CN111481953A - Production method of starch-containing Chinese medicinal spray-dried powder - Google Patents

Production method of starch-containing Chinese medicinal spray-dried powder Download PDF

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Publication number
CN111481953A
CN111481953A CN202010311420.7A CN202010311420A CN111481953A CN 111481953 A CN111481953 A CN 111481953A CN 202010311420 A CN202010311420 A CN 202010311420A CN 111481953 A CN111481953 A CN 111481953A
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China
Prior art keywords
spray
starch
dried powder
chinese medicine
traditional chinese
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Inventor
曾昭君
严玉晶
林伟雄
刘燎原
梁志毅
程学仁
魏梅
孙冬梅
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Guangdong Yifang Pharmaceutical Co Ltd
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Guangdong Yifang Pharmaceutical Co Ltd
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Priority to CN202010311420.7A priority Critical patent/CN111481953A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/16Evaporating by spraying
    • B01D1/18Evaporating by spraying to obtain dry solids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/06Fungi, e.g. yeasts
    • A61K36/07Basidiomycota, e.g. Cryptococcus
    • A61K36/076Poria
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
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    • A61K36/894Dioscoreaceae (Yam family)
    • A61K36/8945Dioscorea, e.g. yam, Chinese yam or water yam
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8966Fritillaria, e.g. checker lily or mission bells
    • AHUMAN NECESSITIES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • A61K36/8967Lilium, e.g. tiger lily or Easter lily
    • AHUMAN NECESSITIES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/899Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/899Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
    • A61K36/8994Coix (Job's tears)
    • AHUMAN NECESSITIES
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/899Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
    • A61K36/8998Hordeum (barley)
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    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/906Zingiberaceae (Ginger family)
    • A61K36/9066Curcuma, e.g. common turmeric, East Indian arrowroot or mango ginger
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    • A61K9/146Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids

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Abstract

The invention relates to a production method of a starch-containing traditional Chinese medicine spray-dried powder, which comprises the following steps: firstly, obtaining concentrated clear paste of traditional Chinese medicine materials; secondly, carrying out colloid grinding on the concentrated clear paste; and thirdly, adding auxiliary materials into the product obtained by grinding, mixing and spray drying. The invention carries out colloid grinding treatment on the concentrated clear paste of the traditional Chinese medicine, and then carries out spray drying powder preparation on the ground product, thereby effectively relieving the wall sticking phenomenon of a spray drying tower; in addition, the inventor unexpectedly discovers that when the production method is adopted to prepare the traditional Chinese medicine spray-dried powder, the obtained traditional Chinese medicine spray-dried powder is easy to form and granulate when the parameters of colloid grinding are controlled in a specific range, the obtained granules are not easy to crack, the dissolubility is better, and the clarity of the solution obtained after dissolution is obviously improved.

Description

Production method of starch-containing Chinese medicinal spray-dried powder
Technical Field
The invention belongs to the technical field of traditional Chinese medicine preparation, and particularly relates to a production method of a starch-containing traditional Chinese medicine spray-dried powder.
Background
The traditional Chinese medicine formula particle is prepared by carrying out water extraction, concentration, drying and granulation on single traditional Chinese medicine decoction pieces, is taken by a patient after being prepared according to a traditional Chinese medicine clinical formula, and is a supplement for the traditional Chinese medicine decoction pieces. The Chinese medicinal spray-dried powder is an intermediate of the Chinese medicinal formula granule, and is closely related to the quality of the Chinese medicinal formula granule product.
The traditional preparation process of the traditional Chinese medicine spray-dried powder comprises the following steps: preparing water extract of traditional Chinese medicinal materials, homogenizing, sterilizing, concentrating, and spray drying to obtain traditional Chinese medicine spray dried powder. That is, the traditional technology is to prepare the Chinese medicine spray dry powder by adopting a mode of homogenizing, concentrating and spraying.
Many Chinese medicinal materials contain starch, sugar, mucilage, protein and other components, and correspondingly, the Chinese medicinal material extract also contains starch, sugar, mucilage, protein and other components, wherein the starch is generally insoluble in cold water and is easy to form suspension. When the starch suspension is heated to a certain temperature, the starch grains begin to irreversibly and violently expand, the amylopectin layer on the periphery of the starch grains is swelled, the starch suspension gradually becomes high-viscosity paste, amylose molecules in the starch are dissociated, sol is formed in the paste, the suspension becomes viscous, after the starch suspension is kept stand for a certain time at a low temperature, the solution becomes turbid, the solubility is reduced, precipitates are separated out, and the precipitates can form hard blocks and can not be dissolved any more. Based on the situation, when the traditional preparation process is adopted to prepare the traditional Chinese medicine spray-drying powder, the sprayed powder is particularly easy to stick on the inner wall of the spray-drying tower.
Disclosure of Invention
Based on the above, the main purpose of the invention is to provide a production method of the starch-containing traditional Chinese medicine spray-drying powder, which can effectively relieve the phenomenon that the spray-drying powder is adhered to the inner wall of a spray-drying tower during spray drying.
The purpose of the invention is mainly realized by the following technical scheme:
a production method of a starch-containing traditional Chinese medicine spray-dried powder comprises the following steps:
firstly, obtaining concentrated clear paste of traditional Chinese medicine materials;
secondly, carrying out colloid grinding on the concentrated clear paste;
and thirdly, adding auxiliary materials into the product obtained by grinding, mixing and spray drying.
In one embodiment, the colloid milling parameter setting comprises: the gap between the stator and the rotor is 5-50 μm, and the flow rate is 1000-10000 g/min.
In one embodiment, the inlet air temperature of the spray drying is 160-200 ℃, and the outlet air temperature of the spray drying is 80-105 ℃.
In one embodiment, the excipient is selected from at least one of dextrin, starch, and lactose.
In one embodiment, 0.0-5.5 kg of the auxiliary materials are added into each 100kg of the traditional Chinese medicinal materials.
In one embodiment, the relative density of the concentrated clear paste is 1.01-1.20.
In one embodiment, the preparation of the concentrated fluid extract comprises:
firstly, preparing traditional Chinese medicine decoction pieces, adding water for decoction, and filtering to obtain an extracting solution;
and (II) concentrating and filtering the extracting solution.
In one embodiment, the concentration is carried out under the conditions of-94 KPa to-43 KPa and 40 ℃ to 85 ℃.
In one embodiment, the mass of the water is 10-20 times of the mass of the traditional Chinese medicine decoction pieces, the decocting times are 1-3 times, and each time of decocting is 0.5-2.0 hours.
In one embodiment, the preparation of the herbal pieces-comprises: obtaining the traditional Chinese medicine materials and removing impurities.
In one embodiment, the starch content of the traditional Chinese medicine is 45.0% -95.0%.
In one embodiment, the Chinese herbal medicine is at least one selected from coix seed, poria cocos, white peony root, angelica dahurica, lily, light wheat, radix glehniae, pinellia ternate, radix curcumae, phaseolus calcaratus, dioscorea nipponica, curcuma zedoary, radix stephaniae tetrandrae, radix puerariae, rhizoma zingiberis, curcuma longa, mung bean, lotus seed, malt, moutan bark, semen euryales, trichosanthes root, aconite, rhizoma alismatis, bulbus fritillariae cirrhosae, Chinese yam and thunberg fritillar.
The invention has the following beneficial effects:
the invention carries out colloid grinding treatment on the concentrated clear paste of the traditional Chinese medicine, and then carries out spray drying on the ground product, and the phenomenon that a large amount of the obtained traditional Chinese medicine spray drying powder is adhered to the inner wall of a spray drying tower can not occur in the drying process. Further, the inventors surprisingly found that when the production method is used for preparing the traditional Chinese medicine spray-dried powder, the parameters of colloid grinding are controlled within a specific range, the obtained traditional Chinese medicine spray-dried powder is easy to form and granulate, the obtained granules are not easy to break, the dissolubility is good, and the clarity of the solution obtained after dissolution is obviously improved.
Drawings
FIG. 1 is a comparison of the paste yield and the spray drying powder yield of the example and the comparative example of coix seed spray drying powder;
FIG. 2 is a comparison of spray drying yields of example and comparative example of Coicis semen spray drying powder;
FIG. 3 is a comparison of extract transfer rates of Coicis semen spray-dried powder example and comparative example.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The embodiment of the invention provides a production method of a starch-containing traditional Chinese medicine spray-dried powder, which comprises the following steps:
firstly, obtaining concentrated clear paste of traditional Chinese medicine materials;
secondly, carrying out colloid grinding on the concentrated clear paste;
and thirdly, adding auxiliary materials into the product obtained by grinding, mixing and spray drying.
The embodiment of the invention carries out colloid grinding treatment on the concentrated clear paste of the traditional Chinese medicinal materials, and then carries out spray drying powder preparation on the ground product, and the phenomenon that the spray drying powder is adhered to the inner wall of a spray drying tower can be effectively relieved in the powder preparation. And moreover, the problems of nozzle blockage, spray dry powder agglomeration, excessive moisture and scorching can be effectively solved. In addition, the inventor unexpectedly discovers that when the production method is adopted to prepare the traditional Chinese medicine spray-dried powder, the obtained traditional Chinese medicine spray-dried powder is easy to form and granulate when the parameters of colloid grinding are controlled in a specific range, the obtained granules are not easy to crack, the dissolubility is better, and the clarity of the solution obtained after dissolution is obviously improved.
The colloid mill is mainly a colloid mill, the equipment is a machine for providing fine processing for wet materials, and the main machine part of the colloid mill is composed of a shell, a dynamic mill, a static mill, an adjusting mechanism, a cooling mechanism, a motor and the like. The main parts are made of stainless steel, corrosion resistant and nontoxic. The principle is that under the combined action of self weight, centrifugal force and the like, the processed material is subjected to the combined action of strong shearing force, friction force, impact force, high-frequency vibration and the like when passing through the adjustable clearance between the stator and the rotor by the relative motion of rotor grinding teeth and stator grinding teeth with different geometric shapes under high-speed rotation, so as to achieve the purposes of dispersion, crushing, emulsification, homogenization and mixing.
The colloid mill comprises the following operation steps:
1. preparation before starting up: after the equipment parts are sterilized, a stator bracket, an adjusting ring, a dial scale, a cover type screw, a cooling water nozzle, a charging hopper sealing ring and a charging hopper are sequentially installed;
2. starting up: the power supply and the electric switch are switched on, the rotating direction of the motor is clockwise when the motor is seen from the upper part to the lower part, and the whole equipment runs stably without any noise; starting the device, idling the device, holding the adjusting handle with two hands to rotate the adjusting ring (clockwise) in an idling state, adjusting the jacking position of the fiber screw, and feeding and trying to grind;
3. adjusting: observing whether the discharging condition meets the requirement, if not, adjusting the clearance between the stator and the rotor, wherein the adjustment needs to be performed in the running state, the adjustment clearance range is 5-50 mu m, the smaller the rotating clearance is, the finer the discharging granularity is, the larger the rotating clearance is, the larger the discharging granularity is, and after the discharging condition meets the requirement, the adjustment is stopped;
4. processing: the feeding speed is adjusted according to the property of the concentrated clear paste, the flow is controlled to be 1000-10000 g/min, the grinding is carried out for 1-3 times, the situation that the materials are stored in a hopper and cannot be fed due to material accumulation is avoided;
5. cleaning: after the use is finished, after the materials in the hopper are completely discharged, the receiving barrel is moved away, the empty barrel is replaced, purified water is added into the hopper, and the purified water is discharged from the discharge port to be clean water;
6. stopping the machine: and the adjusting handle is held by both hands to rotate the adjusting ring for a circle anticlockwise, so that the grinding tooth gap is separated, the switch is turned off, and the power supply is switched off.
Preferably, the parameter setting of the grinding comprises: the gap between the stator and the rotor is 5-50 μm, and the flow rate is 1000-10000 g/min. Through parameter setting, the particle size of the clear paste is controlled within a certain range, the clear pastes are mixed evenly, and after the spray drying, the obtained spray dried powder is more exquisite and even, the quality of the spray dried powder is improved, and the smooth proceeding of the subsequent process is facilitated.
When the colloid mill is adopted for grinding, the concentrated clear paste is refined under the combined action of shearing force, friction force, impact force, high-frequency vibration and other composite forces of the colloid mill, and the problems of layering, material precipitation, precipitation and the like of the starch-containing concentrated clear paste during standing are solved, so that the clear pastes can be mixed with one another more uniformly, and the whole product system is more stable; the concentrated clear paste is ground, homogenized and then spray-dried, so that the wall sticking of a spray-drying tower can be effectively relieved, the technical problems of blockage of a spray head of an atomizer, caking of spray-dried powder, even scorching and the like can be effectively solved, the normal operation of production is maintained, the production efficiency is improved, and the material utilization rate and the product yield are improved. The production method is simple and convenient, easy to operate, low in production cost and suitable for industrial production and application.
It will be appreciated that the number of grindings is not limited and that the concentrated fluid extract may be ground any number of times in order to achieve the desired effect. In consideration of the polishing effect and the production efficiency, the number of times of polishing is preferably 1 to 3, for example, 1, 2, or 3 times. The product obtained by grinding, which can also be called homogeneous clear paste, is stored in a storage tank for later use.
Preferably, the air inlet temperature of the spray drying is 160-200 ℃, and the air outlet temperature of the spray drying is 80-105 ℃. In the above-mentioned air inlet temperature and air outlet temperature range, the fluctuation of temperature value can appear. Conditions for spray drying are, for example: the air inlet temperature is 160 ℃, the air outlet temperature is 80 ℃, the air inlet temperature is 180 ℃, the air outlet temperature is 90 ℃, the air inlet temperature is 200 ℃, the air outlet temperature is 105 ℃ and the like.
Preferably, the auxiliary material is at least one selected from dextrin, starch and lactose, wherein the dextrin includes but is not limited to maltodextrin and β -cyclodextrin.
Preferably, 0.0-5.5 kg of the auxiliary materials are added into each 100kg of the traditional Chinese medicinal materials, such as: 0.4kg, 3.8kg, 4.5kg, 5.0kg, 5.1kg, and 5.4 kg.
Preferably, the relative density of the concentrated clear paste is 1.01-1.20.
It can be understood that the smaller the relative density of the concentrated clear paste is, the larger the amount of the obtained clear paste is, and the longer the spray drying time is, which is not beneficial to the circulation of materials in the production process and can increase the energy consumption; the relative density of the concentrated clear paste is too high, the viscosity of the obtained clear paste is higher, the fluidity is poorer, the effective components are easy to separate out, and the material loss in the circulation process is larger.
It can be understood that the preparation method of the concentrated clear paste is not limited, and any preparation process of the concentrated clear paste can be used. Preferably, the preparation of the concentrated clear paste comprises:
firstly, preparing traditional Chinese medicine decoction pieces, adding water for decoction, and filtering to obtain an extracting solution;
and (II) concentrating and filtering the extracting solution.
After the extracting solution is obtained in the step (one), taking a proper amount of extracting solution, stirring uniformly, precisely absorbing 25m L of the extracting solution, placing the extracting solution in an evaporating dish with constant weight, drying the extracting solution by distillation on a water bath, drying the extracting solution for 3h at 105 ℃, cooling the extracting solution in a dryer for 30min, rapidly and precisely weighing the extracting solution, and calculating the cream yield of the extracting solution.
After the filtration in the step (two), taking a proper amount of the clear paste obtained by filtration, stirring uniformly, precisely weighing 5g of the clear paste, placing the clear paste in an evaporation dish with constant weight, drying the clear paste by distillation on a water bath, drying the dry paste for 3h at 105 ℃, cooling the dry paste in a dryer for 30min, rapidly and precisely weighing the weight, and calculating the paste yield of the clear paste.
Preferably, the concentration is carried out under the conditions of-94 KPa to-43 KPa and 40 ℃ to 85 ℃.
Preferably, the mass of the water is 10-20 times of that of the traditional Chinese medicine decoction pieces, the decocting times are 1-3 times, and each time of decocting is 0.5-2.0 hours. For example, the weight of water is 10 times, 15 times and 20 times of the weight of the traditional Chinese medicine decoction pieces, and the decoction time is 0.5h, 1h, 1.5h and 2 h. During decoction, the water adding amount is too small, the decoction time is too short, and the transfer of effective components is incomplete; the water adding amount is too much, the decocting time is too long, the energy consumption is increased, the concentration time of the extracting solution is correspondingly prolonged, and the circulation of materials in the production process is not facilitated.
Preferably, the preparation of the traditional Chinese medicine decoction pieces comprises the following steps: obtaining the traditional Chinese medicine materials and removing impurities. It is understood that the subsequent corresponding treatment, such as crushing after removing impurities, can be further performed according to the production specification. The medicinal materials are selected and cleaned after impurities are removed, and the preparation is specified under the processing items of medicinal material decoction pieces in the first edition of the pharmacopoeia of the people's republic of China 2015. The size of the decoction piece particle size can affect whether the effective components can be fully dissolved. The particle size of the decoction pieces is too large, so that the effective components are not easy to dissolve out, and the product quality is influenced; similarly, the particle size of the decoction pieces is too small, so that the dissolution of active ingredients is increased, the dissolution of starch, protein and other substances contained in the traditional Chinese medicine is also increased, the viscosity of the extracting solution is increased, and the circulation of materials in the production process is influenced.
Preferably, the starch content of the traditional Chinese medicine is 45.0-95.0%. Preferably, including but not limited to the following categories: poria cocos, coix seeds, white paeony roots, angelica dahurica, lily, light wheat, radix glehniae, pinellia ternate, radix curcumae, phaseolus calcaratus, dioscorea nipponica, curcuma zedoary, radix stephaniae tetrandrae, radix puerariae, rhizoma zingiberis, curcuma longa, mung beans, lotus seeds, malt, moutan barks, gordon euryale seeds, radices trichosanthis, aconite, rhizoma alismatis, bulbus fritillariae cirrhosae, Chinese yams, thun.
The present invention will be further illustrated by the following specific embodiments, which are not intended to limit the scope of the present invention.
Example 1:
a production method of a traditional Chinese medicine spray-dried powder comprises the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding for 1 time at a flow rate of 1000g/min with a gap of 5 μm between stator and rotor to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Example 2:
a production method of a traditional Chinese medicine spray-dried powder comprises the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 1.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding for 2 times at a flow rate of 5000g/min with a gap of 25 μm between stator and rotor to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Example 3:
a production method of a traditional Chinese medicine spray-dried powder comprises the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 2.0 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding 3 times with stator and rotor gap of 50 μm and flow rate of 10000g/min to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Example 4:
a production method of a traditional Chinese medicine spray-dried powder comprises the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 15 times of water according to the amount of the material, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding for 1 time at a flow rate of 10000g/min with a stator-rotor clearance of 50 μm to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Example 5:
a production method of a traditional Chinese medicine spray-dried powder comprises the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 20 times of water according to the amount of the material, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding for 1 time at a flow rate of 10000g/min with a stator-rotor clearance of 50 μm to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Example 6:
the embodiment is a variation of embodiment 1, and the main variation of the embodiment 1 includes different parameter settings of the colloid mill, and specifically, the method for producing the traditional Chinese medicine spray-dried powder of the embodiment includes the following steps:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a colloid mill, wherein the technological parameters are as follows: grinding for 1 time at a flow rate of 500g/min with a gap of 1 μm between stator and rotor to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Comparative example 1: adopting clear paste without grinding
a. Pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. spray drying: taking the coix seed clear paste, adding a proper amount of maltodextrin to dissolve the coix seed clear paste, uniformly stirring, and drying by adopting a spray drying mode, wherein the technological parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Comparative example 2: adopting clear paste without grinding
a. Selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, stirring, decocting for 0.5 hr, and filtering to obtain Coicis semen extract;
c. vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. taking the coix seed clear paste, adding a proper amount of maltodextrin to dissolve the coix seed clear paste, uniformly stirring, and drying by adopting a spray drying mode, wherein the technological parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder.
Comparative example 3: homogenizing with a high-pressure homogenizer
This comparative example is a comparative example to example 1, the main differences with respect to example 1 including: homogenizing with a high-pressure homogenizer without colloid milling, specifically, the steps of the present comparative example include:
a. pretreatment: selecting Coicis semen, removing impurities, and crushing to obtain Coicis semen decoction pieces;
b. extraction: adding Coicis semen decoction pieces into an extraction tank, adding 10 times of water according to the amount of the raw materials, decocting for 0.5 hr without stirring, and filtering to obtain Coicis semen extract;
c. concentration: vacuum concentrating the coix seed extracting solution at 40-85 ℃ until the relative density is 1.01-1.20, and filtering to obtain coix seed concentrated clear paste;
d. homogenizing: adding the coix seed clear paste into a high-pressure homogenizer for homogenization, wherein the technological parameters are as follows: working pressure of 40Mpa, flow rate of 1000g/min, controlling particle size of the obtained fluid extract to 5 μm to obtain homogeneous fluid extract;
e. spray drying: taking the homogeneous clear paste, adding a proper amount of maltodextrin to dissolve and uniformly stirring, and drying by adopting a spray drying mode, wherein the process parameters are as follows: controlling the inlet air temperature to be 160-200 ℃ and the outlet air temperature to be 80-105 ℃, and collecting the spray dry powder. a. The steps b, c and e are the same as in example 1.
The coix seed spray-dried powder prepared in the examples and the comparative examples is measured for the extract content, and the cream yield and the transfer rate are calculated, and the results are shown in table 1:
TABLE 1 example Process parameters for preparing Coicis semen spray-dried powder and related results
Figure BDA0002457984090000131
TABLE 2 comparative examples Process parameters for preparing Coicis semen spray-dried powder and related results
Figure BDA0002457984090000141
In the table:
① extracting, concentrating to obtain dry extract (dry extract/feed amount) 100%;
②, the sprayed dry pure cream yield (weight of the sprayed dry powder-added auxiliary material amount)/the feeding amount is 100%;
③ spray dry powder yield (%) -. spray dry powder weight/batch size 100%;
④ spray drying yield (%). spray drying powder weight/(batch feed rate. concentrated paste yield + malt paste precision). 100%;
⑤ extract transfer rate (%) (amount of spray dried powder extract) ((1-spray dried powder moisture))/[ amount of charge: (1-decoction pieces moisture) ]/(100%);
⑦ decoction piece extract (%) - (decoction piece alcohol soluble extract amount/continuous filtrate volume diluted volume)/[ decoction piece sample amount (1-decoction piece water) ]/100%;
⑧ spray dry powder extract (%) (spray dry powder alcohol soluble extract dry paste volume/continuous filtrate volume diluted volume)/[ spray dry powder sample volume (1-spray dry powder moisture) ]. 100%;
⑨ spray-dried tails are specifically the sum of the amount of spray-dried powder that cannot pass through an 80 mesh screen.
As can be seen from the comparison of the results of the example 1 and the comparative example 1, the invention adopts the clear paste grinding technology to compare with the clear paste non-grinding technology, the yield of the spray-drying powder, the spray-drying yield and the extract transfer rate of the spray-drying process of the example 1 are all higher than those of the comparative example 1, and the spray-drying process of the example 1 only slightly adheres to the tower wall of the spray-drying tower, while the spray-drying tower wall, the sight glass and the blowing rod of the comparative example 1 all adhere to the machine, and the tail material is more after the spray-drying powder is sieved, namely the invention adopts the clear paste grinding technology to.
As can be seen from the comparison of the results of example 1 and comparative example 2, whether stirring is started or not has a great influence on the extraction rate of the extract liquid during the heating and decocting process of the extraction tank; by adopting a clear paste grinding method, the loss in the spray drying process is reduced, and the yield of the spray-dried powder, the spray-dried yield and the extract yield of the spray-dried powder are improved, namely the result of the example 1 is superior to that of the comparative example 2.
The results of the examples 2 to 5 show that the loss of the materials in the spray drying process is obviously reduced by a clear paste colloid grinding method; the water adding amount for extraction is 10-20 times, the heating and decocting time is 0.5-2.0 hours, the gap between a stator and a rotor of a colloid mill is 5-50 mu m, the flow rate of the clear paste is 1000-10000 g/min, and on the premise of ensuring the paste yield of the extracting solution, the obtained spray-dried powder is finer and more uniform by a clear paste grinding method, and the whole product system is more stable.
In addition, the characteristics related to granulation of the Chinese medicinal spray-dried powders obtained in examples 1 and 6 and the melting property of the obtained granules were also examined, specifically, the Chinese medicinal spray-dried powders obtained in examples 1 and 6 were respectively granulated under the same granulation conditions, and then the primary molding rate, hardness, solubility and turbidity values of the obtained granules were measured. The determination method comprises the following steps:
① measurement of forming rate, passing the prepared granule sample through a first sieve and a fifth sieve in turn, collecting the granule sample which can pass through the first sieve but can not pass through the fifth sieve, and weighing the granule sample to obtain a fixed mass, wherein the forming rate (%) -the mass of the granule sample which passes through the first sieve but can not pass through the fifth sieve/the total mass of the granule sample is × 100%;
② hardness determination, weighing the prepared granule sample, about 20g, placing into a plastic bag with a sticky port, locking the bag opening to ensure air in the bag, shaking for 3min in the vertical direction, placing into a 50 mesh screen (with a closed receiving container under the screen), covering on the screen, rotating and shaking for at least 2min in the horizontal direction, tapping the screen in the vertical direction at times, taking the granule sample and powder under the screen, weighing, and calculating the proportion (%);
③ solubility determination, wherein 2 parts of the prepared granule sample, 10g each, are heated with 200m L of water and stirred for 5min, and the soluble granules should be completely dissolved or slightly turbid, but no obvious visible foreign matter is detected;
④ turbidity value determination, 2 parts of prepared particle sample, 10g each, adding 200m L of hot water, stirring for 5min, and determining turbidity value (when the turbidity value of the sample solution is lower than 35NTU value, the particles are all dissolved, the light transmittance of the turbidity value is between 35NTU and 190NTU, and the turbidity degree is increased along with the increase of the value).
The detection results are as follows:
TABLE 3
Figure BDA0002457984090000161
Figure BDA0002457984090000171
As can be seen from table 3, when the spray dried powder of the chinese medicine of example 1 was granulated, the one-shot forming ratio was relatively high and the hardness was relatively low, compared to the spray dried powder of the chinese medicine of example 6, and the obtained granules were better in solubility when they were melted. This indicates that it is important to use the appropriate colloid milling parameters.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (12)

1. The production method of the starch-containing traditional Chinese medicine spray-dried powder is characterized by comprising the following steps:
firstly, obtaining concentrated clear paste of traditional Chinese medicine materials;
secondly, carrying out colloid grinding on the concentrated clear paste;
and thirdly, adding auxiliary materials into the product obtained by grinding, mixing and spray drying.
2. The method for producing starch-containing Chinese medicinal spray-dried powder according to claim 1, wherein the colloid milling parameters include: the gap between the stator and the rotor is 5-50 μm, and the flow rate is 1000-10000 g/min.
3. The production method of the starch-containing traditional Chinese medicine spray-dried powder according to claim 1 or 2, wherein the air inlet temperature of the spray drying is 160-200 ℃, and the air outlet temperature of the spray drying is 80-105 ℃.
4. The method for producing the starch-containing Chinese medicinal spray-dried powder according to claim 1 or 2, wherein the adjuvant is at least one selected from dextrin, starch and lactose.
5. The production method of the starch-containing traditional Chinese medicine spray-dried powder according to claim 1 or 2, characterized in that 0.0-5.5 kg of the auxiliary material is added to every 100kg of the traditional Chinese medicine.
6. The production method of the starch-containing traditional Chinese medicine spray-dried powder according to claim 1 or 2, wherein the relative density of the concentrated clear paste is 1.01-1.20.
7. The production method of the starch-containing Chinese medicinal spray-dried powder according to claim 1 or 2, wherein the preparation of the concentrated fluid extract comprises:
firstly, preparing traditional Chinese medicine decoction pieces, adding water for decoction, and filtering to obtain an extracting solution;
and (II) concentrating and filtering the extracting solution.
8. The method for producing the starch-containing Chinese medicinal spray-dried powder according to claim 7, wherein the concentration is carried out under the conditions of-94 to-43 KPa and 40 to 85 ℃.
9. The method for producing the starch-containing Chinese medicinal spray-dried powder as claimed in claim 7, wherein the mass of the water is 10-20 times of the mass of the Chinese medicinal decoction pieces, and the decoction is carried out for 1-3 times, and each time for 0.5-2.0 h.
10. The method for producing the starch-containing Chinese medicinal spray-dried powder as claimed in claim 7, wherein the preparation of the Chinese medicinal decoction pieces comprises: obtaining the traditional Chinese medicine materials and removing impurities.
11. The method for producing the starch-containing Chinese medicinal spray-dried powder according to any one of claims 1, 2 and 8 to 10, wherein the starch content of the Chinese medicinal materials is 45.0 to 95.0 percent.
12. The method for producing starch-containing dried Chinese medicinal powder according to any one of claims 1, 2 and 8 to 10, wherein the Chinese medicinal materials are at least one selected from coix seed, poria cocos, white peony root, dahurian angelica root, lily bulb, light wheat, glehnia root, pinellia tuber, curcuma aromatica, phaseolus calcaratus, dioscorea nipponica, curcuma zedoary, tetrandra root, kudzu vine root, dried ginger, curcuma longa, mung bean, lotus seed, malt, moutan bark, gorgon fruit, trichosanthes root, aconite root, alisma orientale, fritillaria cirrhosa, yam and thunberg fritillary bulb.
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JPH0789852A (en) * 1993-09-20 1995-04-04 Fujitsukusu Kk Water-soluble powder containing calcium in high concentration and its production
EP1998736A2 (en) * 2006-03-29 2008-12-10 Wm. Wrigley Jr. Company, Et Al. Breath freshening and oral cleansing products with synergistic combinations of magnolia bark extract and essential oils
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