CN102727735B - Xuanmai Ganjie puffed particulate granules and preparation method thereof - Google Patents
Xuanmai Ganjie puffed particulate granules and preparation method thereof Download PDFInfo
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- CN102727735B CN102727735B CN201110088361.2A CN201110088361A CN102727735B CN 102727735 B CN102727735 B CN 102727735B CN 201110088361 A CN201110088361 A CN 201110088361A CN 102727735 B CN102727735 B CN 102727735B
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Abstract
The invention belongs to the medicine field, particularly to Xuanmai Ganjie puffed granules and a preparation method thereof. The invention provides Xuanmai Ganjie puffed granules with good flowing characteristics and a ball-like shape. The extraction or decocting technology can be performed according to the present method during the granulating process. The main difference between the method in the invention and the present method is making the granules in a compressed state. In the process of drying the granules, the moisture of the granules is controlled at 4-5 percent, then the granules are heated at high temperature to become puffed and the finished products of the granules are obtained by drying the puffed granules. The preparation method of the invention can form ball-like granules with smooth surfaces and compact texture. The interiors of the granules have a phenomenon of cavitation expansion which enables the granules to have good shape and not-easily-broken property, An angle of repose of a granule is between 10 degree to 25 degree. The granules prepared by the method have characteristics that the granules have good fluidity, do not easily absorb moisture and require less auxiliary material. Besides, the paste material is hard to appear when the granules are mixed with water, so that the mixing is very easy. The Xuanmai Ganjie puffed granules of the invention can be used as a raw material for preparing tablets and capsules according to the ordinary technology of compressing tablets and stuffing capsules.
Description
Technical field
The invention belongs to field of medicaments, be specifically related to Xuanmai Ganju swelling granular agent and preparation method thereof.
Background technology
At present, for the ease of application Chinese medicine, common mode is granule by dosage form common herbal mixture, tablet, and capsules etc., also have and will after single medicinal material extraction, make granule.Xuanmai Ganju grains has heat clearing away YIN nourishing, effect of dispelling phlegm and relieving sore-throat.Be applicable to hyperactivity of fire caused by deficiency of YIN, mouth and nose are dry, the diseases such as laryngopharynx swelling and pain.
Xuanmai Ganju grains normally crude drug is adopted decoct with water or the organic solvent extraction such as ethanol after obtain extractum, granulate after then adding adjuvant to make soft material, granulate, obtain granule.But the granule of preparing according to existing method need to add a large amount of adjuvants could figurations conventionally, and the shape of granule is generally indefinite form, and granule is loose, broken, and profile is poor, poor fluidity, and easily the moisture absorption, is unfavorable for preserving subpackage and preservation.In order to improve existing method, inventor wants to provide a kind of brand-new Xuanmai Ganju grains agent.
Summary of the invention
Technical problem solved by the invention is to provide a kind of smooth-shaped densification, good fluidity, the Xuanmai Ganju swelling granular agent that class is spherical, its extraction or decocting process, when granulation, all can carry out with reference to existing method, main difference is: (1) makes the granule of compressive state; (2) when dried particles, adopting first low temperature control to moisture is 4-5%, then heated particle makes it expanded under hot conditions, dry.
Xuanmai Ganju swelling granular of the present invention agent is prepared and obtained by following method:
A, take the crude drug of following weight proportioning: Radix Scrophulariae 300-500 part, Radix Ophiopogonis 300-500 part, Radix Glycyrrhizae 300-500 part, Radix Platycodonis 300-500 part, adopt conventional method to be prepared into extractum;
B, extractum is made after soft material, granulated, granulate is to crossing 14-24 mesh sieve;
C, dried particles;
The improvements of Xuanmai Ganju swelling granular agent preparation method of the present invention are:
1, step B prepares bulk density and is greater than 0.78g/cm
3granule.Inventor will " bulk density be greater than 0.78g/cm
3granule " be called " granule of compressive state ", the granular pile density of this compressive state is at least greater than 0.78g/cm
3, with this understanding, just can carry out second committed step of the present invention, realize expanded object; The present invention prepares gained " granule of compressive state " bulk density and is generally 0.78-0.90g/cm
3.
2, step C dried particles is to adopt following method:
(1) first under the cryogenic conditions of 40-60 ℃ dried particles to water content 4-5%;
(2) then under the hot conditions of 65-95 ℃, be heated to granule expanded;
(3) maintain again the hot conditions of 65-95 ℃, below dried particles moisture to 2%, obtain granule.
Coordinate above-mentioned technique, make soft material after extractum need being made to dry extract when extractum is made to soft material again, so processing can reduce supplementary product consumption, reduces and takes in unnecessary adjuvant, reduces production costs.
Committed step of the present invention is first to adopt compressing grains machine to make the granule of compressive state, again in the processing mode of low temperature-high temperature, make granule at drying stage, especially there is the phenomenon (expanded) expanding in granule when high-temperature process, make to form the spherical or spherical particle of smooth in appearance densification, granule interior has the expanded phenomenon of cavity, and granule is not fragmentary, and profile is good; Granule scope angle of repose is 10-25 °, and good fluidity, is difficult for the moisture absorption; Supplementary product consumption is few; While brewing, at the bottom of cup, be not prone to pasty masses, easily brew.Xuanmai Ganju grains agent of the present invention can also be as the raw material of preparing tablet or capsule, technique tabletting or encapsulated routinely.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of compressing grains machine of the present invention.
Fig. 2 is the front view of the poly-charging tray of the present invention.
Fig. 3 is the left view of Fig. 2.
Fig. 4 is the front view of splitter section of the present invention.
Fig. 5 is the rearview of Fig. 4.
Fig. 6 is the A-A profile of Fig. 5.
Fig. 7 is the B-B profile of Fig. 5.
Fig. 8 is the front view of extrusion die of the present invention.
Fig. 9 is the left view of Fig. 8.
Figure 10 is the structure chart of existing Screw Extrusion pay-off screw rod.
Figure 11 is the schematic diagram of cooled screw structure of the present invention.
Figure 12 is the front view of peeling knife of the present invention.
Figure 13 is the top view of Figure 12.
In figure, be labeled as, 1-head, 2-discharge barrel, 3-extrusion die, 4-gathers charging tray, 5-by-passing parts, 6-peeling knife, 7-screw rod, 8-dynamical system, 9-rotary-cut system, 10-water collar, 30-discharge opening, 31-macropore, 32-aperture, 40-centre bore, 51-splitter box, 52-shunts ridge, 53-blow tank, 54-gathers charging tray bayonet socket, 55-central boss, 56-back-up block, 60-elastic, 61-sword limit, 70-blind hole, 71-inner cool tube, 72-cooling cover, 73-nut, the cooling entrance of 74-, 75-coolant outlet, 76-front end fixed disk, 77-gear shaft part, 78-thread segment, 700-cooling duct, 720-cooling cover inner chamber.
The specific embodiment
Illustrate but do not limit the present invention by specific description of embodiments of the present invention below.
Xuanmai Ganju swelling granular of the present invention adopts following method preparation:
A, take the crude drug of following weight proportioning: Radix Scrophulariae 300-500 part, Radix Ophiopogonis 300-500 part, Radix Glycyrrhizae 300-500 part, Radix Platycodonis 300-500 part, adopt conventional method to be prepared into dry extract;
B, dry extract is made after soft material, granulated, granulate is to crossing 14-24 mesh sieve;
C, dried particles;
It is characterized in that:
Step B makes bulk density and is greater than 0.78g/cm
3granule;
Step C dried particles is to adopt following method:
(1) first under the cryogenic conditions of 40-60 ℃ dried particles to water content 4-5% (w/w);
(2) then under the hot conditions of 65-95 ℃ (preferably 75-95 ℃), be heated to granule expanded;
(3) maintain again the hot conditions of 65-95 ℃ (preferably 75-95 ℃), below dried particles moisture to 2% (w/w), obtain granule.
Wherein, preferred feedstock medicine weight proportion is: 400 parts of Radix Scrophulariaes, 400 parts of Radix Ophiopogonis, 400 parts, Radix Glycyrrhizae, 400 parts of Radix Platycodoniss.
The granular pile density of in the past preparing according to existing method is conventionally at 0.55-0.7g/cm
3even if adopt that first low temperature-drying mode of high temperature also cannot be realized expanded object again.And preparing bulk density in step B, granule of the present invention is greater than 0.78g/cm
3" granule of compressive state ", should " granule of compressive state " bulk density be generally 0.78-0.90g/cm
3, be to realize one of expanded key parameter.
Further, the conventional method that steps A is prepared extractum has, and decocts with water, and collecting decoction, filters, and filtrate leaves standstill, and gets the extractum that supernatant concentration to relative density is 1.32～1.35 (80～85 ℃).When preparation, also find, apply after extract powder made by extractum by preparation method of the present invention and prepare again soft material, can obviously reduce supplementary product consumption, reduce the absorption of unnecessary adjuvant, reduce production costs.
The granule of Xuanmai Ganju swelling granular of the present invention agent is in profile, mobility, and moisture absorption, brews and in complexity, is all better than the Xuanmai Ganju grains prepared than existing methods.
The bulk density of will preparing in preparation method of the present invention is at least greater than 0.78g/cm
3granule, the standby granule of the mechanism of compressing grains below need applying in the time that step B granulates, this compressing grains machine is as Fig. 1～Fig. 9, shown in Figure 11～Figure 13, comprise that the double-screw type in head 1 extrudes pay-off and extrude with this discharge barrel 2 that pay-off coordinates, the exit of discharge barrel 2 arranges the extrusion die 3 that has discharge opening 30, in discharge barrel 2, between twin-screw extrusion pay-off and extrusion die 3, be provided with by-passing parts 5, between twin-screw extrusion pay-off and by-passing parts 5, be provided with and the by-passing parts 5 poly-charging tray 4 with centre bore 40 by touching mutually, the supplied materials side of by-passing parts 5 is evenly equipped with splitter box 51, splitter box 51 converges at the blow tank 53 of by-passing parts exit side, blow tank 53 is corresponding with the discharge opening 30 of extrusion die 3.Double Circle stock column that hollow poly-charging tray 4 of the present invention can be sent twin-screw extrusion pay-off is assembled and is changed over mono-cylindrical water conservancy diversion before by-passing parts 5, be evenly equipped with splitter box 51 as material channel in the supplied materials side of by-passing parts 5, guarantee to assemble the mono-cylindrical material strip forming and can evenly be branched to extrusion die 3, material can evenly be extruded, by its powerful extrusion capability, be generally 0.78-0.90g/cm thereby obtain bulk density
3granule, and even particle size, good looking appearance, obviously improves particle appearance quality.The squeeze pressure scope of compressing grains machine can be floated at 45000N～150000N; in the time of initial feeding; feeding amount adopts relatively little squeeze pressure 45000N-6000N more at least; after entering normality, feeding adopts relatively large pressure 70000N～120000N extruding; if feeding amount is large, also can suitably increase squeeze pressure.
As Fig. 4, Fig. 5, shown in Fig. 6 and Fig. 7, for further improving granular mass, described splitter box 51 is sector diffuence groove, it between adjacent two sector diffuence grooves, is shunting ridge 52, the part that shunting ridge 52 contacts with poly-charging tray as the separation between sector diffuence groove and by-passing parts, play the effect of transmitting extruding force, sector diffuence groove is more shallow near the degree of depth of the part groove at middle part, area is less, extruding force is larger, corresponding material flow is less, and the degree of depth of the part groove of close circumference is darker, area is larger, extruding force is less, be conducive to give full play to the homogenization of by-passing parts, make the material bar linear velocity extruded more consistent, granule is more even.
For taking into account uniformity and easy to process, the number of sector diffuence groove is generally 4-7.
As shown in Figure 5 and Figure 6, for extruding force is delivered to extrusion die 3 uniformly, avoid template 3 local pressures excessive and damage, should be provided with central boss 55 at the center of the exit side of described by-passing parts 5, the surrounding of exit side is provided with back-up block 56, and central boss 55 contacts with surrounding with the center of extrusion die 3 respectively with back-up block 56, blow tank 53 is between central boss 55 and back-up block 56, like this, the suffered pressure ratio of template is more even, also makes material to extrude more equably.
As shown in Figure 4 and Figure 6, for convenience of the location of by-passing parts 5, can be provided with and the poly-charging tray bayonet socket 54 of centre bore 40 adaptations in the supplied materials side of described by-passing parts 5.
As shown in figure 11, in the present invention, the screw rod 7 that double-screw type is extruded pay-off is provided with cooling structure, described cooling structure is included in the blind hole 70 and the inner cool tube 71 that be provided with cooling entrance 74 concentric with screw axis on screw rod 7, offered, inner cool tube 71 stretches in described blind hole 70 through the cooling cover 72 of this blind hole 70 of sealing and its built-in length is less than blind hole 70 degree of depth, cooling cover 72 has the cooling cover inner chamber 720 that is provided with coolant outlet 75, and the cooling duct 700 forming between inner cool tube 71 and blind pore wall is communicated with cooling cover inner chamber 720.This structure can pass into cooling medium and carry out cooling to screw rod 7 in running, cooling medium is entered by cooling entrance 74, flow through after inner cool tube 71 and cooling duct 700, cooling cover inner chamber 720 and flowed out by coolant outlet 75, the material viscosity that can avoid equipment when operation temperature arrising caused by friction and cause increases, the easily problem such as bonding, guarantee normal discharging, for mechanical pelletizing provides precondition, also make equipment can be applicable to the material extrusion granulator that viscosity is large.
For same object, as shown in Figure 1, can, on such scheme basis, extrude the additional water collar 10 of barrel of pay-off etc. at double-screw type, barrel is also lowered the temperature, reach better effect.
As shown in figure 11, described inner cool tube 71 can be fixed on cooling cover 72 by nut 73, described cooling cover 72 is fixedly connected with head 1, nut 73 and cooling cover 72 can be simultaneously as the axial limit structure of screw rod 7, be limited to the axial displacement of extruding force screw rod 7 when excessive, avoid two screw rods 7 mutually to hang, improve equipment reliability of operation, also make equipment can be applicable to the material extrusion granulator that viscosity is large.
For same object, on such scheme basis, also can increase front end fixed disk 76 at the bearing side of screw rod 7, front end fixed disk 76 is fixedly connected with barrel, guarantees that screw rod 7 do not hang mutually.
As shown in Figure 8 and Figure 9, for improving granular mass, described extrusion die 3 does not adopt common cylindrical hole, but at the supplied materials sidetracking macropore 31 of described extrusion die 3, the discharging sidetracking aperture 32 of extrusion die, macropore 31 correspondences are communicated with one or two aperture 32 and form discharge opening 30, and material is further compressed when by extrusion die 3 like this, obtains granule more closely.Consider discharging uniformity, the aperture 32 of the exit side of extrusion die generally should be uniform, can be in the periphery of extrusion die 3 with more two apertures 32 of corresponding connection of a macropore 31, extrusion die 3 leans on paracentral position with a more aperture 32 of corresponding connection of a macropore 31.
Usually, can bear larger extruding force for guaranteeing template, guarantee that equipment also can normally move in the time of the very large material of extruding viscosity, give full play to the squeezing action in discharging hole 30 simultaneously, described extrusion die 3 should have suitable thickness, and its thickness is considered the processing in hole more than conventionally should reaching 30mm, thickness also should not be too thick, and its thickness is generally not more than 40mm.
As shown in Fig. 1, Figure 12 and Figure 13, owing to having adopted extruding granulation mode, tightr from extrusion die material strip quality out, the peeling knife 6 of the exit side setting of available extrusion die 3 cuts granulating, injure extrusion die 3 when avoiding peeling knife 6 to move and produce metal fillings, its cutter hub is the elastic 60 being convexly curved near the part on sword limit 61, in the time that feed is adjusted, make 61 two ends, sword limit can with extrusion die 3 cutting of fitting well.
For increasing extrusion pressure, the centre bore 40 of described poly-charging tray 4 is the combination bore of taper hole and circular hole, also material is pushed at poly-charging tray 4 places, makes equipment can be applicable to the material extrusion granulator that viscosity is larger.
Compressing grains facility of the present invention have powerful extruding force (45000N～150000N); reach 40～90% material for dry extract amount; also can mandatoryly extrude, cutting; can be because material affects too much equipment operation, cannot granulate containing extractum yet, the granular pile density obtaining is at least greater than 0.78g/cm
3, scope is 0.78-0.9g/cm
3.
Step B adopts the standby granule of compressing grains mechanism, and the granule then obtaining by cold drying-high temperature puffing, dried is in profile, mobility, and moisture absorption, brews and in complexity, is all better than the granule prepared than existing methods; And preparation time also finds, apply preparation method of the present invention, can obviously reduce supplementary product consumption, minimizing patient takes in unnecessary adjuvant, reduces production costs.
By preparing examples prove beneficial effect of the present invention, when granulation, all adopt compressing grains mechanism grain of the present invention below.
Get Radix Scrophulariae 400g, Radix Ophiopogonis 400g, Radix Glycyrrhizae 400g, Radix Platycodonis 400g, decoct with water three times, 1.5 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and filtrate leaves standstill 12 hours, get the extractum that supernatant concentration to relative density is 1.32～1.35 (80～85 ℃), be dried to dry extract.The dry extract of following embodiment all adopts said method preparation.
Comparative example 1
(1) get extractum, by 1 part of dry extract, with 4.5 parts of sucrose, 1 part, dextrin, granulation, bulk density is about 0.60g/cm
3, dry, obtain granule 1000g, be distributed into 100 bags and get final product.。
(2) get extractum, add appropriate dextrin and sweeting agent, granulation, bulk density is about 0.62g/cm
3, dry, make 300g (Sugarless type) granule, be distributed into 50 bags, to obtain final product.
Embodiment 1
Get dry extract, pulverize, add appropriate amount of starch and sucrose, granulation, bulk density is about 0.86g/cm
3, first under the cryogenic conditions of 40-60 ℃ dried particles to water content 4-5%; Then under the cryogenic conditions of 65-95 ℃, maintain at least 5 minutes, expanded to granule; Maintain again high-temperature condition, below dried particles moisture to 2%, obtain granule 250g, be distributed into 100 bags and get final product.
Embodiment 2
Get dry extract, pulverize, add appropriate dextrin and sweeting agent, granulation, bulk density is about 0.88g/cm
3, first under the cryogenic conditions of 40-60 ℃, dried particles, to water content 4-5%, then maintains at least 5 minutes under the hot conditions of 75-95 ℃, expanded to granule; Maintain again this hot conditions, below dried particles moisture to 2%, be dried to obtain granule 250g, be distributed into 100 bags, to obtain final product.[this granule is Sugarless type]
Get dry extract, pulverize, add appropriate dextrin, granulation, bulk density is about 0.83g/cm
3, first under the cryogenic conditions of 40-60 ℃, dried particles, to water content 4-5%, then maintains at least 5 minutes under the hot conditions of 65-95 ℃, expanded to granule; Maintain again this hot conditions, below dried particles moisture to 2%, be dried to obtain granule 200g, be distributed into 100 bags, to obtain final product.[this granule is Sugarless type]
Get dry extract, pulverize, add sucrose appropriate, granulation, bulk density is about 0.86g/cm
3, first under the cryogenic conditions of 40-60 ℃ dried particles to water content 6%, then under the hot conditions of 65-75 ℃, maintain more than 15 minutes to below pellet moisture to 2% yet for the expanded situation of appearance, obtain granule 250g, be distributed into 100 bags.Particulate amorphous, fugitive, broken, mobility is poor.
Embodiment 5
Get dry extract, pulverize, add appropriate dextrin, granulation, bulk density is about 0.88g/cm
3, first under the cryogenic conditions of 40-60 ℃ dried particles to water content 3%, then under the hot conditions of 65-75 ℃, maintain more than 15 minutes to below pellet moisture to 2% yet for the expanded situation of appearance, obtain granule 250g, be distributed into 100 bags, to obtain final product.Particulate amorphous, fugitive, broken, mobility is poor.[this granule is Sugarless type]
As fully visible, granule prepared by existing technique is amorphous granular, fugitive, broken, mobility is poor, if and adopting cold drying water content when technique of the present invention to exceed the scope of 4-5%, also cannot reach expanded effect under hot conditions, as embodiment 4 and embodiment 5.And the profile of the Xuanmai Ganju swelling granular agent (embodiment 1-3) prepared of technique of the present invention obviously more existing process shape is more attractive in appearance, its smooth in appearance densification, spherical particle, inside have the expanded phenomenon of cavity; Granule scope angle of repose is 10-25 °, and good fluidity, is difficult for the moisture absorption; Supplementary product consumption is few; It is also easier to brew.
Claims (8)
1. the preparation method of Xuanmai Ganju swelling granular agent, prepare and obtain by following method:
A, take the crude drug of following weight proportioning: Radix Scrophulariae 300-500 part, Radix Ophiopogonis 300-500 part, Radix Glycyrrhizae 300-500 part, Radix Platycodonis 300-500 part, adopt conventional method to be prepared into extractum;
B, extractum is made after soft material, granulated, granulate is to crossing 14-24 mesh sieve;
C, dried particles;
It is characterized in that:
Described in step B, granulate as making the granule that bulk density is greater than 0.78g/cm3;
Dried particles described in step C is to adopt following method:
(1) first under the cryogenic conditions of 40-60 ℃ dried particles to water content 4-5%;
(2) then under the hot conditions of 65-95 ℃, be heated to granule expanded;
(3) maintain again 65-95 ℃ of hot conditions, below dried particles moisture to 2%, obtain granule;
Described granulation is to adopt compressing grains machine compressed granulate;
Described compressing grains machine, comprise that the double-screw type in head (1) extrudes pay-off and extrude with this discharge barrel (2) that pay-off coordinates, the exit of discharge barrel (2) arranges the extrusion die (3) that has discharge opening (30), in discharge barrel (2), between twin-screw extrusion pay-off and extrusion die (3), be provided with by-passing parts (5);
The center of the exit side of described by-passing parts (5) is provided with central boss (55), the surrounding of exit side is provided with back-up block (56), central boss (55) contacts with surrounding with the center of extrusion die (3) respectively with back-up block (56), and blow tank (53) is positioned between central boss (55) and back-up block (56); Further preferably be provided with the poly-charging tray bayonet socket (54) adaptive with centre bore (40) in the supplied materials side of described by-passing parts (5);
Between twin-screw extrusion pay-off and by-passing parts (5), be provided with and by-passing parts (5) the poly-charging tray (4) with centre bore (40) by touching mutually, the supplied materials side of by-passing parts (5) is evenly equipped with splitter box (51), splitter box (51) converges at the blow tank (53) of by-passing parts exit side, and blow tank (53) is corresponding with the discharge opening (30) of extrusion die (3).
2. the preparation method of Xuanmai Ganju swelling granular according to claim 1 agent, is characterized in that: step B prepares soft material after extractum is made to dry extract again.
3. the preparation method of Xuanmai Ganju swelling granular according to claim 1 agent, is characterized in that: described splitter box (51) is sector diffuence groove, is shunting ridge (52) between adjacent two sector diffuence grooves.
4. according to the preparation method of the Xuanmai Ganju swelling granular agent described in claim 1 or 3, it is characterized in that: the screw rod (7) that described double-screw type is extruded pay-off is provided with cooling structure, described cooling structure is included in the blind hole concentric with screw axis (70) of offering on screw rod (7) and the inner cool tube (71) that is provided with cooling entrance (74), inner cool tube (71) stretches in described blind hole (70) through the cooling cover (72) of this blind hole of sealing (70) and its built-in length is less than blind hole (70) degree of depth, cooling cover (72) has the cooling cover inner chamber (720) that is provided with coolant outlet (75), the cooling duct (700) forming between inner cool tube (71) and blind pore wall is communicated with cooling cover inner chamber (720), further preferred described inner cool tube (71) is fixed on cooling cover (72) above by nut (73), and described cooling cover (72) is fixedly connected with head (1).
5. according to the preparation method of the Xuanmai Ganju swelling granular agent described in claim 1 or 3, it is characterized in that: the supplied materials side of described extrusion die (3) is macropore (31), the exit side of extrusion die is aperture (32), and a macropore (31) is corresponding is communicated with one or two aperture (32) and formation discharge opening (30).
6. according to the preparation method of the Xuanmai Ganju swelling granular agent described in claim 1 or 3, it is characterized in that: the exit side of described extrusion die (3) is provided with peeling knife (6), its cutter hub is the elastic (60) being convexly curved near the part of sword limit (61).
7. according to the preparation method of the Xuanmai Ganju swelling granular agent described in claim 1 or 3, it is characterized in that: the centre bore (40) of described poly-charging tray (4) is the combination bore of taper hole and circular hole.
Preparation method described in claim 1-7 any one preparation and the agent of Xuanmai Ganju swelling granular.
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