CN101474352A - Ophiopogon root dispensing granule as well as preparation method and quality control method thereof - Google Patents
Ophiopogon root dispensing granule as well as preparation method and quality control method thereof Download PDFInfo
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- CN101474352A CN101474352A CN 200810184565 CN200810184565A CN101474352A CN 101474352 A CN101474352 A CN 101474352A CN 200810184565 CN200810184565 CN 200810184565 CN 200810184565 A CN200810184565 A CN 200810184565A CN 101474352 A CN101474352 A CN 101474352A
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Abstract
The invention discloses a dwarf lilyturf root dispensing granule as well as a preparation method thereof and a quality control method thereof, the dispensing granule takes dwarf lilyturf root pieces as raw materials and is subjected to process flows like extraction twice with water, reduced pressure concentration, spray and drying to obtain the dwarf lilyturf root dispensing granule, the lilyturf root dispensing granule per gram is equivalent to 3-5 grams of crude drug, both the lilyturf root pieces and the dwarf lilyturf root dispensing granule use infrared fingerprint to perform an quality authentication. The inventive dwarf lilyturf root dispensing granule has integral, advanced production processes and controllable quality control criteria with strong specificity, the processes are advanced and can be realized, detection methods to which the quality criteria relates are scientific, advanced, fast and convenient with strong operability. As proved by numerous experiments, the decoction composed by the lilyturf root dispensing granule of the invention has the same ingredients as the pieces mixedly decocted liquor, the prescription granule process of bulk composition is realized and the rationality of the process of the invention is proved; furthermore, the invention applies the technology of infrared fingerprint spectra to the quality control of the traditional Chinese medicine, thus the primary problem in the macro quality control of the traditional Chinese medicine---the authenticity appraisal of the traditional Chinese medicine is instantly solved.
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 Radix Ophiopogonis 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.At present Chinese medicinal granule mostly is traditional water and extracts, and perhaps extracts water extraction behind the volatile oil, and different production unit causes the product quality of different manufacturers inconsistent because production equipment is different with production technology, and there is difference in drug effect.The specificity of its quality standard is limit by certain test conditions and scope, lacks other due quality informations of product, and present standard can't be judged the quality good or not and the overall picture of Chinese medicinal 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 Radix Ophiopogonis of 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 suitable crude drug amount of the every gram of granule Radix Ophiopogonis of the present invention 3-5 gram, the Infrared fingerprint spectra of this granule such as Fig. 1.Radix Ophiopogonis of the present invention, the preparation method of granule comprised: get decoction pieces Radix Ophiopogonis, with twice of water extraction; Wherein Radix Ophiopogonis, decoction pieces adopted Infrared fingerprint spectra to carry out quality discrimination, Radix Ophiopogonis decoction pieces standard Infrared fingerprint spectra such as Fig. 2.
Radix Ophiopogonis of the present invention, the preparation method of granule comprised the steps: to get decoction pieces Radix Ophiopogonis, added the water of 5-15 times of weight portion, extracted 0.5-3 hour, promptly one fried in shallow oil; One fries in shallow oil the water that the back medicinal residues add decoction pieces 5-15 times weight portion Radix Ophiopogonis, extracts 0.5-3 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis.
Radix Ophiopogonis of the present invention, the preparation method of granule was preferably as follows step: get decoction pieces Radix Ophiopogonis, add the water of 8 times of weight portions, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 7 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 1.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.05-1.10; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis.
Radix Ophiopogonis of the present invention, the preparation method of granule was preferably as follows step: get decoction pieces Radix Ophiopogonis, add the water of 10 times of weight portions, 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 decoction pieces Radix Ophiopogonis, extracts 1 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.05; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis.
Radix Ophiopogonis of the present invention, the preparation method of granule was preferably as follows step: get decoction pieces Radix Ophiopogonis, add the water of 14 times of weight portions, extracted 2.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 11 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 2.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.10-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis.
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/mins; Feed voltage: 100-150V; Granular size: 20-60 order.
Radix Ophiopogonis of the present invention, the method for quality control of granule comprised the steps: that Radix Ophiopogonis, granule adopted 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; Radix Ophiopogonis the granule Infrared fingerprint spectra as shown in Figure 1, have following feature: at 1022cm
-1Absorption maximum is arranged, and it is stepped to locate absworption peak, its absorption is 1022cm from high to low
-1, 1079cm
-1, 1155cm
-1At 2928cm
-1, 1664cm
-1, 1421cm
-1, 817cm
-1There is characteristic absorption at the place.
Described in Radix Ophiopogonis of the present invention granule preparation method Radix Ophiopogonis decoction pieces method of quality control comprise the steps: that Radix Ophiopogonis, decoction pieces was the certified products that meet a regulation of Pharmacopoeia of the People's Republic of China version in 2005; Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis decoction pieces Infrared fingerprint spectra as shown in Figure 2, have following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place.
Infrared fingerprint spectra wherein of the present invention can be to reach Infrared fingerprint spectra more than 90% with its dependency.
Description of drawings:
Fig. 1: Radix Ophiopogonis granule Infrared fingerprint spectra;
Fig. 2: Radix Ophiopogonis decoction pieces Radix Ophiopogonis Infrared fingerprint spectra;
Fig. 3: Radix Ophiopogonis granule and decoction pieces thin layer chromatography comparison Radix Ophiopogonis;
Fig. 4: Radix Ophiopogonis granule and decoction pieces thin-layer sample Infrared fingerprint spectra comparison Radix Ophiopogonis;
Fig. 5: contain Radix Ophiopogonis classics side's decoction pieces decocting liquid and soup that granule is joined Radix Ophiopogonis " whole part " infrared spectrogram relatively.
Tuber of dwarf lilyturf of the present invention granule have complete, advanced production technology and specificity strong, Controlled quality control standard, technology advanced person can realize, the detection method that quality standard relates to Science, advanced person, quick, workable. By great many of experiments, contrasted the warp that contains the medicine materical crude slice tuber of dwarf lilyturf Allusion quotation side's medicine materical crude slice closes decocting liquid and soup that granule the is joined tuber of dwarf lilyturf of the present invention " full composition " infrared spectrogram, and is right Compared tuber of dwarf lilyturf of the present invention granule and the tuber of dwarf lilyturf medicine materical crude slice thin-layer chromatogram, contrasted granule and the wheat tuber of dwarf lilyturf Winter medicine materical crude slice thin-layer sample infrared finger print atlas, the result show the classical side's medicine materical crude slice that contains the medicine materical crude slice tuber of dwarf lilyturf close decocting liquid with Tuber of dwarf lilyturf of the present invention, granule was joined soup infrared finger print atlas peak shape, peak position, Relative Peak intensity basic one Cause, namely the tuber of dwarf lilyturf of the present invention soup that granule is joined and medicine materical crude slice to close the decocting liquid composition suitable, and wheat of the present invention The infrared finger print atlas peak shape of winter granule and medicine materical crude slice thin-layer sample, peak position, Relative Peak intensity basic one Cause, so tuber of dwarf lilyturf of the present invention, granule was realized the technology of full component prescription particle proving worker of the present invention The reasonability of skill; And the present invention is applied to the quality control of Chinese medicine with infrared spectrum technology, and this is a kind of Innovation on the thinking, this not only meets traditional chinese medicine about the theory of " monarch, minister, help, make ", Also given prominence to the group effect of Chinese medicine, simultaneously the problem of complexity oversimplified, certain Chinese medicine as one Integral body is observed its " fingerprint ", thereby has solved rapidly a head in the control of Chinese medicine macroscopic quality Want problem---the evaluation of the Chinese medicine true and false.
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
Experimental example 1
(1) tuber of dwarf lilyturf granule and the medicine materical crude slice thin-layer chromatography comparison tuber of dwarf lilyturf
According to the middle discriminating tuber of dwarf lilyturf lower thin layer look of Pharmacopoeia of the People's Republic of China version in 2005 Spectrometry test, with the tuber of dwarf lilyturf medicine materical crude slice and tuber of dwarf lilyturf of the present invention granule prepare sample, measure institute The result as shown in Figure 3, in the tuber of dwarf lilyturf granule chromatogram, with the tuber of dwarf lilyturf medicine materical crude slice chromatogram corresponding On the position, the spot of aobvious same color.
(2) tuber of dwarf lilyturf granule and the medicine materical crude slice thin-layer sample infrared finger print atlas comparison tuber of dwarf lilyturf
With FTIS measure preparation in (1) the tuber of dwarf lilyturf medicine materical crude slice and the tuber of dwarf lilyturf prescription The grain thin-layer sample, its result as shown in Figure 4, the tuber of dwarf lilyturf granule and the tuber of dwarf lilyturf medicine materical crude slice thin layer Sample infrared finger print atlas peak shape, peak position, Relative Peak intensity are basically identical.
The result proves, tuber of dwarf lilyturf of the present invention granule with the tuber of dwarf lilyturf medicine materical crude slice composition consistent, technology of the present invention is to close Reason.
Experimental example 2 contains classics side's medicine materical crude slice decocting liquid and soup that granule the is joined tuber of dwarf lilyturf " full composition " infrared spectrogram comparative experiments tuber of dwarf lilyturf
Modified Pulse-Restoring Decoction comes from " the warm disease bar is distinguished ", and prescription forms and comprises honey-fried licorice root, glutinous rehmannia, the root of herbaceous peony, wheat Winter, 5 flavour of a drug of Semen sesami nigrum; The effect tonifying yin.
1, experiment purpose: the similarities and differences of research Modified Pulse-Restoring Decoction medicine materical crude slice decocting liquid and granular recipe, determine the tuber of dwarf lilyturf The reasonability of granule technology and equivalent.
2, experimental technique: get 5 flavour of a drug prescriptions such as the tuber of dwarf lilyturf by Modified Pulse-Restoring Decoction prescription proportioning, press medicine materical crude slice The decocting method of decoction decocts preparation medicine materical crude slice decocting liquid sample; Get respectively by Modified Pulse-Restoring Decoction prescription proportioning in addition and remove Other medicine materical crude slice that the tuber of dwarf lilyturf is outer, the decocting method of pressing the medicine materical crude slice decoction decocts, and soup suitably concentrates, and is multiple by plus-minus Arteries and veins soup recipe proportioning and equivalent relation are got in the granule adding tuber of dwarf lilyturf concentrated medicament, are stirred to fully molten Separate preparation granular recipe sample; Drink respectively sheet decocting liquid sample, the granular recipe sample carries out infrared spectrum Detect.
3, testing conditions: instrument is FTIS, and measurement range is 4000 cm-1-400cm
-1, DTGS detector, resolution ratio 4cm-1, scanning times 16 times, in the scanning process constantly Deduction water and carbon dioxide disturb, and envionmental humidity is lower than 60%, and the KBr direct compression process is examined Survey.
4, 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 95.99%.Prove Radix Ophiopogonis of the present invention soup that granule is joined to close the decocting liquid composition consistent with decoction pieces, it is consistent with decoction pieces institute Radix Ophiopogonis fried composition promptly to add Radix Ophiopogonis of the present invention granule, Radix Ophiopogonis of the present invention granule 1g to be equivalent to equivalent and the production technology of decoction pieces 3-5g Radix Ophiopogonis be rational.
Following embodiment all can realize the effect of above-mentioned experimental example, and required decoction pieces employing Radix Ophiopogonis Infrared fingerprint spectra is carried out quality discrimination among the following embodiment, meet in the technique scheme Radix Ophiopogonis decoction pieces the standard Infrared fingerprint spectra; Following embodiment makes Radix Ophiopogonis, granule adopted Infrared fingerprint spectra to carry out quality discrimination, meet in the technique scheme Radix Ophiopogonis granule Infrared fingerprint spectra; The every gram of granule Radix Ophiopogonis described in the following embodiment contains suitable crude drug amount 3-5 gram.
The specific embodiment
Embodiment 1: Radix Ophiopogonis granule
Get decoction pieces 100kg Radix Ophiopogonis, add the water of 800kg, extracted 2 hours, promptly one fry 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; Merge two liquid of boiling medicine, be evaporated to relative density 1.05-1.10; 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, Radix Ophiopogonis spray drying powder; The adjuvant dextrin that in the Radix Ophiopogonis spray drying powder, adds himself weight portion 0-5%; Radix Ophiopogonis, spray drying powder was 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 dry granulation under the condition of 120V, 20-60 purpose granule Radix Ophiopogonis, suitable crude drug amount 5 grams of the every gram of granule Radix Ophiopogonis.
Embodiment 2: Radix Ophiopogonis granule
Get decoction pieces 100kg Radix Ophiopogonis, add the water of 1000kg, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 600kg water, extracts 1 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to relative density 1.00-1.05; 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, Radix Ophiopogonis spray drying powder; The adjuvant dextrin that in the Radix Ophiopogonis spray drying powder, adds himself weight portion 5-15%; 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 purpose granule Radix Ophiopogonis, suitable crude drug amount 4 grams of the every gram of granule Radix Ophiopogonis;
Wherein said Radix Ophiopogonis, the method for quality control of decoction pieces comprised the steps: that Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis decoction pieces Infrared fingerprint spectra as shown in Figure 2, have following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place.
Embodiment 3: Radix Ophiopogonis granule
Get decoction pieces 100kg Radix Ophiopogonis, add the water of 1400kg, extracted 2.5 hours, promptly one fry in shallow oil; One fries in shallow oil the back medicinal residues adds 1100kg water, extracts 2.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to relative density 1.10-1.15; 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, Radix Ophiopogonis spray drying powder; The lactose that in the Radix Ophiopogonis spray drying powder, adds himself weight portion 15-25%; 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 purpose granule Radix Ophiopogonis, suitable crude drug amount 10 grams of per 3 grams of granule Radix Ophiopogonis;
The method of quality control of gained granule Radix Ophiopogonis comprises the steps: to adopt 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; Radix Ophiopogonis the granule Infrared fingerprint spectra as shown in Figure 1, have following feature: at 1022cm
-1Absorption maximum is arranged, and it is stepped to locate absworption peak, its absorption is 1022cm from high to low
-1, 1079cm
-1, 1155cm
-1At 2928cm
-1, 1664cm
-1, 1421cm
-1, 817cm
-1There is characteristic absorption at the place.
Claims (10)
1, a kind of Radix Ophiopogonis granule, it is characterized in that the suitable crude drug amount of the described every gram of granule Radix Ophiopogonis 3-5 gram.
2, Radix Ophiopogonis as claimed in claim 1 granule, it is characterized in that suitable crude drug amount 10 grams of per 3 grams of described granule Radix Ophiopogonis.
3, a kind of Radix Ophiopogonis granule, it is characterized in that this, granule Infrared fingerprint spectra had following feature Radix Ophiopogonis: adopt Fourier transform infrared spectrometer to measure, at 1022cm
-1Absorption maximum is arranged, and it is stepped to locate absworption peak, its absorption is 1022cm from high to low
-1, 1079cm
-1, 1155cm
-1At 2928cm
-1, 1664cm
-1, 1421cm
-1, 817cm
-1There is characteristic absorption at the place.
4, as claim 1 or 2 arbitrary described Radix Ophiopogonis granule, it is characterized in that the Infrared fingerprint spectra of this granule has following feature: at 1022cm
-1Absorption maximum is arranged, and it is stepped to locate absworption peak, its absorption is 1022cm from high to low
-1, 1079cm
-1, 1155cm
-1At 2928cm
-1, 1664cm
-1, 1421cm
-1, 817cm
-1There is characteristic absorption at the place.
5, a kind of Radix Ophiopogonis granule preparation method, it is characterized in that this method comprises a kind of in the following method:
Get decoction pieces Radix Ophiopogonis, add the water of 5-15 times of weight portion, extracted 0.5-3 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add decoction pieces 5-15 times weight portion Radix Ophiopogonis, extracts 0.5-3 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, Radix Ophiopogonis granule;
Or get decoction pieces Radix Ophiopogonis, and add the water of 8 times of weight portions, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 7 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 1.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.05-1.10; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, Radix Ophiopogonis granule;
Or get decoction pieces Radix Ophiopogonis, and add the water of 10 times of weight portions, 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 decoction pieces Radix Ophiopogonis, extracts 1 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.05; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, Radix Ophiopogonis granule;
Or get decoction pieces Radix Ophiopogonis, and add the water of 14 times of weight portions, extracted 2.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 11 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 2.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.10-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, Radix Ophiopogonis granule.
6, Radix Ophiopogonis as claimed in claim 5 granule preparation method, it is characterized in that wherein said drying process with atomizing parameter is: 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; Wherein said granulation parameter is: main pinch roller pressure: 4-6MPa; Side pressure wheel pressure: 0.4-0.6MPa; The speed of mainshaft: 300-500 rev/mins; Feed voltage: 100-150V; Granular size: 20-60 order.
7, Radix Ophiopogonis as claimed in claim 5 granule preparation method, it is characterized in that wherein Radix Ophiopogonis, the quality discrimination of decoction pieces Infrared fingerprint spectra was: 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; Radix Ophiopogonis, the Infrared fingerprint spectra of decoction pieces had following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place.
8, a kind of Radix Ophiopogonis granule preparation method, it is characterized in that this method comprises a kind of in the following method:
Get decoction pieces Radix Ophiopogonis, add the water of 5-15 times of weight portion, extracted 0.5-3 hour, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add decoction pieces 5-15 times weight portion Radix Ophiopogonis, extracts 0.5-3 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis; Wherein Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis, the Infrared fingerprint spectra of decoction pieces had following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place;
Or get decoction pieces Radix Ophiopogonis, and add the water of 8 times of weight portions, extracted 2 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 7 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 1.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.05-1.10; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis; Wherein Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis, the Infrared fingerprint spectra of decoction pieces had following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place;
Or get decoction pieces Radix Ophiopogonis, and add the water of 10 times of weight portions, 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 decoction pieces Radix Ophiopogonis, extracts 1 hour, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.00-1.05; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis; Wherein Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis, the Infrared fingerprint spectra of decoction pieces had following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place;
Or get decoction pieces Radix Ophiopogonis, and add the water of 14 times of weight portions, extracted 2.5 hours, promptly one fry in shallow oil; One fries in shallow oil the water that the back medicinal residues add 11 times of weight portions of decoction pieces Radix Ophiopogonis, extracts 2.5 hours, promptly two fries in shallow oil; Merge two liquid of boiling medicine, be evaporated to the concentrated solution of relative density 1.10-1.15; The concentrated solution spray drying gets spray drying powder Radix Ophiopogonis; Spray drying powder was directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Ophiopogonis spray drying powder Radix Ophiopogonis, 20-60 purpose granule Radix Ophiopogonis; Wherein Radix Ophiopogonis, decoction pieces adopted 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; Radix Ophiopogonis, the Infrared fingerprint spectra of decoction pieces had following feature: at 1027cm
-1Absorption maximum is arranged, and there are two more weak absworption peaks both sides; At 2933cm
-1, 1656cm
-1, 1455cm
-1, 1270cm
-1, 819cm
-1There is characteristic absorption at the place.
9, Radix Ophiopogonis as claimed in claim 8 granule preparation method, it is characterized in that wherein said drying process with atomizing parameter is: 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; Wherein said granulation parameter is: main pinch roller pressure: 4-6MPa; Side pressure wheel pressure: 0.4-0.6MPa; The speed of mainshaft: 300-500 rev/mins; Feed voltage: 100-150V; Granular size: 20-60 order.
10, as claim 3,4 arbitrary described Radix Ophiopogonis granule, it is characterized in that wherein said Infrared fingerprint spectra testing conditions 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.
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| CN 200810184564 Pending CN101474333A (en) | 2007-12-18 | 2008-12-17 | Yam dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184559 Active CN101518577B (en) | 2007-12-18 | 2008-12-17 | Fried bitter almond formula granules as well as preparation method and quality control method thereof |
| CN 200810184568 Active CN101474232B (en) | 2007-12-18 | 2008-12-17 | White atractylodes rhizome dispensing granule as well as preparation method and quality control method |
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| CN 200810184582 Active CN101474265B (en) | 2007-12-18 | 2008-12-17 | Coptis root dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184581 Active CN101474273B (en) | 2007-12-18 | 2008-12-17 | Stir-fried fructus gardenia dispensing granule as well as preparation method and quality control method thereof |
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