CN106963799A - A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder - Google Patents
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder Download PDFInfo
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Abstract
The invention discloses a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze；（2）Freeze grinding 30~40 minutes, obtains fresh powder；（3）Fresh powder is placed in vacuum freeze drier, temperature is down to 40~50 DEG C, is then evacuated to 15~20Pa, then temperature rises to 20~30 DEG C, continued to handle 5~6 hours under current vacuum degree condition, obtain the first powder agglomates；（4）By the first powder agglomates, soak at room temperature, addition starch, mixing mashing in distilled water, add lauryl sodium sulfate and fully mix, gained mixed material then is obtained into the second powder agglomates in 40~50 DEG C of freeze-dryings；（5）Second powder agglomates is broken into Ultramicro-powder by micronizer.Ultramicro-powder good fluidity prepared by the present invention, it is long-term to preserve caking of not reuniting；Rehydration is good, and can absorb water rapidly recovery, and its color and luster and quality and fresh goods are essentially identical, and active ingredient more can be retained preferably.
Description
Technical field
The present invention relates to a kind of preparation technology of Ultramicro-powder, and in particular to a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder.Belong to
Chinese medicine processing technique field.
Background technology
The bighead atractylodes rhizome is used as medicine with rhizome, with strengthening the spleen and replenishing qi, eliminate dampness and have diuretic effect, hidroschesis and it is antiabortive the effects such as, be mainly used in insufficiency of the spleen
Deficiency of food, abdominal distention diarrhea, phlegm retention anti-dazzle nervous, oedema, spontaneous perspiration, fetal irritability.
Traditional concocting method of the bighead atractylodes rhizome has following three kinds：
1st, the raw bighead atractylodes rhizome：Net impurity is picked, is soaked in water, soak time should suitably be grasped according to season, climate change and bighead atractylodes rhizome size,
Pull out, run through after bubble, cut into slices, dry；
2nd, rhizoma atractylodis macrocephalae：First wheat bran is spread in hot pot, when time cigarette is emerged, bighead atractylodes rhizome piece is poured into micro- stir-fry to faint yellow, takes out, weeds out
Cooled after wheat bran（Per 100 jin of bighead atractylodes rhizome piece, with 10 jin of wheat bran）3. Rhizoma Atractylodis Macrocephalae preparata：Bighead atractylodes rhizome piece is put in pot and fried with high heat to coke yellow,
Clear water is sprayed, taking-up is dried；
4th, stir-baked RHIZOMA ATRACTYLODIS MACROCEPHALAE with soil：Humus flava usta fine powder is taken, puts in pot and makes popular, bighead atractylodes rhizome piece is added, stir-fry is taken out when hanging with ashen to outside, weeded out
Soil, is cooled（Per 100 jin of bighead atractylodes rhizome piece, with 20 jin of humus flava usta fine powder）.
Modern study shows that these traditional concocting methods can destroy many active ingredients, and decocting in the later stage
Being fully dissolved out for active ingredient can not be realized in journey, Chinese medicine loss is undoubtedly caused.
The content of the invention
The purpose of the present invention is that there is provided a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder to overcome above-mentioned the deficiencies in the prior art.
To achieve the above object, the present invention uses following technical proposals：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 8~13 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 30~40 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -40~-50 DEG C, then it is evacuated to 15~
20Pa, then temperature rise to 20~30 DEG C, continue to handle 5~6 hours under current vacuum degree condition, obtain the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 2~3 hours, addition starch, mixing mashing in distilled water, add dodecyl sulphur
Sour sodium is fully mixed, and then gained mixed material is freeze-dried 10~15 hours in -40~-50 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.1~0.2：1~1.2：0.3
~0.4.
It is preferred that, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 5~10 minutes.
It is preferred that, step（2）In, liquid nitrogen was added again at interval of 4~6 minutes, the bighead atractylodes rhizome is kept liquid nitrogen moistening shape all the time
State.
It is preferred that, step（4）Advanced row pre-freeze before middle freeze-drying, is by mixed material under the conditions of -10~-18 DEG C
Solid is frozen into, and maintains the state 2~3 hours.
It is preferred that, step（4）In normal temperature be 25 DEG C.
It is preferred that, step（5）In micronizer be airslide disintegrating mill.
It is further preferred that the condition of work of airslide disintegrating mill is：Stream pressure is 1100kPa, and charging rate is 180r/
Min, grade frequency is 35Hz, and grinding time is 60~80 minutes.
It is preferred that, step（5）Middle control Ultramicro-powder particle diameter more than 95% reaches less than 10 μm.
Beneficial effects of the present invention：
The fresh bighead atractylodes rhizome is first put into liquid nitrogen and freezed by the present invention, and it is 8~13 minutes to control cooling time, is both freezed beneficial to next step
Grinding, turn avoid that cooling time is long to cause active ingredient to be lost in.Freeze grinding and first time are carried out after liquid nitrogen frozen processing
Vacuum freeze drying, obtain the first powder agglomates, grind in a cold or frozen state, it is to avoid active ingredient loss, in freeze-drying causes
Portion forms hole；Then by the first powder agglomates in distilled water soak at room temperature, distilled water enter hole in, add starch after be beaten,
In pulping process, the surface of grinding bodies is constantly filled, be wrapped in starch, greatly reduces pulping process and active ingredient is broken
It is bad；Then a small amount of lauryl sodium sulfate is added, causes material that integrally there is preferably dispersiveness after mixing, it is ensured that finally to freeze
Dry has splendid mobility with products obtained therefrom after ultramicro grinding, long-term to preserve caking of not reuniting.Starch and dodecyl sulphur
Sour sodium is conventional pharmaceutic adjuvant, harmless, and they are attached on the surface of bighead atractylodes rhizome Ultramicro-powder, both water imbibitions or water
Dissolubility make it that the rehydration of product is good, and can absorb water rapidly recovery, and its color and luster and quality and fresh goods are essentially identical, is processed with tradition
Product is compared, and active ingredient more can be retained preferably.
Embodiment
With reference to embodiment, the present invention will be further elaborated, it should explanation, the description below merely to
The present invention is explained, its content is not defined.
Embodiment 1：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 8 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 30 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -40 DEG C, is then evacuated to 15Pa, then temperature
20 DEG C are risen to, continues to handle 5 hours under current vacuum degree condition, obtains the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 2 hours, addition starch, mixing mashing in distilled water, add lauryl sodium sulfate
Fully mix, then gained mixed material is freeze-dried 10 hours in -40 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.1：1：0.3.
Wherein, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 5 minutes.During freeze grinding, every
Liquid nitrogen was added again every 4 minutes, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
Step（4）Advanced row pre-freeze before middle freeze-drying, is that mixed material is frozen into solid under the conditions of -10 DEG C, and
And maintain the state 2 hours.
Step（5）In micronizer be airslide disintegrating mill, condition of work is：Stream pressure is 1100kPa, charging speed
Spend for 180r/min, grade frequency is 35Hz, grinding time is 60 minutes.Control Ultramicro-powder particle diameter more than 95% reach 10 μm with
Under.
Embodiment 2：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 13 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 40 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -50 DEG C, is then evacuated to 20Pa, then temperature
30 DEG C are risen to, continues to handle 6 hours under current vacuum degree condition, obtains the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 3 hours, addition starch, mixing mashing in distilled water, add lauryl sodium sulfate
Fully mix, then gained mixed material is freeze-dried 15 hours in -50 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.2：1.2：0.4.
Wherein, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 10 minutes.During freeze grinding, often
Liquid nitrogen is added in 6 minutes in interval again, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
Step（4）Advanced row pre-freeze before middle freeze-drying, is that mixed material is frozen into solid under the conditions of -18 DEG C, and
And maintain the state 3 hours.
Step（5）In micronizer be airslide disintegrating mill, condition of work is：Stream pressure is 1100kPa, charging speed
Spend for 180r/min, grade frequency is 35Hz, grinding time is 80 minutes.Control Ultramicro-powder particle diameter more than 95% reach 10 μm with
Under.
Embodiment 3：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 8 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 40 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -40 DEG C, is then evacuated to 20Pa, then temperature
20 DEG C are risen to, continues to handle 6 hours under current vacuum degree condition, obtains the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 2 hours, addition starch, mixing mashing in distilled water, add lauryl sodium sulfate
Fully mix, then gained mixed material is freeze-dried 10 hours in -50 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.2：1：0.4.
Wherein, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 5 minutes.During freeze grinding, every
Liquid nitrogen was added again every 6 minutes, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
Step（4）Advanced row pre-freeze before middle freeze-drying, is that mixed material is frozen into solid under the conditions of -10 DEG C, and
And maintain the state 3 hours.
Step（5）In micronizer be airslide disintegrating mill, condition of work is：Stream pressure is 1100kPa, charging speed
Spend for 180r/min, grade frequency is 35Hz, grinding time is 60 minutes.Control Ultramicro-powder particle diameter more than 95% reach 10 μm with
Under.
Embodiment 4：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 13 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 30 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -50 DEG C, is then evacuated to 15Pa, then temperature
30 DEG C are risen to, continues to handle 5 hours under current vacuum degree condition, obtains the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 3 hours, addition starch, mixing mashing in distilled water, add lauryl sodium sulfate
Fully mix, then gained mixed material is freeze-dried 15 hours in -40 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.1：1.2：0.3.
Wherein, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 10 minutes.During freeze grinding, often
Liquid nitrogen is added in 4 minutes in interval again, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
Step（4）Advanced row pre-freeze before middle freeze-drying, is that mixed material is frozen into solid under the conditions of -18 DEG C, and
And maintain the state 2 hours.
Step（5）In micronizer be airslide disintegrating mill, condition of work is：Stream pressure is 1100kPa, charging speed
Spend for 180r/min, grade frequency is 35Hz, grinding time is 80 minutes.Control Ultramicro-powder particle diameter more than 95% reach 10 μm with
Under.
Embodiment 5：
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 10 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 35 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -45 DEG C, is then evacuated to 18Pa, then temperature
25 DEG C are risen to, continues to handle 5.5 hours under current vacuum degree condition, obtains the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 2.5 hours, addition starch, mixing mashing in distilled water, add dodecyl sulphate
Sodium is fully mixed, and then gained mixed material is freeze-dried 12 hours in -45 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.15：1.1：0.35.
Wherein, step（2）In refrigeration grinding machine using preceding with Liquid nitrogen precooler 8 minutes.During freeze grinding, every
Liquid nitrogen was added again every 5 minutes, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
Step（4）Advanced row pre-freeze before middle freeze-drying, is that mixed material is frozen into solid under the conditions of -15 DEG C, and
And maintain the state 2.5 hours.
Step（5）In micronizer be airslide disintegrating mill, condition of work is：Stream pressure is 1100kPa, charging speed
Spend for 180r/min, grade frequency is 35Hz, grinding time is 70 minutes.Control Ultramicro-powder particle diameter more than 95% reach 10 μm with
Under.
Comparative example 1
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, step（1）In cooling time be 20 minutes, remaining be the same as Example 5.
Comparative example 2
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, step（4）In, the first powder agglomates, distilled water are directly mixed into mashing with starch, its
Remaining be the same as Example 5.
Comparative example 3
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, omited steps（4）, remaining be the same as Example 5.
Comparative example 4
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, step（4）Specific method be：By the first powder agglomates in distilled water soak at room temperature
2~3 hours, then it is freeze-dried 10~15 hours in -40~-50 DEG C, obtains the second powder agglomates.Remaining be the same as Example 5.
Comparative example 5
A kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, step（4）Specific method be：By the first powder agglomates in distilled water soak at room temperature
2~3 hours, starch is added, then gained mixed material is freeze-dried 10~15 hours by mixing mashing in -40~-50 DEG C,
Obtain the second powder agglomates.Remaining be the same as Example 5.
Comparative example 6
The raw bighead atractylodes rhizome：Net impurity is picked, is soaked in water 24 hours, is pulled out, run through after bubble, cuts into slices, dries.
Test example
1st, active constituent content measuring is tested
Atractylenolide be the bighead atractylodes rhizome main active, using atractylenolide as the bighead atractylodes rhizome index components.Using efficient liquid
Phase chromatography, to the bighead atractylodes rhizome from the same place of production, is made product according to embodiment 1~5 and comparative example 1~6 respectively, carries out
The assay of atractylenolide, the results are shown in Table 1.
Chromatographic condition：Chromatographic column：Kromasil-C18Post（4.6 × 250mm, 5 μm）, mobile phase：Methanol-water（Volume ratio
80：20）, flow velocity：1.0mL/min, ultraviolet detection wavelength：276nm, column temperature：30 DEG C, the μ L of sample size 10.
The preparation of solution：Weigh atractylenolide reference substance in right amount, plus the reference substance that every 1mL contains 40 μ g is made in methanol dissolving
Solution.The life bighead atractylodes rhizome pulverized product of embodiment 1~5, the bighead atractylodes rhizome Ultramicro-powder of comparative example 1~5 or comparative example 6 is weighed respectively（Cross 80
Mesh sieve）0.5g, precision calibration is placed in conical flask with stopper, plus methanol 10mL, weighed weight, and ultrasonic extraction 15 minutes is supplied and subtracted
The weight of mistake, solution is crossed after 0.45 μm of miillpore filter, obtains need testing solution.
The atractylenolide content of table 1.
As shown in Table 1, the atractylenolide content in the Ultramicro-powder product of embodiment 1~5 is higher, and comparative example 1 and comparative example 2 contain
Amount is lower slightly, and atractylenolide has certain loss in the processing procedure of comparative example 3~5, and the atractylenolide of comparative example 6 is lost in serious.
Illustrate the superfine preparation method of the present invention, more contribute to retaining for active ingredient.
2nd, fluidity determining
Angle of repose measure is carried out to the Ultramicro-powder of embodiment 1~5 and comparative example 1~5 using Repose angle gauge, be the results are shown in Table
2。
The fluidity determining of table 2.
As can be seen from Table 2, the angle of repose of embodiment 1~5 and comparative example 1 is small, and mobility more preferably, and adjusts starch and 12
The feeding mode of sodium alkyl sulfate or correlation step is omitted, mobility variation can be directly resulted in.Illustrate starch and dodecyl
The addition of sodium sulphate ensure that the mobility of product.
3rd, rehydration is tested
The Ultramicro-powder 10g of embodiment 1~5 and comparative example 1~5 is weighed respectively, is added the distilled water that 20mL temperature is 80 DEG C, is seen
Examine appearance luster recover to the bighead atractylodes rhizome fresh goods similar time used, the results are shown in Table 3.
The rehydration implementations of table 3.
As can be seen from Table 3, the rehydration of embodiment 1~5 and comparative example 1 is more preferable, and adjusts starch and dodecyl sulphate
The feeding mode of sodium or correlation step is omitted, rehydration variation can be directly resulted in.Illustrate starch and lauryl sodium sulfate
Add the rehydration that ensure that product.
Although the above-mentioned embodiment to the present invention is described, not to the limit of the scope of the present invention
System, on the basis of technical scheme, it is each that those skilled in the art need not pay that creative work can make
Plant modification or deform still within protection scope of the present invention.
Claims (7)
1. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder, it is characterised in that including step：
（1）Drained after the fresh bighead atractylodes rhizome is cleaned, be put into liquid nitrogen and freeze 8~13 minutes；
（2）By the bighead atractylodes rhizome after freezing in refrigeration grinding machine freeze grinding 30~40 minutes, obtain fresh powder；
（3）Fresh powder is placed in vacuum freeze drier, temperature is down to -40~-50 DEG C, then it is evacuated to 15~
20Pa, then temperature rise to 20~30 DEG C, continue to handle 5~6 hours under current vacuum degree condition, obtain the first powder agglomates；
（4）By the first powder agglomates, soak at room temperature 2~3 hours, addition starch, mixing mashing in distilled water, add dodecyl sulphur
Sour sodium is fully mixed, and then gained mixed material is freeze-dried 10~15 hours in -40~-50 DEG C, the second powder agglomates is obtained；
（5）Second powder agglomates is broken into Ultramicro-powder by micronizer；
Wherein, the mass ratio of the first powder agglomates, starch, distilled water and lauryl sodium sulfate is 1：0.1~0.2：1~1.2：0.3
~0.4.
2. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 1, it is characterised in that step（2）In freezing
Grinder is using Liquid nitrogen precooler 5~10 minutes using preceding.
3. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 1, it is characterised in that step（2）In, at interval of
Again add liquid nitrogen within 4~6 minutes, the bighead atractylodes rhizome is kept liquid nitrogen moisture state all the time.
4. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 1, it is characterised in that step（4）Middle freezing is dry
Pre-freeze is first carried out before dry, is that mixed material is frozen into solid under the conditions of -10~-18 DEG C, and maintain the state 2~3 small
When.
5. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 1, it is characterised in that step（5）In ultra micro
Pulverizer is airslide disintegrating mill.
6. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 5, it is characterised in that the work of airslide disintegrating mill
Condition is：Stream pressure is 1100kPa, and charging rate is 180r/min, and grade frequency is 35Hz, and grinding time is 60~80 points
Clock.
7. a kind of preparation technology of bighead atractylodes rhizome Ultramicro-powder according to claim 1, it is characterised in that step（5）Middle control is super
Grain size of micropowder more than 95% reaches less than 10 μm.
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| CN109549963A (en) * | 2019-01-15 | 2019-04-02 | 长沙秋点兵信息科技有限公司 | A kind of production method of the prepared slices of Chinese crude drugs |
| CN112007110A (en) * | 2020-08-04 | 2020-12-01 | 安徽天安生物科技股份有限公司 | Process for processing gastrointestinal viable micro powder |
| CN115501262A (en) * | 2022-11-10 | 2022-12-23 | 安顺市宝林科技中药饮片有限公司 | Preparation method of bighead atractylodes rhizome ultrafine powder granular decoction pieces |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108186823A (en) * | 2018-02-05 | 2018-06-22 | 浙江中医药大学 | A kind of pharmaceutical composition for being used to treat nephrotic syndrome |
| CN108186823B (en) * | 2018-02-05 | 2021-04-06 | 浙江中医药大学 | Pharmaceutical composition for treating nephrotic syndrome |
| CN109549963A (en) * | 2019-01-15 | 2019-04-02 | 长沙秋点兵信息科技有限公司 | A kind of production method of the prepared slices of Chinese crude drugs |
| CN112007110A (en) * | 2020-08-04 | 2020-12-01 | 安徽天安生物科技股份有限公司 | Process for processing gastrointestinal viable micro powder |
| CN115501262A (en) * | 2022-11-10 | 2022-12-23 | 安顺市宝林科技中药饮片有限公司 | Preparation method of bighead atractylodes rhizome ultrafine powder granular decoction pieces |
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