CN101396417B - Honeysuckle dispensing granule and preparation method and quality control method thereof - Google Patents
Honeysuckle dispensing granule and preparation method and quality control method thereof Download PDFInfo
- Publication number
- CN101396417B CN101396417B CN 200710175351 CN200710175351A CN101396417B CN 101396417 B CN101396417 B CN 101396417B CN 200710175351 CN200710175351 CN 200710175351 CN 200710175351 A CN200710175351 A CN 200710175351A CN 101396417 B CN101396417 B CN 101396417B
- Authority
- CN
- China
- Prior art keywords
- flos lonicerae
- spray drying
- shallow oil
- water
- hour
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Abstract
The invention discloses honeysuckle flower formula particles, a preparation method and a quality control method thereof. The formula particles take Flos Lonicerae Japonicae as raw material, honeysuckle flower spray-dried powder is prepared by water extraction, pressure reduction concentration, spray drying, and the like, the honeysuckle flower spray-dried powder is directly dry-granulated or dry-granulated after being mixed with appropriate amount of excipients to prepare the honeysuckle flower formula particles; each gram of the honeysuckle flower formula particles is equal to 5g of crude drug, and the honeysuckle flower formula particles have the infrared fingerprint spectrum which is shown in Figure 3. The preparation method can effectively ensure that each gram of the honeysuckle flower formula particles is equal to 5g of the crude drug; the invention adopts the infrared fingerprint spectrum technology for carrying out the quality control, and the quality control method is scientific, advanced, rapid and strong in specificity and operability.
Description
Technical field
The present invention relates to a kind of Chinese medicinal granule and preparation method thereof and method of quality control, particularly a kind of honeysuckle dispensing granule and preparation method thereof and method of quality control.
Background technology
Chinese medicinal granule is under Chinese medical theory instructs, and the prepared slices of Chinese crude drugs are formed through various processes, is used for the granule that clinical tcm prescription allotment is used; Compare with traditional Chinese herbs decoction, its taking convenience, dose is little, and is quality controllable, preserves easily, is easy to carry; Chinese medicinal granule is in the pilot production status at home at present, product technology and quality standard disunity.Honeysuckle dispensing granule is a kind of of conventional Chinese medicine granule, and honeysuckle dispensing granule mostly is the traditional water extraction at present, and different production units cause the product quality of different manufacturers inconsistent because production equipment is different with production technology, and there is difference in drug effect.Its quality standard is generally the discriminating of chlorogenic acid thin-layer qualitative and chlorogenic acid and luteoloside assay, the specificity of this standard is limit by certain test conditions and scope, lack other due quality informations of product, this standard can't be judged the quality good or not and the overall picture of honeysuckle dispensing granule product comprehensively.
Infrared spectrometry is one of conventional means of differentiating chemical compound and definite structure of matter.In pharmaceutical analysis, " fingerprint " characteristic that has with infrared spectrum is the common method that adopts of various countries' pharmacopeia as the foundation of drug identification.But since Chinese crude drug, the prepared slices of Chinese crude drugs and Chinese patent medicine itself all be more than the Western medicine complexity many mixture systems, the spectrum analysis difficulty makes conventional infrared spectrometry fail its due effect of performance in Chinese medicine quality control and management in the long term.
Summary of the invention
The objective of the invention is to disclose a kind of honeysuckle dispensing granule; The present invention also aims to disclose the preparation method of this granule; The present invention also aims to disclose the method for quality control of this granule.
The present invention seeks to be achieved through the following technical solutions.
The every gram of honeysuckle dispensing granule of the present invention contains suitable crude drug amount 5 grams; Chlorogenic acid (C in the granule
16H
18O
9) content be not less than 2.0%; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer, at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm
-1, 1409cm
-1, 1270cm
-1At the place characteristic absorption is arranged also;
Its Infrared fingerprint spectra condition determination: instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
The preparation method of honeysuckle dispensing granule of the present invention is:
Get the water that the raw material Flos Lonicerae adds 5-15 times of weight portion, soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5-15 times of weight portion of raw material Flos Lonicerae, extracts 0.5-3 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10-1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Amount of water can be a 6-7 times of weight portion in the above-mentioned preparation method, 8-12 times of weight portion or 13-14 times of weight portion.
Extraction time can be 1-1.5 hour or 2-2.5 hour in the above-mentioned preparation method.
Above-mentioned preparation method is preferably: get the water that the raw material Flos Lonicerae adds 10 times of weight portions, soaked into 1 hour, extracted 1 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Flos Lonicerae, extracts 1 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.12, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule.
Get the water that the raw material Flos Lonicerae adds 9 times of weight portions, soaked into 0.8 hour, extracted 1.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Flos Lonicerae, extracts 2 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Get the water that the raw material Flos Lonicerae adds 11 times of weight portions, soaked into 1.5 hours, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Flos Lonicerae, extracts 0.75 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
The drying process with atomizing parameter is in the above-mentioned preparation method: 40 ℃-60 ℃ of medicinal liquid preheat temperatures; 170 ℃-185 ℃ of inlet temperature; 450-700 rev/min of material revolution speed; 70 ℃-85 ℃ of leaving air temps; Wind send 40 ℃-50 ℃ of temperature.
The granulation parameter is in the above-mentioned preparation method: main pinch roller pressure: 4-6MPa; Side pressure wheel pressure: 0.4-0.6MPa; The speed of mainshaft: 300-500 rev/min; Feed voltage: 100-150V; Granular size: 20-60 order.
The method of quality control of honeysuckle dispensing granule of the present invention comprises one or more in the following method:
A. the method for quality control of Flos Lonicerae spray drying powder: the Flos Lonicerae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae spray drying powder standard Infrared fingerprint spectra (Fig. 2) is: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1047cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1697cm
-1, 1614cm
-1At 2927cm
-1, 1411cm
-1, 1278cm
-1At the place characteristic absorption is arranged also;
B. the method for quality control of honeysuckle dispensing granule: honeysuckle dispensing granule adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; Honeysuckle dispensing granule standard Infrared fingerprint spectra (Fig. 3) is: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm-
1, 1409cm
-1, 1270cm
-1At the place characteristic absorption is arranged also.
Flos Lonicerae raw material of the present invention can be the certified products that meet a regulation of Pharmacopoeia of the People's Republic of China version in 2005.
Infrared fingerprint spectra of the present invention can be to reach Infrared fingerprint spectra more than 90% with its dependency.
Description of drawings
Fig. 1: Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra
Fig. 2: Flos Lonicerae spray drying powder standard Infrared fingerprint spectra
Fig. 3: honeysuckle dispensing granule standard Infrared fingerprint spectra
Fig. 4: contain the classical medicine of Flos Lonicerae decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram are compared
Fig. 5: contain Flos Lonicerae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram relatively
Fig. 6: honeysuckle dispensing granule and Chinese medicine honeysuckle thin layer chromatography are relatively
Fig. 7: honeysuckle dispensing granule and Chinese medicine honeysuckle thin-layer sample Infrared fingerprint spectra are relatively
Granule of the present invention has complete, advanced production technology and strong, the controlled quality control standard of specificity, and technology advanced person can realize, the detection method science that quality standard relates to, advanced person, quick, workable.The present invention is applied to infrared spectrum technology the quality control of Chinese medicine, this is the innovation on a kind of thinking, this not only meets the theory of Chinese medicine about " monarch, minister, help, make ", also given prominence to the group effect of Chinese medicine, simultaneously complicated problems is oversimplified, certain Chinese medicine is done as a whole, observed its " fingerprint ", thereby solved a matter of utmost importance--the evaluation of-Chinese medicine true and false in the control of Chinese medicine macroscopic quality apace.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
The chlorogenic acid utilization of experimental example 1 granule of the present invention and Chinese medicine honeysuckle relatively
Extracting honeysuckle decoction pieces 50 grams extracted 30 minutes with 10 times of water gagings, leached medicinal liquid; Medicinal residues add 8 times of amounts of water, extract 20 minutes, leach medicinal liquid, merge two liquid of boiling medicine, suitably concentrate 100 milliliters of concentrated solutions.According to middle determination of chlorogenic acid item method of Pharmacopoeia of the People's Republic of China version in 2005, measure chlorogenic acid contents in the concentrated solution, and the amount of chlorogenic acid in the calculating decocting liquid, above-mentioned test repeats to do 3 times with the Flos Lonicerae of different batches, record in the decocting liquid amount of chlorogenic acid and be followed successively by 0.21 gram, 0.20 gram and 0.22 restrains.Measure the chlorogenic acid content in three batches of honeysuckle dispensing granules, be followed successively by 2.2%, 2.4%, 2.0%, promptly the contained chlorogenic acid of 10 gram honeysuckle dispensing granules is respectively 0.22 gram, 0.24 gram, 0.20 gram.Illustrate that the amount of chlorogenic acid in the 10 gram honeysuckle dispensing granules is equivalent to the utilization of 50 gram Flos Lonicerae decoction pieces chlorogenic acid in decoction, the equivalent that 1 gram honeysuckle dispensing granule of the present invention is equivalent to 5 gram Chinese medicine honeysuckles is a science.
Experimental example 2 contains the classical medicine of Flos Lonicerae decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram is compared
Flos Lonicerae-Fructus Forsythiae medicine is to coming from " the pestilence bar is distinguished ".
Experiment purpose: research Flos Lonicerae-Fructus Forsythiae medicine is determined honeysuckle dispensing granule technology and normal reasonability to the similarities and differences that decoction pieces closes decocting liquid and granular recipe.
Experimental technique: extracting honeysuckle decoction pieces 10g, Fructus Forsythiae decoction pieces 10g prescription, the decocting method of pressing the decoction pieces decoction decocts preparation decoction pieces decocting liquid sample; Other gets Fructus Forsythiae decoction pieces 10g, and the decocting method of pressing the decoction pieces decoction decocts, and medicinal liquid suitably concentrates, and adds honeysuckle dispensing granule 2g of the present invention, is stirred to dissolving fully, preparation granular recipe sample; Drinking sheet decocting liquid sample, granular recipe sample respectively carries out infrared spectrum and detects.
Testing conditions: detecting instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
Testing result: decoction pieces decocting liquid sample and granular recipe sample Infrared fingerprint spectra peak shape, peak position, relative peak intensity basically identical as shown in Figure 4, dependency reaches 93.4%.It is consistent to prove that soup that granule of the present invention is joined and decoction pieces close the decocting liquid composition, be that 1g honeysuckle dispensing granule of the present invention is consistent with a 5g Flos Lonicerae decoction pieces fried composition, equivalent and production technology that honeysuckle dispensing granule 1g of the present invention is equivalent to Flos Lonicerae decoction pieces 5g are rational.
Experimental example 3 contains Flos Lonicerae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram compares
Wuwei xiaodu drink comes from Golden Mirror of Medicine, and prescription is formed and comprised Flos Lonicerae, Flos Chrysanthemi Indici, Herba Taraxaci, Herba Violae, 5 flavour of a drug of Radix Semiaquilegiae; The effect heat-clearing and toxic substances removing, the dissipation furuncle.
Experiment purpose: the similarities and differences of research wuwei xiaodu drink decoction pieces decocting liquid and granular recipe, determine honeysuckle dispensing granule technology and normal reasonability.
Experimental technique: press 5 flavour of a drug prescriptions such as wuwei xiaodu drink proportioning extracting honeysuckle, the decocting method of pressing the decoction pieces decoction decocts preparation decoction pieces decocting liquid sample; In addition get other decoction pieces except that Flos Lonicerae respectively by wuwei xiaodu drink prescription proportioning, the decocting method of pressing the decoction pieces decoction decocts, medicinal liquid suitably concentrates, getting honeysuckle dispensing granule of the present invention by wuwei xiaodu drink prescription proportioning and equivalent relation adds in the concentrated medicament, be stirred to dissolving fully, preparation granular recipe sample; Drinking sheet decocting liquid sample, granular recipe sample respectively carries out infrared spectrum and detects.
Testing conditions: instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
Testing result: decoction pieces decocting liquid sample and granular recipe sample Infrared fingerprint spectra peak shape, peak position, relative peak intensity basically identical as shown in Figure 5, dependency reaches 97.3%.It is consistent to prove that soup that granule is joined and decoction pieces close the decocting liquid composition, it is consistent with a Flos Lonicerae decoction pieces fried composition promptly to add honeysuckle dispensing granule of the present invention, and equivalent and production technology that honeysuckle dispensing granule 1g of the present invention is equivalent to Flos Lonicerae decoction pieces 5g are rational.
Experimental example 4
(1) honeysuckle dispensing granule and the comparative study of Chinese medicine honeysuckle thin layer chromatography
Differentiate a thin layer chromatography test down according to middle Chinese medicine honeysuckle of Pharmacopoeia of the People's Republic of China version in 2005, prepare sample with Chinese medicine honeysuckle and honeysuckle dispensing granule of the present invention, measure, the gained result as shown in Figure 6, in the honeysuckle dispensing granule chromatograph, with the corresponding position of Chinese medicine honeysuckle chromatograph on, show the speckle of same color.
(2) honeysuckle dispensing granule and Chinese medicine honeysuckle thin-layer sample Infrared fingerprint spectra are relatively
Measure the Chinese medicine honeysuckle of preparation in (1) and the thin-layer sample of honeysuckle dispensing granule with Fourier transform infrared spectrometer, its result as shown in Figure 7, the thin-layer sample Infrared fingerprint spectra peak shape of honeysuckle dispensing granule and Chinese medicine honeysuckle, peak position, relative peak intensity basically identical.
The result proves that honeysuckle dispensing granule of the present invention is consistent with the Chinese medicine honeysuckle composition, and technology of the present invention is rational.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: honeysuckle dispensing granule of the present invention
Get raw material Flos Lonicerae 100kg, added the 1000kg water infiltration 1 hour, extracted 1 hour, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 800kg water, extracts 1 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.12, concentrated solution; Concentrated solution is 50 ℃ of preheatings, 175 ℃ of inlet temperature, 550 rev/mins of material revolution speeds, 80 ℃ of leaving air temps, wind send spray drying under the condition of 45 ℃ of temperature, Flos Lonicerae spray drying powder 30kg; The Flos Lonicerae spray drying powder is 5MPa at main pinch roller pressure, and side pressure wheel pressure is 0.5MPa, and the speed of mainshaft is 400 rev/mins, and feed voltage is a direct dry granulation under the condition of 120V, 20-60 order honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae.Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Embodiment 2: honeysuckle dispensing granule of the present invention
Get raw material Flos Lonicerae 100kg, added the 900kg water infiltration 0.8 hour, extracted 1.5 hours, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 1000kg water, extracts 2 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; Concentrated solution is 55 ℃ of preheatings, 170 ℃ of inlet temperature, 600 rev/mins of material revolution speeds, 75 ℃ of leaving air temps, wind send spray drying under the condition of 50 ℃ of temperature, Flos Lonicerae spray drying powder 28kg; In the Flos Lonicerae spray drying powder, add 5.6kg adjuvant dextrin; At main pinch roller pressure is 6MPa, and side pressure wheel pressure is 0.4MPa, and the speed of mainshaft is 450 rev/mins, and feed voltage is a dry granulation under the condition of 110V, 20-60 order honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Embodiment 3: honeysuckle dispensing granule of the present invention
Get raw material Flos Lonicerae 100kg, added the 1100g water infiltration 1.5 hours, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 600kg water, extracts 0.75 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.15, concentrated solution; Concentrated solution is 45 ℃ of preheatings, 180 ℃ of inlet temperature, 500 rev/mins of material revolution speeds, 85 ℃ of leaving air temps, wind send spray drying under the condition of 40 ℃ of temperature, Flos Lonicerae spray drying powder 32kg; The adjuvant lactose that in the Flos Lonicerae spray drying powder, adds 3.2kg; At main pinch roller pressure is 4MPa, and side pressure wheel pressure is 0.6MPa, and the speed of mainshaft is 350 rev/mins, and feed voltage is a dry granulation under the condition of 140V, 20-60 order honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Embodiment 4: honeysuckle dispensing granule of the present invention
Get raw material Flos Lonicerae 100kg, added the 700kg water infiltration 0.75 hour, extracted 1.25 hours,
Promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 1300kg water, extracts 2.5 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.11, concentrated solution; Concentrated solution is 60 ℃ of preheatings, 170 ℃ of inlet temperature, 600 rev/mins of material revolution speeds, 75 ℃ of leaving air temps, wind send spray drying under the condition of 50 ℃ of temperature, Flos Lonicerae spray drying powder 29kg; In the Flos Lonicerae spray drying powder, add 4.3kg adjuvant dextrin; At main pinch roller pressure is 5MPa, and side pressure wheel pressure is 0.4MPa, and the speed of mainshaft is 500 rev/mins, and feed voltage is a dry granulation under the condition of 100V, 20-60 order honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Embodiment 5: honeysuckle dispensing granule of the present invention
Get raw material Flos Lonicerae 100kg, added the 1300g water infiltration 1.25 hours, extracted 2.5 hours, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 700kg water, extracts 1.5 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.14, concentrated solution; Concentrated solution is 40 ℃ of preheatings, 180 ℃ of inlet temperature, 500 rev/mins of material revolution speeds, 85 ℃ of leaving air temps, wind send spray drying under the condition of 40 ℃ of temperature, Flos Lonicerae spray drying powder 31kg; The adjuvant lactose that in the Flos Lonicerae spray drying powder, adds 2kg; At main pinch roller pressure is 5MPa, and side pressure wheel pressure is 0.6MPa, and the speed of mainshaft is 300 rev/mins, and feed voltage is a dry granulation under the condition of 130V, 20-60 order honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1Also there is characteristic absorption at the place.
Embodiment 6: the method for quality control of the Flos Lonicerae spray drying powder of the present invention of embodiment 1 preparation
The method of quality control of Flos Lonicerae spray drying powder: the Flos Lonicerae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra of Flos Lonicerae spray drying powder is characterized as: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1047cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1697cm
-1, 1614cm
-1At 2927cm
-1, 1411cm
-1, 1278cm
-1At the place characteristic absorption is arranged also.
Embodiment 7: the method for quality control of the honeysuckle dispensing granule of the present invention of embodiment 2 preparations
The method of quality control of honeysuckle dispensing granule: honeysuckle dispensing granule adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; The standard Infrared fingerprint spectra of honeysuckle dispensing granule is characterized as: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm
-1, 1409cm
-1, 1270cm
-1At the place characteristic absorption is arranged also.
Embodiment 8: the method for quality control of the honeysuckle dispensing granule of the present invention of embodiment 3 preparations
A. the method for quality control of Flos Lonicerae spray drying powder: the Flos Lonicerae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra of Flos Lonicerae spray drying powder is characterized as: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1047cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1697cm
-1, 1614cm
-1At 2927cm
-1, 1411cm
-1, 1278cm
-1At the place characteristic absorption is arranged also;
B. the method for quality control of honeysuckle dispensing granule: honeysuckle dispensing granule adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; The standard Infrared fingerprint spectra of honeysuckle dispensing granule is characterized as: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm
-1, 1409cm
-1, 1270cm
-1At the place characteristic absorption is arranged also.
Claims (10)
1. a honeysuckle dispensing granule is characterized in that the every gram of this granule contains suitable crude drug amount 5 grams; Chlorogenic acid contents is not less than 2.0% in the granule; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer, at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm
-1, 1409cm
-1, 1270cm
-1There is characteristic absorption at the place;
Its Infrared fingerprint spectra condition determination: instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects;
Wherein, honeysuckle dispensing granule is prepared from by following method:
Get the water that the raw material Flos Lonicerae adds 5-15 times of weight portion, soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5-15 times of weight portion of raw material Flos Lonicerae, extracts 0.5-3 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10-1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae Flos Lonicerae Japonicae standard Infrared fingerprint spectra has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1There is characteristic absorption at the place.
2. honeysuckle dispensing granule as claimed in claim 1 is characterized in that wherein said Infrared fingerprint spectra is to reach Infrared fingerprint spectra more than 90% with its dependency.
3. honeysuckle dispensing granule as claimed in claim 1 or 2 is characterized in that, amount of water is a 6-7 times of weight portion in the preparation method of wherein said honeysuckle dispensing granule, 8-12 times of weight portion or 13-14 times of weight portion.
4. honeysuckle dispensing granule as claimed in claim 1 or 2 is characterized in that, extraction time is 1-1.5 hour or 2-2.5 hour in the preparation method of wherein said honeysuckle dispensing granule.
5. honeysuckle dispensing granule as claimed in claim 1 or 2 is characterized in that, wherein said honeysuckle dispensing granule is by a kind of being prepared from the following method:
Get the water that the raw material Flos Lonicerae adds 10 times of weight portions, soaked into 1 hour, extracted 1 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Flos Lonicerae, extracts 1 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.12, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Or get the water that the raw material Flos Lonicerae adds 9 times of weight portions, and soaked into 0.8 hour, extracted 1.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Flos Lonicerae, extracts 2 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Or get the water that the raw material Flos Lonicerae adds 11 times of weight portions, and soaked into 1.5 hours, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Flos Lonicerae, extracts 0.75 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule.
6. the method for preparing honeysuckle dispensing granule as claimed in claim 1 or 2 is characterized in that this method is: get the water that the raw material Flos Lonicerae adds 5-15 times of weight portion, soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5-15 times of weight portion of raw material Flos Lonicerae, extracts 0.5-3 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10-1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule; Wherein the raw material Flos Lonicerae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae F1os Lonicerae Japonicae standard Infrared fingerprint spectra has following feature: at 1633cm
-1, 1051cm
-1There are two feature Dan Qiangfeng, wherein 1051cm in the place
-1It is main strong peak; In addition, at 2923cm
-1, 1378cm
-1, 1262cm
-1, 768cm
-1, 607cm
-1There is characteristic absorption at the place.
7. method as claimed in claim 6 is characterized in that amount of water is a 6-7 times of weight portion in this method, 8-12 times of weight portion or 13-14 times of weight portion.
8. method as claimed in claim 6 is characterized in that extraction time is 1-1.5 hour or 2-2.5 hour in this method.
9. the method for preparing honeysuckle dispensing granule as claimed in claim 5 is characterized in that this method is: get the water that the raw material Flos Lonicerae adds 10 times of weight portions, soaked into 1 hour, extracted 1 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Flos Lonicerae, extracts 1 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.12, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Or get the water that the raw material Flos Lonicerae adds 9 times of weight portions, and soaked into 0.8 hour, extracted 1.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Flos Lonicerae, extracts 2 hours, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1～0, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule;
Or get the water that the raw material Flos Lonicerae adds 11 times of weight portions, and soaked into 1.5 hours, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Flos Lonicerae, extracts 0.75 hour, promptly two fries in shallow oil; Two liquid of boiling medicine merge, and are evaporated to relative density 1.15, concentrated solution; The concentrated solution spray drying gets the Flos Lonicerae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0-25% in the Flos Lonicerae spray drying powder; Dry granulation gets honeysuckle dispensing granule.
10. as the quality determining method of the arbitrary described honeysuckle dispensing granule of claim 1-5, it is characterized in that this quality determining method comprises one or more in the following method:
A. the quality determining method of Flos Lonicerae spray drying powder: the Flos Lonicerae spray drying powder adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; Flos Lonicerae spray drying powder standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1047
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1697cm
-1, 1614cm
-1At 2927cm
-1, 1411cm
-1, 1278cm
-1There is characteristic absorption at the place;
B. the quality determining method of honeysuckle dispensing granule: honeysuckle dispensing granule adopts Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process is measured; Honeysuckle dispensing granule standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between the strong peak of master of a broad is arranged, peak position is 1049cm
-1At 2000cm
-1-1500cm
-1Between have one to become stair-stepping broad peak to be time strong peak, ladder absworption peak peak position from low to high is respectively 1691cm
-1, 1612cm
-1At 2922cm
-1, 1409cm
-1, 1270cm
-1There is characteristic absorption at the place.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710175351 CN101396417B (en) | 2007-09-28 | 2007-09-28 | Honeysuckle dispensing granule and preparation method and quality control method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710175351 CN101396417B (en) | 2007-09-28 | 2007-09-28 | Honeysuckle dispensing granule and preparation method and quality control method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101396417A CN101396417A (en) | 2009-04-01 |
| CN101396417B true CN101396417B (en) | 2011-08-03 |
Family
ID=40515417
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710175351 Active CN101396417B (en) | 2007-09-28 | 2007-09-28 | Honeysuckle dispensing granule and preparation method and quality control method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101396417B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102204935A (en) * | 2011-06-07 | 2011-10-05 | 江苏省中医药研究院 | Preparation method of single Chinese medicinal formula tablets |
| CN103239413A (en) * | 2013-05-27 | 2013-08-14 | 内蒙古大漠药业股份有限公司 | Method for large-scale production of traditional Chinese medicine powder particles |
| CN104127471A (en) * | 2014-07-31 | 2014-11-05 | 安徽济人药业有限公司 | Preparation method and quality control method for honeysuckle flower formula granule |
| CN104873391A (en) * | 2015-05-23 | 2015-09-02 | 神威药业集团有限公司 | Preparation method for flower formula granules |
| CN106770001A (en) * | 2016-11-11 | 2017-05-31 | 本溪国家中成药工程技术研究中心有限公司 | Method and application using extract solution concentration process in the preparation process of near infrared spectroscopy quick detection qizhi weitong granules |
| CN107091887A (en) * | 2017-03-29 | 2017-08-25 | 哈尔滨珍宝制药有限公司 | The detection method and method of quality control of a kind of characteristic spectrum of honeysuckle dispensing granule |
| CN109568371A (en) * | 2018-02-06 | 2019-04-05 | 广东方制药有限公司 | A kind of preparation method of honeysuckle dispensing granule |
| CN108653370A (en) * | 2018-07-31 | 2018-10-16 | 庐山市环绿时代农业科技开发有限公司 | A kind of preparation method of honeysuckle particle |
| CN111358824A (en) * | 2020-04-08 | 2020-07-03 | 亳州益智健康产业有限公司 | Preparation method of honeysuckle flower formula granules |
-
2007
- 2007-09-28 CN CN 200710175351 patent/CN101396417B/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 仇法新 等.中药配方颗粒的发展现状及应用前景.《中国药房》.2007,第18卷(第3期),164页"1 中药配方颗粒名称的确定"章节和"2.1制备工艺的研究"章节. |
| 周群 等.中药配方颗粒红外光谱法的快速鉴别.《分析化学研究报告》.2003,第31卷(第3期),第294页图4. * |
| 郭用庄 等.金银花配方颗粒质量标准的研究.《中成药》.2002,第24卷(第6期),第424页左栏第1段，第425页左栏表2. * |
| 黄喜茹 申朋.金银花及其制剂指纹图谱的构建解析与质量标准研究进展.《上海中医药杂志》.2006,第40卷(第10期),第74页"3 金银花及其制剂质量标准的研究"章节. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101396417A (en) | 2009-04-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101474273B (en) | Stir-fried fructus gardenia dispensing granule as well as preparation method and quality control method thereof | |
| CN101396417B (en) | Honeysuckle dispensing granule and preparation method and quality control method thereof | |
| CN101396426B (en) | Glycyrrhiza dispensing granule and preparation method and quality control method thereof | |
| CN101396458B (en) | Tangerine peel dispensing granule, and preparation method and quality control method thereof | |
| CN101396430B (en) | Scutellaria dispensing granule and preparation method and quality control method thereof | |
| CN101396423B (en) | Kudzu root dispensing granule and preparation method and quality control method thereof | |
| CN101342258A (en) | Hooked uncaria prescription particle, preparation method and quality control method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: BEIJING KANGRENTANG MEDICINE CO., LTD. Free format text: FORMER OWNER: WEIMING TIANREN CHINESE MEDICINE CO., LTD. Effective date: 20090612 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20090612 Address after: Postal code 16, Hebei Avenue, Shunyi District, Beijing: 101300 Applicant after: Beijing Kangrentang Pharmaceutical Co., Ltd. Address before: Postal code 16, Lin Hebei street, Lin River Industrial Development Zone, Beijing, Shunyi District: 101300 Applicant before: WenMingTianRen Traditional Chinese Medicine Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |