CN101474244A - Honey-fried licorice root dispensing granule as well as preparation method and quality control method - Google Patents
Honey-fried licorice root dispensing granule as well as preparation method and quality control method Download PDFInfo
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- CN101474244A CN101474244A CN 200810184583 CN200810184583A CN101474244A CN 101474244 A CN101474244 A CN 101474244A CN 200810184583 CN200810184583 CN 200810184583 CN 200810184583 A CN200810184583 A CN 200810184583A CN 101474244 A CN101474244 A CN 101474244A
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Abstract
The invention discloses a honey-fried licorice root formula particle and preparation and quality control methods thereof. The formula particle uses honey-fried licorice root decoction pieces as raw materials, and the decoction pieces are processed by the technological processes of twice water extraction, vaccum concentration, sponging drying and the like to gain the honey-fried licorice root formula particle; and one gram of honey-fried licorice root formula particle is equivalent to 3 to 5 grams of crude medicines, the content of glycyrrhizic acid in the formula particle is not lower than 2.0 percent, and the quality of the honey-fried licorice root decoction pieces and the honey-fried licorice root formula particle is respectively discriminated by the infrared fingerprint spectra. The honey-fried licorice root formula particle of the invention has the advantages of integrated and advanced production process, specific and controllable quality control standard and advanced and realizable process, and a test method related to the quality standard is scientific, advanced, fast and highly operable. Proved by a lot of experiments, the ingredient of a herbal decoction prepared by the honey-fried licorice root formula particle of the invention is equivalent to the ingredient of the mixed simmer liquid of the honey-fried licorice root contained classical formula, the full ingredient formula particle process is achieved, and the process of the invention is proved to be reasonable; and the invention applies the infrared spectroscopy technology to the quality control of the traditional Chinese medicines, thereby fast solving the principal problem of traditional Chinese medicine truth discrimination in the macroscopic quality control of the traditional Chinese medicines.
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 honey-fried licorice root 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.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 honey-fried licorice root 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 suitable crude drug amount of the every gram of honey-fried licorice root dispensing granule of the present invention 3-5 gram, the Infrared fingerprint spectra of this granule such as Fig. 1.The preparation method of honey-fried licorice root dispensing granule of the present invention comprises: get the Radix Glycyrrhizae Preparata decoction pieces, use twice of water extraction; Wherein the Radix Glycyrrhizae Preparata decoction pieces adopts Infrared fingerprint spectra to carry out quality discrimination, Radix Glycyrrhizae Preparata decoction pieces standard Infrared fingerprint spectra such as Fig. 2.The content of glycyrrhizic acid is not less than 2.0% in the honey-fried licorice root dispensing granule,
The preparation method of honey-fried licorice root dispensing granule of the present invention comprises the steps: to get the Radix Glycyrrhizae Preparata decoction pieces, adds the water of 5-15 times of weight portion, extracts 0.5-3 hour, promptly one fries in shallow oil; One fries in shallow oil the water that the back medicinal residues add 5-15 times of weight portion of Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule.
The preparation method of honey-fried licorice root dispensing granule of the present invention is preferably as follows step: get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule.
The preparation method of honey-fried licorice root dispensing granule of the present invention is preferably as follows step: get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule.
The preparation method of honey-fried licorice root dispensing granule of the present invention is preferably as follows step: get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root 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/mins; Feed voltage: 100-150V; Granular size: 20-60 order.
The method of quality control of honey-fried licorice root dispensing granule of the present invention comprises the steps: that honey-fried licorice root dispensing granule 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 honey-fried licorice root dispensing granule Infrared fingerprint spectra has following feature: as shown in Figure 1 at 1610cm
-1, 1054cm
-1Two strong absworption peaks, wherein 1054cm are arranged
-1Place's absorption peak strength maximum; At 2929cm
-1, 1419cm
-1, 1244cm
-1, 778cm
-1There is characteristic absorption at the place.
The method of quality control of the Radix Glycyrrhizae Preparata decoction pieces described in the honey-fried licorice root dispensing granule preparation method of the present invention comprises the steps: that the Radix Glycyrrhizae Preparata decoction pieces is the certified products that meet a regulation of Pharmacopoeia of the People's Republic of China version in 2005; The Radix Glycyrrhizae Preparata decoction pieces 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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: as shown in Figure 2 at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-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: the Infrared fingerprint spectra of honey-fried licorice root dispensing granule;
Fig. 2: the Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces Radix Et Rhizoma Glycyrrhizae Praeparata CumMelle;
Fig. 3: honey-fried licorice root dispensing granule and Radix Glycyrrhizae Preparata decoction pieces thin layer chromatography are relatively;
Fig. 4: honey-fried licorice root dispensing granule and Radix Glycyrrhizae Preparata decoction pieces thin-layer sample Infrared fingerprint spectra are relatively;
Fig. 5: contain Radix Glycyrrhizae Preparata classics side decoction pieces decocting liquid and soup that honey-fried licorice root dispensing granule is joined " whole part " infrared spectrogram relatively.
Complete, advanced production technology that honey-fried licorice root dispensing granule of the present invention has 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 honey-fried licorice root of the present invention and joined The utilization of index components in side's particle and the honey-fried licorice root medicine materical crude slice has contrasted the classics side's drink that contains the honey-fried licorice root medicine materical crude slice Sheet closes decocting liquid and soup that honey-fried licorice root dispensing granule of the present invention is joined " full composition " infrared spectrogram, has contrasted Honey-fried licorice root dispensing granule of the present invention and honey-fried licorice root medicine materical crude slice thin-layer chromatogram, contrasted honey-fried licorice root dispensing granule with Honey-fried licorice root medicine materical crude slice thin-layer sample infrared finger print atlas, the result shows that the classical side's medicine materical crude slice that contains the honey-fried licorice root medicine materical crude slice closes It is strong that decocting liquid and honey-fried licorice root dispensing granule of the present invention are joined soup infrared finger print atlas peak shape, peak position, Relative Peak Spend basically identically, namely to close the decocting liquid composition suitable for soup that honey-fried licorice root dispensing granule of the present invention is joined and medicine materical crude slice, and And the infrared finger print atlas peak shape of honey-fried licorice root dispensing granule of the present invention and medicine materical crude slice thin-layer sample, peak position, relative Peak intensity is basically identical, so honey-fried licorice root dispensing granule of the present invention has been realized the worker of full component prescription particle Plant, prove the reasonability of technology of the present invention; And the present invention is applied to infrared spectrum technology the matter of Chinese medicine Amount control, this is the innovation on a kind of thinking, this not only meet traditional chinese medicine about " monarch, minister, Assistant, make " theory, also given prominence to the group effect of Chinese medicine, simultaneously the problem of complexity is oversimplified, Certain Chinese medicine is done as a whole, observes its " fingerprint ", thereby has solved rapidly Chinese medicine macroscopic view matter Matter of utmost importance---the evaluation of the Chinese medicine true and false in the amount control.
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
Experimental example 1
(1) honey-fried licorice root dispensing granule and the comparative experiments of honey-fried licorice root medicine materical crude slice thin-layer chromatography
Differentiate a lower thin layer according to middle honey-fried licorice root of Pharmacopoeia of the People's Republic of China version in 2005 The chromatography test prepares sample with honey-fried licorice root medicine materical crude slice and honey-fried licorice root dispensing granule of the present invention, surveys Fixed, acquired results as shown in Figure 3, in the honey-fried licorice root dispensing granule chromatogram, with the honey-fried licorice root medicine materical crude slice On the corresponding position of chromatogram, the spot of aobvious same color.
(2) honey-fried licorice root dispensing granule and the comparative experiments of honey-fried licorice root medicine materical crude slice thin-layer sample infrared finger print atlas
Measure honey-fried licorice root medicine materical crude slice and the honey-fried licorice root of preparation in (1) joins with FTIS The thin-layer sample of side's particle, its result as shown in Figure 4, honey-fried licorice root dispensing granule and honey-fried licorice root drink The thin-layer sample infrared finger print atlas peak shape of sheet, peak position, Relative Peak intensity are basically identical.
The result proves that honey-fried licorice root dispensing granule of the present invention is consistent with honey-fried licorice root medicine materical crude slice composition, technology of the present invention Rational.
The utilization contrast experiment of index components in experimental example 2 honey-fried licorice root dispensing granules and the honey-fried licorice root medicine materical crude slice
Get honey-fried licorice root medicine materical crude slice 50 grams, extracted 30 minutes with 10 times of water gagings, leach soup; The dregs of a decoction add water 8 Doubly amount was extracted 20 minutes, leached soup, merged two liquid of boiling medicine, and suitably concentrated and to get concentrate 100 in the least Rise. Measure item method according to middle glycyrrhizic acid content of Pharmacopoeia of the People's Republic of China version in 2005, Measure the content of glycyrrhizic acid in the concentrate, and calculate the amount of glycyrrhizic acid in the decocting liquid, above-mentioned test is with different batches Inferior honey-fried licorice root repeats to do 3 times, record in the decocting liquid amount of glycyrrhizic acid and be followed successively by 0.40 gram, 0.48 gram and 0.54 gram.
Measure the glycyrrhizic acid content in three batches of honey-fried licorice root dispensing granules
(1) 1 gram honey-fried licorice root dispensing granule is equivalent to 3 gram honey-fried licorice root medicine materical crude slice
Be followed successively by 2.4%, 2.9%, 3.0%, i.e. the contained glycyrrhizic acid of 16.7 gram honey-fried licorice root dispensing granules Be respectively 0.40 gram, 0.48 gram, 0.50 gram. Glycyrrhizic acid in the 16.7 gram honey-fried licorice root dispensing granules is described Amount be equivalent to the utilization of 50 gram honey-fried licorice root medicine materical crude slice glycyrrhizic acids in decoction, 1 gram honey-fried licorice root dispensing granule The equivalent that is equivalent to 3 gram honey-fried licorice root medicine materical crude slice is science. The honey-fried licorice root dispensing granule of this equivalent relation sweet Oxalic acid content is 2.0%-3.0%.
(2) 1 gram honey-fried licorice root dispensing granules are equivalent to 5 gram Radix Glycyrrhizae Preparata decoction pieces
Be followed successively by 4.2%, 4.9%, 5.5%, promptly the contained glycyrrhizic acid of 10 gram honey-fried licorice root dispensing granules is respectively 0.42 gram, 0.49 gram, 0.55 gram.Illustrate that the amount of glycyrrhizic acid in the 10 gram honey-fried licorice root dispensing granules is equivalent to the utilization of 50 gram Radix Glycyrrhizae Preparata decoction pieces glycyrrhizic acid in decoction, the equivalent that 1 gram honey-fried licorice root dispensing granule is equivalent to 5 gram Radix Glycyrrhizae Preparata decoction pieces is a science.The glycyrrhizic acid content of the honey-fried licorice root dispensing granule of this equivalent relation is 4.0%-6.0%.
Experimental example 3 contains Radix Glycyrrhizae Preparata classics side decoction pieces decocting liquid and soup that honey-fried licorice root dispensing granule is joined " whole part " infrared spectrogram comparative experiments
SHENGMA GEGEN TANG comes from " Yan Shi children's side opinion ", and prescription is formed and comprised Rhizoma Cimicifugae, Radix Puerariae, Radix Paeoniae, 4 flavour of a drug of Radix Glycyrrhizae; The effect relieving the exterior syndrome with drugs of pungent in flavor and cool in nature.
1, experiment purpose: the similarities and differences of research SHENGMA GEGEN TANG decoction pieces decocting liquid and granular recipe, determine honey-fried licorice root dispensing granule technology and normal reasonability.
2, experimental technique: get 4 flavour of a drug prescriptions such as Radix Glycyrrhizae Preparata by SHENGMA GEGEN TANG prescription 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 Radix Glycyrrhizae Preparata respectively by SHENGMA GEGEN TANG prescription proportioning, the decocting method of pressing the decoction pieces decoction decocts, medicinal liquid suitably concentrates, getting honey-fried licorice root dispensing granule by SHENGMA GEGEN TANG prescription proportioning and equivalent relation adds in the concentrated medicament, be stirred to dissolving fully, preparation granular recipe sample; Drinking sheet decocting liquid sample, granular recipe sample respectively carries out infrared spectrum and detects.
3, 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.
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 95.86%.It is consistent to prove that soup that honey-fried licorice root dispensing granule of the present invention is joined and decoction pieces close the decocting liquid composition, it is consistent with a Radix Glycyrrhizae Preparata decoction pieces fried composition promptly to add honey-fried licorice root dispensing granule of the present invention, and equivalent and production technology that honey-fried licorice root dispensing granule 1g of the present invention is equivalent to Radix Glycyrrhizae Preparata decoction pieces 3-5 gram are rational.
Following embodiment all can realize the effect of above-mentioned experimental example, and required Radix Glycyrrhizae Preparata decoction pieces adopts Infrared fingerprint spectra to carry out quality discrimination among the following embodiment, meets the standard Infrared fingerprint spectra of the Radix Glycyrrhizae Preparata decoction pieces in the technique scheme; The honey-fried licorice root dispensing granule that following embodiment makes adopts Infrared fingerprint spectra to carry out quality discrimination, meets the Infrared fingerprint spectra of the honey-fried licorice root dispensing granule in the technique scheme; The every gram of honey-fried licorice root dispensing granule described in the following embodiment contains suitable crude drug amount 3-5 gram.
The specific embodiment
Embodiment 1: honey-fried licorice root dispensing granule
Get Radix Glycyrrhizae Preparata decoction pieces 100kg, 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, the Radix Glycyrrhizae Preparata spray drying powder; The adjuvant dextrin that in the Radix Glycyrrhizae Preparata spray drying powder, adds himself weight portion 0-5%; The Radix Glycyrrhizae Preparata spray drying powder is 5MPa at main pinch roller pressure, 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, get 20-60 purpose honey-fried licorice root dispensing granule, suitable crude drug amount 5 grams of the every gram of honey-fried licorice root dispensing granule.Glycyrrhizic acid content is 4.0%-6.0% in the Radix Glycyrrhizae Preparata.
Embodiment 2: honey-fried licorice root dispensing granule
Get Radix Glycyrrhizae Preparata decoction pieces 100kg, 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, the Radix Glycyrrhizae Preparata spray drying powder; The adjuvant dextrin that in the Radix Glycyrrhizae Preparata 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 honey-fried licorice root dispensing granule, suitable crude drug amount 4 grams of the every gram of honey-fried licorice root dispensing granule.Glycyrrhizic acid content is 3.0%-4.0% in the Radix Glycyrrhizae Preparata.
The method of quality control of wherein said Radix Glycyrrhizae Preparata decoction pieces comprises the steps: that the Radix Glycyrrhizae Preparata decoction pieces 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 4cmm
-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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: as shown in Figure 2 at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place.
Embodiment 3: honey-fried licorice root dispensing granule
Get Radix Glycyrrhizae Preparata decoction pieces 100kg, 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, the Radix Glycyrrhizae Preparata spray drying powder; The lactose that in the Radix Glycyrrhizae Preparata 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 honey-fried licorice root dispensing granule, suitable crude drug amount 3 grams of the every gram of honey-fried licorice root dispensing granule.Glycyrrhizic acid content is 2.0%-3.0% in the Radix Glycyrrhizae Preparata.
The method of quality control of gained honey-fried licorice root dispensing granule 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; The honey-fried licorice root dispensing granule Infrared fingerprint spectra has following feature: as shown in Figure 1 at 1610cm
-1, 1054cm
-1Two strong absworption peaks, wherein 1054cm are arranged
-1Place's absorption peak strength maximum; At 2929cm
-1, 1419cm
-1, 1244cm
-1, 778cm
-1There is characteristic absorption at the place.
Claims (10)
1, a kind of honey-fried licorice root dispensing granule is characterized in that the suitable crude drug amount of the every gram of described honey-fried licorice root dispensing granule 3-5 gram.
2, a kind of honey-fried licorice root dispensing granule is characterized in that this honey-fried licorice root dispensing granule Infrared fingerprint spectra has following feature: adopt Fourier transform infrared spectrometer to measure, at 1610cm
-1, 1054cm
-1Two strong absworption peaks, wherein 1054cm are arranged
-1Place's absorption peak strength maximum; At 2929cm
-1, 1419cm
-1, 1244cm
-1, 778cm
-1There is characteristic absorption at the place.
3, honey-fried licorice root dispensing granule as claimed in claim 1 is characterized in that the Infrared fingerprint spectra of this granule has following feature: at 1610cm
-1, 1054cm
-1Two strong absworption peaks, wherein 1054cm are arranged
-1Place's absorption peak strength maximum; At 2929cm
-1, 1419cm
-1, 1244cm
-1, 778cm
-1There is characteristic absorption at the place.
4, a kind of preparation method of honey-fried licorice root dispensing granule is characterized in that this method comprises a kind of in the following method:
Get the Radix Glycyrrhizae Preparata decoction pieces, 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 5-15 times of weight portion of Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, honey-fried licorice root dispensing granule;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, honey-fried licorice root dispensing granule;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, honey-fried licorice root dispensing granule;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, honey-fried licorice root dispensing granule.
5, the preparation method of honey-fried licorice root dispensing granule as claimed in claim 4 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.
6, the preparation method of honey-fried licorice root dispensing granule as claimed in claim 4 is characterized in that wherein the quality discrimination of Radix Glycyrrhizae Preparata decoction pieces Infrared fingerprint spectra 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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place.
7, a kind of preparation method of honey-fried licorice root dispensing granule is characterized in that this method comprises a kind of in the following method:
Get the Radix Glycyrrhizae Preparata decoction pieces, 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 5-15 times of weight portion of Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule; Wherein the Radix Glycyrrhizae Preparata decoction pieces adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is 4000cm for using Fourier transform infrared spectrometer, measurement range
-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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule; Wherein the Radix Glycyrrhizae Preparata decoction pieces 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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule; Wherein the Radix Glycyrrhizae Preparata decoction pieces 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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place;
Or get the Radix Glycyrrhizae Preparata decoction pieces, 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 Radix Glycyrrhizae Preparata decoction pieces, 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 the Radix Glycyrrhizae Preparata spray drying powder; The Radix Glycyrrhizae Preparata spray drying powder is directly granulated or add adjuvant dextrin or the lactose dry granulation of himself weight portion 0-25% in the Radix Glycyrrhizae Preparata spray drying powder, 20-60 purpose honey-fried licorice root dispensing granule; Wherein the Radix Glycyrrhizae Preparata decoction pieces 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 Infrared fingerprint spectra of Radix Glycyrrhizae Preparata decoction pieces has following feature: at 1000cm
-1-1200cm
-1Scope in an absworption peak that intensity is big, peak shape is wide is arranged, be stairstepping, maximum absorption band is positioned at 1049cm
-1At 2929cm
-1, 1631cm
-1, 1424cm
-1, 1241cm
-1, 776cm
-1There is characteristic absorption at the place.
8, the preparation method of honey-fried licorice root dispensing granule as claimed in claim 7 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.
9, as claim 2,3 arbitrary described honey-fried licorice root dispensing granules, 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.
10, honey-fried licorice root dispensing granule as claimed in claim 1 is characterized in that the content of glycyrrhizic acid in this granule is not less than 2.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810184583 CN101474244A (en) | 2007-12-18 | 2008-12-17 | Honey-fried licorice root dispensing granule as well as preparation method and quality control method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710179748 | 2007-12-18 | ||
| CN200710179748.2 | 2007-12-18 | ||
| CN 200810184583 CN101474244A (en) | 2007-12-18 | 2008-12-17 | Honey-fried licorice root dispensing granule as well as preparation method and quality control method |
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| CN101474244A true CN101474244A (en) | 2009-07-08 |
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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 200810184570 Active CN101474290B (en) | 2007-12-18 | 2008-12-17 | Detection method of figwort root dispensing granule |
| 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 |
| CN 200810184561 Active CN101474225B (en) | 2007-12-18 | 2008-12-17 | Ledebouriella root granule as well as preparation method and quality control method |
| CN 200810184580 Active CN101474278B (en) | 2007-12-18 | 2008-12-17 | Processed fructus evodiae dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184579 Pending CN101474318A (en) | 2007-12-18 | 2008-12-17 | Rhizoma alismatis dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184563 Active CN101474253B (en) | 2007-12-18 | 2008-12-17 | Detection method of cassia twig dispensing granule |
| CN 200810184575 Active CN101480420B (en) | 2007-12-18 | 2008-12-17 | Detection method of ballonflower dispensing granule |
| 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 |
| 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 200810184569 Active CN101474237B (en) | 2007-12-18 | 2008-12-17 | Detection method of trichosanthes dispensing granule |
| CN 200810184578 Active CN101474229B (en) | 2007-12-18 | 2008-12-17 | Oriental wormwood dispensing granule as well as preparation method and quality control method |
| CN 200810184560 Active CN101518589B (en) | 2007-12-18 | 2008-12-17 | Rehmannia Root formula granules as well as preparation method and quality control method thereof |
| CN 200810184576 Active CN101474287B (en) | 2007-12-18 | 2008-12-17 | Detection method of prepared rehmannia root dispensing granule |
| CN 200810184567 Active CN101474224B (en) | 2007-12-18 | 2008-12-17 | Notopterygium root dispensing granule as well as preparation method and quality control method |
| CN 200810184573 Active CN101474293B (en) | 2007-12-18 | 2008-12-17 | Medlar dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184562 Active CN101474223B (en) | 2007-12-18 | 2008-12-17 | Chinese angelica root dispensing granule as well as preparation method and quality control method |
| CN 200810184566 Active CN101474219B (en) | 2007-12-18 | 2008-12-17 | Detection method of achyranthes bidentata dispensing granule |
| CN 200810184565 Pending CN101474352A (en) | 2007-12-18 | 2008-12-17 | Ophiopogon root dispensing granule as well as preparation method and quality control method thereof |
| 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 200810184571 Active CN101474241B (en) | 2007-12-18 | 2008-12-17 | Detection method of astragalus dispensing granule |
| CN 200810184572 Active CN101474221B (en) | 2007-12-18 | 2008-12-17 | Detection method of glehnia root dispensing granule |
| CN 200810184583 Pending CN101474244A (en) | 2007-12-18 | 2008-12-17 | Honey-fried licorice root dispensing granule as well as preparation method and quality control method |
| CN 200810184577 Active CN101474228B (en) | 2007-12-18 | 2008-12-17 | Detection method of wild chrysanthemum dispensing granule |
| CN 200810184574 Active CN101474263B (en) | 2007-12-18 | 2008-12-17 | White peony root dispensing granule as well as preparation method and quality control method thereof |
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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 200810184570 Active CN101474290B (en) | 2007-12-18 | 2008-12-17 | Detection method of figwort root dispensing granule |
| 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 |
| CN 200810184561 Active CN101474225B (en) | 2007-12-18 | 2008-12-17 | Ledebouriella root granule as well as preparation method and quality control method |
| CN 200810184580 Active CN101474278B (en) | 2007-12-18 | 2008-12-17 | Processed fructus evodiae dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184579 Pending CN101474318A (en) | 2007-12-18 | 2008-12-17 | Rhizoma alismatis dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184563 Active CN101474253B (en) | 2007-12-18 | 2008-12-17 | Detection method of cassia twig dispensing granule |
| CN 200810184575 Active CN101480420B (en) | 2007-12-18 | 2008-12-17 | Detection method of ballonflower dispensing granule |
| 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 |
| 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 200810184569 Active CN101474237B (en) | 2007-12-18 | 2008-12-17 | Detection method of trichosanthes dispensing granule |
| CN 200810184578 Active CN101474229B (en) | 2007-12-18 | 2008-12-17 | Oriental wormwood dispensing granule as well as preparation method and quality control method |
| CN 200810184560 Active CN101518589B (en) | 2007-12-18 | 2008-12-17 | Rehmannia Root formula granules as well as preparation method and quality control method thereof |
| CN 200810184576 Active CN101474287B (en) | 2007-12-18 | 2008-12-17 | Detection method of prepared rehmannia root dispensing granule |
| CN 200810184567 Active CN101474224B (en) | 2007-12-18 | 2008-12-17 | Notopterygium root dispensing granule as well as preparation method and quality control method |
| CN 200810184573 Active CN101474293B (en) | 2007-12-18 | 2008-12-17 | Medlar dispensing granule as well as preparation method and quality control method thereof |
| CN 200810184562 Active CN101474223B (en) | 2007-12-18 | 2008-12-17 | Chinese angelica root dispensing granule as well as preparation method and quality control method |
| CN 200810184566 Active CN101474219B (en) | 2007-12-18 | 2008-12-17 | Detection method of achyranthes bidentata dispensing granule |
| CN 200810184565 Pending CN101474352A (en) | 2007-12-18 | 2008-12-17 | Ophiopogon root dispensing granule as well as preparation method and quality control method thereof |
| 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 200810184571 Active CN101474241B (en) | 2007-12-18 | 2008-12-17 | Detection method of astragalus dispensing granule |
| CN 200810184572 Active CN101474221B (en) | 2007-12-18 | 2008-12-17 | Detection method of glehnia root dispensing granule |
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| CN 200810184574 Active CN101474263B (en) | 2007-12-18 | 2008-12-17 | White peony root dispensing granule as well as preparation method and quality control method thereof |
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