CN101396458B - Tangerine peel dispensing granule, and preparation method and quality control method thereof - Google Patents
Tangerine peel dispensing granule, and preparation method and quality control method thereof Download PDFInfo
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- CN101396458B CN101396458B CN 200710175354 CN200710175354A CN101396458B CN 101396458 B CN101396458 B CN 101396458B CN 200710175354 CN200710175354 CN 200710175354 CN 200710175354 A CN200710175354 A CN 200710175354A CN 101396458 B CN101396458 B CN 101396458B
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- citri reticulatae
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Abstract
The invention discloses tangerine peel formula particles, a preparation method and a quality control method thereof. The formula particles take Pericarpium Citri Reticulatae as raw material, tangerine peel spray-dried powder is prepared by ethanol extraction, water extraction, pressure reduction concentration, spray drying, and the like; the tangerine peel spray-dried powder is directly dry-granulated or dry-granulated after being mixed with appropriate amount of excipients to prepare the tangerine peel formula particles; each gram of the tangerine peel formula particles is equal to 6g of crude drug, and the tangerine peel formula particles have the infrared fingerprint spectrum which is shown in Figure 3. The preparation method can effectively ensure that each gram of the tangerine peel formula particles is equal to 6g 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 tangerine peel 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.Tangerine peel dispensing granule is a kind of of conventional Chinese medicine granule, at present tangerine peel dispensing granule mostly is traditional water and extracts, and perhaps extract water extraction behind the volatile oil, and different production unit is because production equipment is different with production technology, cause the product quality of different manufacturers inconsistent, there is difference in drug effect.Its quality standard is generally the discriminating of Hesperidin thin-layer qualitative and content of hesperidin is measured, 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 tangerine peel 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 tangerine peel 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 tangerine peel dispensing granule of the present invention contains suitable crude drug amount 6 grams; Hesperidin (C in the granule
28H
34O
15) content be not less than 1.0%; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer; At 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-1At the place characteristic absorption is also arranged;
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 tangerine peel dispensing granule of the present invention is:
After getting the chopping of raw material Pericarpium Citri Reticulatae, the 40%-70% ethanol that adds 5-15 times of weight portion of raw material Pericarpium Citri Reticulatae soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fried 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 Pericarpium Citri Reticulatae, extracts 0.5-3 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.05-1.10, and two liquid of boiling medicine are evaporated to relative density 1.10-1.15, merge two and fry in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; Pericarpium Citri Reticulatae Pericarpium Citri Reticulatae standard Infrared fingerprint spectra (Fig. 1) has following feature: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Alcoholic acid amount of adding or amount of water can be 6-7 times of weight portions 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: after getting the chopping of raw material Pericarpium Citri Reticulatae, 50% ethanol that adds 8 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1 hour, extracted 1.5 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1.5 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.08, two liquid of boiling medicine and is evaporated to relative density 1.12, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule.
Above-mentioned preparation method is preferably: after getting the chopping of raw material Pericarpium Citri Reticulatae, 45% ethanol that adds 10 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1.5 hours, extracted 2 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.09, two liquid of boiling medicine and is evaporated to relative density 1.11, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule.
Above-mentioned preparation method is preferably: after getting the chopping of raw material Pericarpium Citri Reticulatae, 60% ethanol that adds 6 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 0.75 hour, extracted 1 hour, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 2 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.14, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule.
The drying process with atomizing parameter is in the above-mentioned preparation method: 40 ℃-50 ℃ 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 tangerine peel dispensing granule of the present invention comprises one or more in the following method:
A. the method for quality control of Pericarpium Citri Reticulatae spray drying powder: the Pericarpium Citri Reticulatae 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; Pericarpium Citri Reticulatae spray drying powder standard Infrared fingerprint spectra (Fig. 2) is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1051cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1622cm
-1, acromion is 1732cm
-1At 2931cm
-1, 1419cm
-1, 1261cm
-1, 817cm
-1, 777cm
-1At the place characteristic absorption is also arranged;
B. the method for quality control of tangerine peel dispensing granule: tangerine peel 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; Tangerine peel dispensing granule standard Infrared fingerprint spectra (Fig. 3) is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-1At the place characteristic absorption is also arranged.
Pericarpium Citri Reticulatae 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: Pericarpium Citri Reticulatae Pericarpium Citri Reticulatae standard Infrared fingerprint spectra
Fig. 2: Pericarpium Citri Reticulatae spray drying powder standard Infrared fingerprint spectra
Fig. 3: tangerine peel dispensing granule standard Infrared fingerprint spectra
Fig. 4: contain the classical medicine of Pericarpium Citri Reticulatae decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram are compared
Fig. 5: contain Pericarpium Citri Reticulatae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram relatively
Fig. 6: tangerine peel dispensing granule and Pericarpium Citri Reticulatae medical material thin layer chromatography are relatively
Fig. 7: tangerine peel dispensing granule and Pericarpium Citri Reticulatae medical material 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 Hesperidin utilization comparative test of experimental example 1 granule of the present invention and Pericarpium Citri Reticulatae medical material
Get Pericarpium Citri Reticulatae decoction pieces 60 grams, extracted 30 minutes, leach medicinal liquid with 10 times of water gagings; 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.Measure item method according to middle content of hesperidin of Pharmacopoeia of the People's Republic of China version in 2005, measure Determination of Hesperidin Content in the concentrated solution, and the amount of Hesperidin in the calculating decocting liquid, above-mentioned test repeats to do 3 times with the Pericarpium Citri Reticulatae of different batches, record in the decocting liquid amount of Hesperidin and be followed successively by 0.100 gram, 0.110 gram and 0.108 restrains; Measure the content of hesperidin in three batches of tangerine peel dispensing granules, be followed successively by 1.06%, 1.00%, 1.11%, promptly the contained Hesperidin of 10 gram tangerine peel dispensing granules is respectively 0.106 gram, 0.100 gram, 0.111 gram.Illustrate that the amount of Hesperidin in the 10 gram tangerine peel dispensing granules is equivalent to the utilization of 60 gram Pericarpium Citri Reticulatae decoction pieces Hesperidin in decoction, the equivalent that 1 gram tangerine peel dispensing granule of the present invention is equivalent to 6 gram Pericarpium Citri Reticulatae medical materials is a science.
Experimental example 2 contains the classical medicine of Pericarpium Citri Reticulatae decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram is compared
Pericarpium Citri Reticulatae-Caulis Bambusae In Taenia medicine is to coming from " Medical Treasures of the Golden Chamber ".
Experiment purpose: research Pericarpium Citri Reticulatae-Caulis Bambusae In Taenia medicine is determined tangerine peel dispensing granule technology and normal reasonability to the similarities and differences that decoction pieces closes decocting liquid and granular recipe.
Experimental technique: get Pericarpium Citri Reticulatae decoction pieces, each 6g prescription of Caulis Bambusae In Taenia decoction pieces, the decocting method of pressing the decoction pieces decoction decocts preparation decoction pieces decocting liquid sample; Other gets Caulis Bambusae In Taenia decoction pieces 6g, and the decocting method of pressing the decoction pieces decoction decocts, and medicinal liquid suitably concentrates, and adds tangerine peel dispensing granule 1g 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 95.7%.It is consistent to prove that soup that granule of the present invention is joined and decoction pieces close the decocting liquid composition, and promptly 1g tangerine peel dispensing granule of the present invention is consistent with a 6g Pericarpium Citri Reticulatae decoction pieces fried composition, and equivalent and production technology that tangerine peel dispensing granule 1g of the present invention is equivalent to Pericarpium Citri Reticulatae decoction pieces 6g are rational.
Experimental example 3 contains Pericarpium Citri Reticulatae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram compares
Xiangsu San comes from " peaceful Huimin mixture office side ", and prescription is formed and comprised Pericarpium Citri Reticulatae, Rhizoma Cyperi, Folium Perillae, 4 flavour of a drug of Radix Glycyrrhizae Preparata; The effect expelling wind and cold pathogens, regulate the flow of vital energy and in.
Experiment purpose: the similarities and differences of research Xiangsu San decoction pieces decocting liquid and granular recipe, determine tangerine peel dispensing granule technology and normal reasonability.
Experimental technique: get 4 flavour of a drug prescriptions such as Pericarpium Citri Reticulatae by the Xiangsu San proportioning, the decocting method of pressing the decoction pieces decoction decocts preparation decoction pieces decocting liquid sample; In addition get other decoction pieces except that Pericarpium Citri Reticulatae respectively by Xiangsu San prescription proportioning, the decocting method of pressing the decoction pieces decoction decocts, and medicinal liquid suitably concentrates, and gets tangerine peel dispensing granule of the present invention by Xiangsu San prescription proportioning and equivalent relation and 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 95.2%.It is consistent to prove that soup that granule is joined and decoction pieces close the decocting liquid composition, and it is consistent with a Pericarpium Citri Reticulatae decoction pieces fried composition promptly to add tangerine peel dispensing granule of the present invention, and equivalent and production technology that tangerine peel dispensing granule 1g of the present invention is equivalent to Pericarpium Citri Reticulatae decoction pieces 6g are rational.
Experimental example 4
(1) tangerine peel dispensing granule and the comparative study of Pericarpium Citri Reticulatae medical material thin layer chromatography
Differentiate a thin layer chromatography test down according to middle Pericarpium Citri Reticulatae medical material of Pharmacopoeia of the People's Republic of China version in 2005, prepare sample with Pericarpium Citri Reticulatae medical material and tangerine peel dispensing granule of the present invention, measure, the gained result as shown in Figure 6, in the tangerine peel dispensing granule chromatograph, with the corresponding position of Pericarpium Citri Reticulatae medical material chromatograph on, show the speckle of same color.
(2) tangerine peel dispensing granule and Pericarpium Citri Reticulatae medical material thin-layer sample Infrared fingerprint spectra are relatively
Measure the Pericarpium Citri Reticulatae medical material of preparation in (1) and the thin-layer sample of tangerine peel dispensing granule with Fourier transform infrared spectrometer, its result as shown in Figure 7, the thin-layer sample Infrared fingerprint spectra peak shape of tangerine peel dispensing granule and Pericarpium Citri Reticulatae medical material, peak position, relative peak intensity basically identical.
The result proves that tangerine peel dispensing granule of the present invention is consistent with the Pericarpium Citri Reticulatae medicinal ingredient, 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: tangerine peel dispensing granule of the present invention
Get raw material Pericarpium Citri Reticulatae 100kg, chopping, 50% ethanol that adds 800kg soaked into 1 hour, extracted 1.5 hours, promptly one fried in shallow oil; One fries in shallow oil the back medicinal residues adds 800kg water, extracts 1.5 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.08, two liquid of boiling medicine and is evaporated to relative density 1.12, merges two and fries in shallow oil concentrated solution; Concentrated solution is 45 ℃ of preheatings, 180 ℃ 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, Pericarpium Citri Reticulatae spray drying powder 30kg; The Pericarpium Citri Reticulatae 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 tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; The gained Infrared fingerprint spectra specifically is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Embodiment 2: tangerine peel dispensing granule of the present invention
Get raw material Pericarpium Citri Reticulatae 100kg, chopping adds 1000kg45% ethanol and soaked into 1.5 hours, extracts 2 hours, promptly one fries in shallow oil; One fries in shallow oil the back medicinal residues adds 600kg water, extracts 1 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.09, two liquid of boiling medicine and is evaporated to relative density 1.11, merges two and fries in shallow oil concentrated solution; Concentrated solution is 50 ℃ 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, Pericarpium Citri Reticulatae spray drying powder 32kg; The adjuvant dextrin that in the Pericarpium Citri Reticulatae spray drying powder, adds 3.2kg; 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 tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; The gained Infrared fingerprint spectra specifically is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Embodiment 3: tangerine peel dispensing granule of the present invention
Get raw material Pericarpium Citri Reticulatae 100kg, chopping, 60% ethanol that adds 600kg soaked into 0.75 hour, extracted 1 hour, promptly one fried in shallow oil; One fries in shallow oil the back medicinal residues adds 1000kg water, extracts 2 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.14, merges two and fries in shallow oil 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, Pericarpium Citri Reticulatae spray drying powder 28kg; The adjuvant lactose that in the Pericarpium Citri Reticulatae spray drying powder, adds 5.6kg; 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 tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; The gained Infrared fingerprint spectra specifically is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Embodiment 4: tangerine peel dispensing granule of the present invention
Get raw material Pericarpium Citri Reticulatae 100kg, chopping adds 1300kg45% ethanol and soaked into 2 hours, extracts 1.5 hours, promptly one fries in shallow oil; One fries in shallow oil the back medicinal residues adds 700kg water, extracts 1 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.15, merges two and fries in shallow oil concentrated solution; Concentrated solution is 45 ℃ 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, Pericarpium Citri Reticulatae spray drying powder 31kg; The adjuvant dextrin that in the Pericarpium Citri Reticulatae spray drying powder, adds 2.5kg; At main pinch roller pressure is 4MPa, 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 130V, 20-60 order tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; The gained Infrared fingerprint spectra specifically is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Embodiment 5: tangerine peel dispensing granule of the present invention
Get raw material Pericarpium Citri Reticulatae 100kg, chopping, 60% ethanol that adds 700kg soaked into 1 hour, extracted 1.5 hours, promptly one fried 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; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.15, merges two and fries in shallow oil 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, Pericarpium Citri Reticulatae spray drying powder 29kg; The adjuvant lactose that in the Pericarpium Citri Reticulatae spray drying powder, adds 7kg; At main pinch roller pressure is 6MPa, 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 100V, 20-60 order tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; The gained Infrared fingerprint spectra specifically is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1At the place characteristic absorption is also arranged.
Embodiment 6: the method for quality control of the Pericarpium Citri Reticulatae spray drying powder of the present invention of embodiment 1 preparation
The method of quality control of Pericarpium Citri Reticulatae spray drying powder: the Pericarpium Citri Reticulatae 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 Pericarpium Citri Reticulatae spray drying powder is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1051cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1622cm
-1, acromion is 1732cm
-1At 2931cm
-1, 1419cm
-1, 1261cm
-1, 817cm
-1, 777cm
-1At the place characteristic absorption is also arranged.
Embodiment 7: the method for quality control of the tangerine peel dispensing granule of the present invention of embodiment 2 preparations
The method of quality control of tangerine peel dispensing granule: tangerine peel 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 tangerine peel dispensing granule is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-1At the place characteristic absorption is also arranged.
Embodiment 8: the method for quality control of the tangerine peel dispensing granule of the present invention of embodiment 3 preparations
A. the method for quality control of Pericarpium Citri Reticulatae spray drying powder: the Pericarpium Citri Reticulatae 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 Pericarpium Citri Reticulatae spray drying powder is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1051cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1622cm
-1, acromion is 1732cm
-1At 2931cm
-1, 1419cm
-1, 1261cm
-1, 817cm
-1, 777cm
-1At the place characteristic absorption is also arranged;
B. the method for quality control of tangerine peel dispensing granule: tangerine peel 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 tangerine peel dispensing granule is characterized as: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-1At the place characteristic absorption is also arranged.
Claims (12)
1. a tangerine peel dispensing granule is characterized in that the every gram of this granule contains suitable crude drug amount 6 grams; Determination of Hesperidin Content is not less than 1.0% in the granule; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer, at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-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, tangerine peel dispensing granule is prepared from by following method:
After getting the chopping of raw material Pericarpium Citri Reticulatae, the 40%-70% ethanol that adds 5-15 times of weight portion of raw material Pericarpium Citri Reticulatae soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fried 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 Pericarpium Citri Reticulatae, extracts 0.5-3 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.05-1.10, and two liquid of boiling medicine are evaporated to relative density 1.10-1.15, merge two and fry in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule; Wherein the raw material Pericarpium Citri Reticulatae 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; Pericarpium Citri Reticulatae Pericarpium Citri Reticulatae standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1There is characteristic absorption at the place.
2. tangerine peel dispensing granule as claimed in claim 1, the Infrared fingerprint spectra that it is characterized in that this tangerine peel dispensing granule are to reach Infrared fingerprint spectra more than 90% with its dependency.
3. tangerine peel dispensing granule as claimed in claim 1 or 2 is characterized in that wherein adding alcoholic acid amount in the preparation method or amount of water is a 6-7 times of weight portion, 8-12 times of weight portion or 13-14 times of weight portion.
4. tangerine peel dispensing granule as claimed in claim 1 or 2 is characterized in that wherein extraction time is 1-1.5 hour or 2-2.5 hour in the preparation method.
5. tangerine peel dispensing granule as claimed in claim 3 is characterized in that wherein extraction time is 1-1.5 hour or 2-2.5 hour in the preparation method.
6. tangerine peel dispensing granule as claimed in claim 1 or 2 is characterized in that wherein tangerine peel dispensing granule is by a kind of being prepared from the following method:
After getting the chopping of raw material Pericarpium Citri Reticulatae, 50% ethanol that adds 8 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1 hour, extracted 1.5 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1.5 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.08, two liquid of boiling medicine and is evaporated to relative density 1.12, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Or after getting the chopping of raw material Pericarpium Citri Reticulatae, 45% ethanol that adds 10 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1.5 hours, extracted 2 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.09, two liquid of boiling medicine and is evaporated to relative density 1.11, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Or after getting the chopping of raw material Pericarpium Citri Reticulatae, 60% ethanol that adds 6 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 0.75 hour, extracted 1 hour, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 2 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.14, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule.
7. the preparation method of tangerine peel dispensing granule as claimed in claim 1 or 2 is characterized in that this method is: after getting the chopping of raw material Pericarpium Citri Reticulatae, the 40%-70% ethanol that adds 5-15 times of weight portion of raw material Pericarpium Citri Reticulatae soaked into 0.5-2 hour, extracted 0.5-3 hour, promptly one fried 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 Pericarpium Citri Reticulatae, extracts 0.5-3 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.05-1.10, and two liquid of boiling medicine are evaporated to relative density 1.10-1.15, merge two and fry in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Wherein the raw material Pericarpium Citri Reticulatae 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; Pericarpium Citri Reticulatae Pericarpium Citri Reticulatae standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1055cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1637cm
-1, acromion is 1739cm
-1At 2928cm
-1, 1418cm
-1, 1371cm
-1, 1269cm
-1, 816cm
-1There is characteristic absorption at the place.
8. the preparation method of tangerine peel dispensing granule as claimed in claim 7 is characterized in that adding alcoholic acid amount in this method or amount of water is a 6-7 times of weight portion, 8-12 times of weight portion or 13-14 times of weight portion.
9. the preparation method of tangerine peel dispensing granule as claimed in claim 7 is characterized in that extraction time is 1-1.5 hour or 2-2.5 hour in this method.
10. the preparation method of tangerine peel dispensing granule as claimed in claim 8 is characterized in that extraction time is 1-1.5 hour or 2-2.5 hour in this method.
11. the preparation method of tangerine peel dispensing granule as claimed in claim 7 is characterized in that this method is a kind of in the following method:
After getting the chopping of raw material Pericarpium Citri Reticulatae, 50% ethanol that adds 8 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1 hour, extracted 1.5 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 8 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1.5 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.08, two liquid of boiling medicine and is evaporated to relative density 1.12, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Or after getting the chopping of raw material Pericarpium Citri Reticulatae, 45% ethanol that adds 10 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 1.5 hours, extracted 2 hours, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 6 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 1 hour, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.09, two liquid of boiling medicine and is evaporated to relative density 1.11, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule;
Or after getting the chopping of raw material Pericarpium Citri Reticulatae, 60% ethanol that adds 6 times of weight portions of raw material Pericarpium Citri Reticulatae soaked into 0.75 hour, extracted 1 hour, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add 10 times of weight portions of raw material Pericarpium Citri Reticulatae, extracts 2 hours, promptly two fries in shallow oil; One liquid of boiling medicine is evaporated to relative density 1.06, two liquid of boiling medicine and is evaporated to relative density 1.14, merges two and fries in shallow oil concentrated solution; The concentrated solution spray drying gets the Pericarpium Citri Reticulatae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Pericarpium Citri Reticulatae spray drying powder, tangerine peel dispensing granule.
12. the quality determining method of tangerine peel dispensing granule as claimed in claim 1 or 2 is characterized in that this quality determining method comprises one or more in the following method:
A. the quality determining method of Pericarpium Citri Reticulatae spray drying powder: the Pericarpium Citri Reticulatae 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; Pericarpium Citri Reticulatae spray drying powder standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1051cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1622cm
-1, acromion is 1732cm
-1At 2931cm
-1, 1419cm
-1, 1261cm
-1, 817cm
-1, 777cm
-1There is characteristic absorption at the place;
B. the quality determining method of tangerine peel dispensing granule: tangerine peel 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; Tangerine peel dispensing granule standard Infrared fingerprint spectra is: at 1200cm
-1-800cm
-1Between a broad peak is arranged is main strong peak, peak position is 1052cm
-1At 2000cm
-1-1500cm
-1Between time strong peak of a broad is arranged, peak position is 1618cm
-1, acromion is 1741cm
-1At 2930cm
-1, 1420cm
-1, 1259cm
-1, 817cm
-1, 778cm
-1There is characteristic absorption at the place.
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| CN101852730A (en) * | 2010-03-25 | 2010-10-06 | 丽珠集团利民制药厂 | Infrared spectrum detection method of ginseng and astragalus injection liquid |
| CN103033486B (en) * | 2012-11-23 | 2015-04-22 | 广东药学院 | Method for near infrared spectrum monitoring of quality of pericarpium citri reticulatae and citrus chachiensis hortorum medicinal materials |
| CN103055128A (en) * | 2013-02-01 | 2013-04-24 | 山东华信制药集团股份有限公司 | Preparation process of stomach invigorating and digestion helping tablet |
| CN106074796B (en) * | 2016-06-20 | 2017-08-22 | 广东一方制药有限公司 | A kind of dried orange peel particle and its Chinese medicine preparation |
| CN109091563A (en) * | 2018-11-13 | 2018-12-28 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of preparation method and its anti-trioxypurine application of dried orange peel extracts |
| CN114113435A (en) * | 2021-11-19 | 2022-03-01 | 华润三九（雅安）药业有限公司 | Method for constructing characteristic spectrum of dried orange peel medicinal material and preparation |
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| CN1584586A (en) * | 2004-05-26 | 2005-02-23 | 江西江中药业股份有限公司 | Quality control of Jianweixiaoshi tablets for promotnig digest |
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| CN1584586A (en) * | 2004-05-26 | 2005-02-23 | 江西江中药业股份有限公司 | Quality control of Jianweixiaoshi tablets for promotnig digest |
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