that it is 40 microns or less that the process of the ultramicro grinding, which crushes the five fingers mandarin orange particle,
The micropowders of (preferably 5-40 microns, more preferably 5-30 microns).Equipment used in pulverizing can be wall cell disruption powder
Broken machine, such as CW5-100QA broken wall micronizer.
In step (5), 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 the preferred case, the concentration of the ethanol water
It can be 65-75 weight %.
In step (5), the mixing mass ratio of the micropowders and the ethanol water is 1:0.3-1, preferably
1:0.5-0.7。
In step (5), the method for the drying can be contact drying, pneumatic conveying drying, tunnel type baking oven drying, vacuum
Drying, fluidized drying, freeze-drying, far-infrared ray drying or microwave drying.In the preferred case, the method for the drying is freezing
It is dry.
The present invention also provides the five fingers mandarin orange 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 the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of the five fingers mandarin orange particle
The ethanol solution of 45 long-pending weight % impregnates 2 hours at 70 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter cake that will be obtained
It is freeze-dried at -20 DEG C, under 30Pa vacuum degree.It is placed 2 hours at -5 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with the ethanol water that concentration is 70 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A1 be made.
Embodiment 2
(1) 2.0kg the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 80 mesh, is subsequently added into 3 times of bodies of the five fingers mandarin orange particle
The ethanol solution of 60 long-pending weight % impregnates 3 hours at 50 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter cake that will be obtained
It is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 1 hour at -8 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with the ethanol water that concentration is 65 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A2 be made.
Embodiment 3
(1) 2.0kg the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 40 mesh, is subsequently added into 5 times of bodies of the five fingers mandarin orange particle
The ethanol solution of 40 long-pending weight % impregnates 1 hour at 80 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter cake that will be obtained
It is freeze-dried at -10 DEG C, under 10Pa vacuum degree.It is placed 3 hours at -2 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
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 75 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A3 be made.
Embodiment 4
(1) 2.0kg the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 100 mesh, is subsequently added into 4 times of the five fingers mandarin orange particle
The ethanol solution of 60 weight % of volume impregnates 3 hours at 75 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 3 hours at 0 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.6 is mixed with weight ratio with the ethanol water that concentration is 65 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -20 DEG C, under 30Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A4 be made.
Embodiment 5
(1) 2.0kg the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 50 mesh, is subsequently added into 4 times of bodies of the five fingers mandarin orange particle
The ethanol solution of 40 long-pending weight % impregnates 3 hours at 60 DEG C, with the stainless steel wire net filtration of 200 mesh, the filter cake that will be obtained
It is freeze-dried at -30 DEG C, under 20Pa vacuum degree.It is placed 3 hours at -5 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
The micropowders for being 5-30 microns to granularity.
It (4) is that 1:0.7 is mixed with weight ratio with the ethanol water that concentration is 80 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -30 DEG C, under 20Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A5 be made.
Embodiment 6
(1) 2.0kg the five fingers mandarin orange medicinal material is taken, precomminution to granularity is the particle of 100 mesh, is subsequently added into 5 times of the five fingers mandarin orange particle
The ethanol solution of 50 weight % of volume impregnates 3 hours at 70 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 2 hours at -5 DEG C after the five fingers mandarin orange particle drying.
(2) the five fingers mandarin orange 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) the five fingers mandarin orange particle that step (2) obtains is pulverized with CW5-100QA broken wall micronizer, is obtained
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 60 weight % by the micropowders,
Then extrusion granulator is freeze-dried at -10 DEG C, under 10Pa vacuum degree, so that the five fingers mandarin orange broken wall medicine materical crude slice sample A6 be made.
Comparative example 1
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D1 be made.
Comparative example 2
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D2 be made.
Comparative example 3
The five fingers mandarin orange broken wall medicine materical crude slice is prepared according to the method for embodiment 3, the difference is that not implementing ethanol water immersion
Process, so that the five fingers mandarin orange broken wall medicine materical crude slice sample D3 be made.
Comparative example 4
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D4.
Comparative example 5
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D5.
Comparative example 6
The five fingers mandarin orange broken wall medicine materical crude slice is prepared according to the method for embodiment 3, the difference is that being replaced with the mode of natural air drying cold
Be lyophilized it is dry, thus be made the five fingers mandarin orange broken wall medicine materical crude slice sample D6.
Comparative example 7
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D7 be made.
Comparative example 8
The five fingers mandarin orange 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 the five fingers mandarin orange broken wall medicine materical crude slice sample D8 be made.
Comparative example 9
The five fingers mandarin orange broken wall medicine materical crude slice is prepared according to the method for embodiment 3, the difference is that after freeze without cold
Freeze storage, but directly carry out microwave treatment, so that the five fingers mandarin orange broken wall medicine materical crude slice sample D9 be made.
Test case
The non-broken cells limit of the five fingers mandarin orange broken wall medicine materical crude slice is tested with the following method: taking the five fingers mandarin orange 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 the higher the five fingers of broken wall ratio using method of the present invention
Mandarin orange 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 (7)
1. a kind of preparation method of the five fingers mandarin orange broken wall medicine materical crude slice with liver-smoothing, qi-regulating protecting the stomach and relieve the pain, which is characterized in that the party
Method the following steps are included:
It (1) is the particle of 10-100 mesh by dry the five fingers mandarin orange medicinal material precomminution to granularity；
(2) it is small that the five fingers mandarin orange herb in granule form made impregnates 1-3 in the ethanol water of 30-60 weight % at 50-80 DEG C
When；
(3) it filters, it is dry that obtained filter cake is carried out to freezing under conditions of temperature is -10 DEG C~-50 DEG C, vacuum degree is 5-50Pa
It is dry, then -10 DEG C~0 DEG C at a temperature of place 1-3 hours；
(4) the five fingers mandarin orange particle that step (3) obtains is placed under vacuum condition and carries out microwave treatment, then pulverized,
Obtaining granularity is 40 microns of micropowders below；
(5) micropowders that step (4) obtains are mixed with 60-80 weight % ethanol water with mass ratio for 1:0.3-1, so
After pelletized and dried.
2. the method according to claim 1, wherein in step (2), the concentration of the ethanol water is
40-50 weight %.
3. the method according to claim 1, wherein the granularity of the micropowders is 5-30 in step (4)
Micron.
4. the method according to claim 1, wherein in step (5), the concentration of the ethanol water is
65-75 weight %.
5. method according to claim 1 or 4, which is characterized in that in step (5), the micropowders and the second
The mixing mass ratio of alcohol solution is 1:0.5-0.7.
6. the method according to claim 1, wherein the drying is freeze-drying in step (5).
7. the five fingers mandarin orange broken wall medicine materical crude slice of the preparation of the method as described in any one of claim 1-6.
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| CN201811543087.1A CN109602801A (en) | 2018-12-17 | 2018-12-17 | Have effects that the preparation method of the five fingers mandarin orange broken wall medicine materical crude slice of liver-smoothing, qi-regulating protecting the stomach and relieve the pain and the five fingers mandarin orange broken wall medicine materical crude slice prepared therefrom |
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Application publication date: 20190412 |