CN101342199A - Chinese ephedra prescription particle, preparation method and quality control method thereof - Google Patents
Chinese ephedra prescription particle, preparation method and quality control method thereof Download PDFInfo
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- CN101342199A CN101342199A CN 200710118746 CN200710118746A CN101342199A CN 101342199 A CN101342199 A CN 101342199A CN 200710118746 CN200710118746 CN 200710118746 CN 200710118746 A CN200710118746 A CN 200710118746A CN 101342199 A CN101342199 A CN 101342199A
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Abstract
The invention discloses a herba ephedra prescription particle and a preparation method and a quality control method thereof. The prescription particle adopts the herba ephedrae as raw materials. Spraying dried herba ephedra powder is made by extracting the herba ephedrae with acidified water, concentrating the herba ephedrae under low pressure and low temperature and spray-drying the herba ephedrae. The herba ephedra particle is made by the spraying dried herba ephedra powder directly or by mixing the praying dried herba ephedra powder with proper quantities of auxiliary materials. Each herba ephedra prescription particle is equivalent to 10 grams of crude drug and the content of the ephedrine hydrochloride in the particle is not less than 3.0 percent. The herba ephedra prescription particle of the invention is provided with an IR fingerprint spectra as indicated in figure3.
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 Chinese ephedra prescription particle and preparation method thereof and method of quality control.
Background technology
Traditional method for making of Chinese medicine granules is: get the prepared slices of Chinese crude drugs, decoct with water, decocting liquid is evaporated to thick paste, adds dextrin or lactose or maltodextrin, wet granulation, and oven dry, encapsulation is promptly.This wet granulation need add a large amount of adjuvant (7-8 that is generally thick paste doubly measures) and fill in thick paste.But the preparation of making, drug level is low, and dose is big, and curative effect is not obvious.Chinese medicinal granule, be under Chinese medical theory instructs, with the prepared slices of Chinese crude drugs of concocting processing through standard is raw material, adopts Technologies such as extraction, cryoconcentration, spray drying to be processed into, and uses or as the granule of preparation raw material medicine use for doctor formula.
Chinese ephedra prescription particle is a kind of of conventional Chinese medicine granule, and common process is that water extraction concentrates, granulate after vacuum drying or the spray drying; Its quality standard is generally the thin-layer qualitative discriminating and Determination of Ephedrine Hydrochloride is measured.The defective that this product exists at present is: (1) big production technology falls behind, and mostly is traditional water and extracts, and the rate of transform of ephedrine is quite limited, and drug effect is seriously influenced; (2) quality standard is general at the quality control specificity of Chinese ephedra prescription particle, can not really realize the quality control of the product on the complete meaning.The quality standard of this product can only guarantee to contain in the product ephedrine hydrochloride at present, can not guarantee that product is that raw material is produced with the Herba Ephedrae, the information that lacks other due quality of product can't accurately be judged the quality good or not and the overall picture of Chinese ephedra prescription particle product.
Summary of the invention
The objective of the invention is to disclose a kind of Chinese ephedra prescription particle; The present invention also aims to disclose the preparation method of this granule; The present invention also aims to disclose the method for quality control of this granule.
The present invention seeks to be achieved through the following technical solutions:
The every gram of Chinese ephedra prescription particle of the present invention contains suitable crude drug amount 10 grams; Determination of Ephedrine Hydrochloride is not less than 3.0% in the granule; Measure its Infrared fingerprint spectra with infrared spectrum technology, measurement result is: highest peak: peak position 1023cm
-1, at 1078cm
-1, 1152cm
-1Have two peaks and form peak bunch with it; Inferior strong peak: peak position 1629cm
-1With 1726cm
-1, 1514cm
-1Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762cm
-1, 843cm
-1A peak is respectively arranged; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peak (see figure 3)s;
Its Infrared fingerprint spectra condition determination: instrument is a Fourier transform infrared spectrometer, Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
The preparation method of Chinese ephedra prescription particle of the present invention is:
The raw material Herba Ephedrae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range 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; Herba Ephedrae HERBA EPHEDRAE standard Infrared fingerprint spectra (Fig. 1) has following feature: highest peak: peak position 1623cm
-1, have 1547cm
-1The peak forms peak bunch with it; Inferior strong peak: peak position 1032cm
-1, have 1103cm
-1The peak forms peak bunch with it; Strong peak: peak position 2922cm
-1, at 2851cm
-1There is a peak to form peak bunch with it; Intensity according to the peak has 1317cm from height successively to hanging down in addition
-1, 1384cm
-1, 1443cm
-1, 1240cm
-1Peak that forms bunch and 516cm
-1, 780cm
-1Two peaks;
Get the hydrochloric acid that above-mentioned raw materials Herba Ephedrae chopping back adds the 1%-2% of 1-2 times of weight portion, soaked into 4-8 hour, add the water extraction one time of 4-8 times of weight portion of raw material Herba Ephedrae again, promptly one fry in shallow oil extraction time 1.5-2 hour; One fries in shallow oil the water that the back medical material adds 6-8 times of weight portion of raw material Herba Ephedrae, promptly two fries in shallow oil, and extracts 1-1.5 hour; Two liquid of boiling medicine merge, and are evaporated to relative density 1.05-1.15, concentrated solution; The concentrated solution spray drying gets the Herba Ephedrae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0%-20% in the Herba Ephedrae spray drying powder; Dry granulation gets Chinese ephedra prescription particle.
Above-mentioned preparation method is preferably: get 1.5% the hydrochloric acid that raw material Herba Ephedrae chopping back adds 1.5 times of weight portions, soaked into 6 hours, add the water extraction one time of 6 times of weight portions of raw material Herba Ephedrae again, promptly one fry in shallow oil 2 hours extraction times; One fries in shallow oil the water that the back medical material adds 7 times of weight portions of raw material Herba Ephedrae, promptly two fries in shallow oil, and extracts 1.5 hours; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; The concentrated solution spray drying gets the Herba Ephedrae spray drying powder; Xeraphium is directly granulated or add the adjuvant dextrin or the lactose of himself weight portion 10% in the Herba Ephedrae spray drying powder; Dry granulation gets Chinese ephedra prescription particle.
The drying process with atomizing parameter is in the preparation method of Chinese ephedra prescription particle of the present invention: the medicinal liquid preheat temperature is lower than 60 ℃; 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 preparation method of Chinese ephedra prescription particle of the present invention: main pinch roller pressure: 4-6MPa; Side pressure wheel pressure: 0.4-0.6MPa; The speed of mainshaft: 300-500 rev/min; Feed voltage: 100-150V; Granular size: 20-60 order.
The method of quality control of Chinese ephedra prescription particle of the present invention comprises one or more in the following method:
A. the quality control of Herba Ephedrae spray drying powder: the Herba Ephedrae spray drying powder adopts Fourier transform infrared spectrometer, measurement range 4000cm-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra (see figure 2) of Herba Ephedrae spray drying powder is characterized as:
Highest peak: peak position 1616cm
-1, have 1727cm
-1, 1515cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1076cm
-1Strong peak: peak position 1384cm
-1, at 1407cm
-1Have a peak and form peak bunch with it; Intensity according to the peak has 621cm from height successively to hanging down in addition
-1, 703cm
-1Two peaks;
B. the quality control of Chinese ephedra prescription particle: Chinese ephedra prescription particle adopts Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects: the standard Infrared fingerprint spectra (Fig. 3) of Chinese ephedra prescription particle is characterized as:
Highest peak: peak position 1023cm
-1, have 1078cm
-1, 1152cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1629cm
-1, with 1726cm
-1, 1514cm
-1Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762cm
-1, 843cm
-1Respectively has a peak; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peaks.
Description of drawings
Fig. 1: Herba Ephedrae HERBA EPHEDRAE standard Infrared fingerprint spectra;
Fig. 2: Herba Ephedrae spray drying powder standard Infrared fingerprint spectra;
Fig. 3: Chinese ephedra prescription particle standard Infrared fingerprint spectra;
Fig. 4: Herba Ephedrae-Radix Puerariae medicine compares decoction pieces decocting liquid and granular recipe of the present invention " whole part " infrared spectrogram;
Fig. 5: Mahuang Fuzi Xixin Tang decoction pieces decocting liquid and granular recipe of the present invention " whole part " infrared spectrogram are relatively.
Fig. 6 Herba Ephedrae medical material and Chinese ephedra prescription particle thin layer chromatography be (annotate: lamellae is followed successively by 1 Chinese ephedra prescription particle, 2 Herba Ephedrae medical materials, 3 blank from left to right) relatively
Fig. 7 Herba Ephedrae medical material and Chinese ephedra prescription particle thin-layer sample Infrared fingerprint spectra are relatively
Complete, advanced production technology that Chinese ephedra prescription particle of the present invention has and specificity strong, controlled Quality control standard, technology advanced person can realize, quality standard relates to detection method science, advanced person, fast Victory, workable. Chinese ephedra prescription particle of the present invention has taking convenience, and auxiliary material content is low, and medicine is dense Degree is high, and dose is little, and is quality controllable, preserves easily, and the advantage such as be easy to carry.
Following experimental example and embodiment are used for further specifying but are not limited to the present invention.
The ephedrine hydrochloride utilization of experimental example 1 granule of the present invention and Herba Ephedrae relatively
Get Chinese ephedra medicine materical crude slice 50 grams, extracted 30 minutes with 10 times of amounts, leach the soup dregs of a decoction and add 8 times in water 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. According to an epheday intermedia medicinal material of Pharmacopoeia of the People's Republic of China version in 2005 assay item method, measure Ephedrine hydrochloride gets content in the concentrate, and calculates the amount of ephedrine hydrochloride in the decocting liquid, above-mentioned test Repeat to do 3 times with the Chinese ephedra of different batches, record that the amount of ephedrine hydrochloride is followed successively by 0.18 in the decocting liquid Gram, 0.15 gram and 0.16 gram. Measure the Determination of ephedrine hydrochloride in three batches of Chinese ephedra prescription particles, comply with Inferior is 3.0%, 3.4%, 3.3%, i.e. the contained ephedrine hydrochloride difference of 5 gram Chinese ephedra prescription particles Be 0.15 gram, 0.17 gram, 0.165 gram. Ephedrine hydrochloride in the 5 gram Chinese ephedra prescription particles is described Amount is equivalent to the utilization of 50 gram Chinese ephedra medicine materical crude slice ephedrine hydrochloride in decoction, 1 gram Chinese ephedra of the present invention The equivalent that granule is equivalent to 10 gram Herba Ephedraes is science.
Experimental example 2 extraction process screening studies
According to the result of modern pharmacology research, the ephedrines composition is the functions such as Chinese ephedra cough-relieving, diuresis The main pharmacodynamics composition, so the content of Chinese ephedra prescription particle epheday intermedia alkaloids will directly have influence on Chinese ephedra The curative effect of granule. We determine the extraction process of Chinese ephedra by orthogonal experiment, and experimental design is as follows:
Table 1 experimental design table
Table 2 experiment and result
In the above-mentioned experimentation, time 2 h is fried in shallow oil in all experiments one, and 2 fry in shallow oil 1.5 hours time.
Quadrature intuitive analysis result:
1. infiltrating time and acid concentration are obvious to the Content of Ephedrine With impact, and especially infiltrating time shows Trend is conducive to carry the content of spray dried powder Ephedrine for increasing acid concentration and infiltrating time, but This trend when being mainly manifested in acid concentration and being lower than 1.5%, when acid concentration is higher than 1.5%, this Trend is not obvious.
2. one fry in shallow oil two to fry in shallow oil amount of water obvious to the impact of flour extraction, influence degree approaches, and amount of water strengthens out The powder rate increases.
3. infiltrating time has some impacts to flour extraction, and impact is not clearly.
4. acid concentration is to almost not impact of flour extraction.
Take all factors into consideration from the various conditions of flour extraction, Content of Ephedrine With and production cost, preferred actual production conditions is 1.5% salt acid soakage 8 hours, and one fries in shallow oil 6-8 times of water, and two fry in shallow oil 6-8 times of water.
Repeat above-mentioned preferred working condition and produce 3 batches, Content of Ephedrine With is followed successively by 3.56%, 3.62%, 3.57%, and flour extraction is followed successively by 13.8%, 13.5%, 13.6% process stabilizing, and Content of Ephedrine With is stable.
Experimental example 3 contains Herba Ephedrae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram compares
Herba Ephedrae-Radix Puerariae 5 usefulness come from the treatise on Febrile Diseases GEGEN TANG.The turbid suffering of Herba Ephedrae property is loose, and opens and closes diaphoresis, and the kind wind and cold of separating at table is the Taiyang channel medicine; Radix Puerariae suffering cool in nature is sweet, returns the taste warp, is good at the diaphoresis expelling pathogenic factors from muscles for reducing heat, rises the clearing heat in QI system promoting the production of body fluid to quench thirst of Fa Yangming.The two medicine mutual-assistances are usefulness, rise to distribute antiperspirant, and the eliminating evil effect of inducing sweat is strengthened, and with controlling the exterior tightened by pathogenic windcold, meridians are unfavorable and classical medicine that the real double stiffness of the nape and back of seeing of table that cause is demonstrate,proved is right.
This is tested routine purpose and is to study the similarities and differences that the two decoction pieces closes decocting liquid and granular recipe, determines Chinese ephedra prescription particle technology and normal reasonability.
Experimental technique: get Herba Ephedrae decoction pieces, each 10g prescription of Radix Puerariae decoction pieces, the decocting method of pressing the decoction pieces decoction decocts preparation decoction pieces decocting liquid sample; Other gets Radix Puerariae decoction pieces 10g, and the decocting method of pressing the decoction pieces decoction decocts, and medicinal liquid suitably concentrates, and adds Chinese ephedra prescription particle 1g of the present invention, is stirred to dissolving fully, system granular recipe sample; Drinking sheet decocting liquid sample, granular recipe sample respectively carries out infrared spectrum and detects.
Testing conditions: detecting instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
Testing result: decoction pieces decocting liquid sample and granular recipe sample Infrared fingerprint spectra peak shape, peak position, peak intensity basically identical as shown in Figure 4, dependency reaches 98.2%.It is consistent to prove that soup that granule of the present invention is joined and decoction pieces close the decocting liquid composition, be that 1g Chinese ephedra prescription particle of the present invention is consistent with a 10g Herba Ephedrae decoction pieces fried composition, equivalent and production technology that Chinese ephedra prescription particle 1g of the present invention is equivalent to Herba Ephedrae decoction pieces 10g are rational.
Experimental example 4 contains Herba Ephedrae classics side decoction pieces decocting liquid and granular recipe " whole part " infrared spectrogram compares
Mahuang Fuzi Xixin Tang comes from treatise on Febrile Diseases, and prescription is formed and comprised Herba Ephedrae, Radix Aconiti Lateralis Preparata, 3 flavour of a drug of Herba Asari.The function warming the meridian and promoting blood circulation, supporing yang expelling cold for relieving asthma effect.
This tests the similarities and differences of routine purpose research Mahuang Fuzi Xixin Tang decoction pieces decocting liquid and granular recipe, determines Chinese ephedra prescription particle technology and normal reasonability.
Experimental technique: get each flavour of a drug prescription of Herba Ephedrae by the Mahuang Fuzi Xixin Tang 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 Herba Ephedrae respectively by Mahuang Fuzi Xixin Tang prescription proportioning, the decocting method of pressing the decoction pieces decoction decocts, medicinal liquid suitably concentrates, getting Chinese ephedra prescription particle of the present invention by Mahuang Fuzi Xixin 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.
Testing conditions: instrument is a Fourier transform infrared spectrometer, and measurement range is 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects.
Testing result: decoction pieces decocting liquid sample and granular recipe sample Infrared fingerprint spectra peak shape, peak position, peak intensity basically identical as shown in Figure 5, dependency reaches 93.2%.It is consistent to prove that soup that granule is joined and decoction pieces close the decocting liquid composition, and it is consistent with a Herba Ephedrae decoction pieces fried composition promptly to add Chinese ephedra prescription particle of the present invention, and equivalent and production technology that Chinese ephedra prescription particle 1g of the present invention is equivalent to Herba Ephedrae decoction pieces 10g are rational.
Experimental example 5
(1) Chinese ephedra prescription particle and the comparative study of Herba Ephedrae medical material thin layer chromatography
Differentiate a thin layer chromatography test down according to epheday intermedia medical material of Pharmacopoeia of the People's Republic of China version in 2005, prepare sample with Herba Ephedrae medical material and Chinese ephedra prescription particle of the present invention, measure, the gained result as shown in Figure 6, in the Chinese ephedra prescription particle chromatograph, with the corresponding position of Herba Ephedrae medical material chromatograph on, show the speckle of same color.
(2) Chinese ephedra prescription particle and Herba Ephedrae medical material thin-layer sample Infrared fingerprint spectra are relatively
Measure the Herba Ephedrae medical material of preparation in (1) and the thin-layer sample of Chinese ephedra prescription particle with Fourier transform infrared spectrometer, its result as shown in Figure 7, the thin-layer sample Infrared fingerprint spectra peak shape of Chinese ephedra prescription particle and Herba Ephedrae medical material, peak position, peak intensity basically identical, dependency reaches 97.1%.
Prove that Chinese ephedra prescription particle of the present invention is consistent with the Herba Ephedrae medicinal ingredient, technology of the present invention is rational.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: the preparation method of Chinese ephedra prescription particle
The raw material Herba Ephedrae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects: the gained result is consistent with Herba Ephedrae standard Infrared fingerprint spectra; Herba Ephedrae standard Infrared fingerprint spectra is characterized as: highest peak: peak position 1623cm
-1, have 1547cm
-1The peak forms peak bunch with it; Inferior strong peak: peak position 1032cm
-1, have 1103cm
-1The peak forms peak bunch with it; Strong peak: peak position 2922cm
-1, at 2851cm
-1There is a peak to form peak bunch with it; Intensity according to the peak has 1317cm from height successively to hanging down in addition
-1, 1384cm
-1, 1443cm
-1, 1240cm
-1Peak that forms bunch and 516cm
-1, 780cm
-1Two peaks;
Get 1.5% the hydrochloric acid that above-mentioned raw materials Herba Ephedrae 1kg chopping back adds 1.5kg, soaked into 6 hours, add the water extraction one time of raw material Herba Ephedrae 6kg again, promptly one fry in shallow oil 2 hours extraction times; One fries in shallow oil the water that the back medical material adds raw material Herba Ephedrae 7kg, promptly two fries in shallow oil, and extracts 1.5 hours; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; Concentrated solution is lower than spray drying under the condition that 60 ℃, 170 ℃ of inlet temperature, 700 rev/mins of revolution speeds of material, 70 ℃ of leaving air temps, wind send 50 ℃ of temperature in the medicinal liquid preheat temperature, Herba Ephedrae spray drying powder 0.13kg; Xeraphium is direct dry granulation under the granulation condition of main pinch roller pressure 4MPa, side pressure wheel pressure 0.6MPa, 300 rev/mins of the speeds of mainshaft, feed voltage 150V, gets the Chinese ephedra prescription particle of 20～60 order granular sizes.
Embodiment 2: the preparation method of Chinese ephedra prescription particle
The raw material Herba Ephedrae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range 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: gained result and Herba Ephedrae standard Infrared fingerprint spectra similarity are 98%; Herba Ephedrae standard Infrared fingerprint spectra is characterized as: highest peak: peak position 1623cm
-1, have 1547cm
-1The peak forms peak bunch with it; Inferior strong peak: peak position 1032cm
-1, have 1103cm
-1The peak forms peak bunch with it; Strong peak: peak position 2922cm
-1, at 2851cm
-1There is a peak to form peak bunch with it; Intensity according to the peak has 1317cm from height successively to hanging down in addition
-1, 1384cm
-1, 1443cm
-1, 1240cm
-1Peak that forms bunch and 516cm
-1, 780cm
-1Two peaks;
Get 1.5% the hydrochloric acid that above-mentioned raw materials Herba Ephedrae 1kg chopping back adds 1.5kg, soaked into 6 hours, add the water extraction one time of raw material Herba Ephedrae 6kg again, promptly one fry in shallow oil 2 hours extraction times; One fries in shallow oil the water that the back medical material adds raw material Herba Ephedrae 7kg, promptly two fries in shallow oil, and extracts 1.5 hours; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; Concentrated solution is lower than spray drying under the condition that 60 ℃, 185 ℃ of inlet temperature, 450 rev/mins of revolution speeds of material, 85 ℃ of leaving air temps, wind send 40 ℃ of temperature in the medicinal liquid preheat temperature, Herba Ephedrae spray drying powder 0.14kg; Xeraphium adds the adjuvant dextrin of 0.014kg; Dry granulation under the granulation condition of main pinch roller pressure 6MPa, side pressure wheel pressure 0.4MPa, 500 rev/mins of the speeds of mainshaft, feed voltage 100V, the Chinese ephedra prescription particle of 20～60 order granular sizes.
Embodiment 3: the method for quality control of the Chinese ephedra prescription particle of embodiment 1 preparation
A. the quality control of Herba Ephedrae spray drying powder: the Herba Ephedrae spray drying powder adopts Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The gained result is consistent with Herba Ephedrae spray drying powder standard Infrared fingerprint spectra, and the standard Infrared fingerprint spectra (Fig. 2) of Herba Ephedrae spray drying powder is characterized as:
Highest peak: peak position 1616cm
-1, have 1727cm
-1, 1515cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1076cm
-1Strong peak: peak position 1384cm
-1, at 1407cm
-1Have a peak and form peak bunch with it; Intensity according to the peak has 621cm from height successively to hanging down in addition
-1, 703cm
-1Two peaks;
B. the quality control of Chinese ephedra prescription particle: Chinese ephedra prescription particle adopts Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The gained result is consistent with Chinese ephedra prescription particle standard Infrared fingerprint spectra, and the standard Infrared fingerprint spectra (Fig. 3) of Chinese ephedra prescription particle is characterized as:
Highest peak: peak position 1023cm
-1, have 1078cm
-1, 1152cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1629cm
-1, with 1726cm
-1, 1514cm
-1Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762cm
-1, 843cm
-1Respectively has a peak; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peaks.
Embodiment 4: the method for quality control of the Chinese ephedra prescription particle of embodiment 1 preparation
The quality control of Herba Ephedrae spray drying powder: the Herba Ephedrae spray drying powder adopts Fourier transform infrared spectrometer, measurement range 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; Gained result and Herba Ephedrae spray drying powder standard Infrared fingerprint spectra similarity are 96%, and the standard Infrared fingerprint spectra (Fig. 2) of Herba Ephedrae spray drying powder is characterized as:
Highest peak: peak position 1616cm
-1, have 1727cm
-1, 1515cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1076cm
-1Strong peak: peak position 1384cm
-1, at 1407cm
-1Have a peak and form peak bunch with it; Intensity according to the peak has 621cm from height successively to hanging down in addition
-1, 703cm
-1Two peaks.
Embodiment 5: the method for quality control of the Chinese ephedra prescription particle of embodiment 2 preparations
The quality control of Chinese ephedra prescription particle: Chinese ephedra prescription particle adopts Fourier transform infrared spectrometer, measurement range 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; Gained result and Chinese ephedra prescription particle standard Infrared fingerprint spectra similarity are 99%, and the standard Infrared fingerprint spectra (Fig. 3) of Chinese ephedra prescription particle is characterized as:
Highest peak: peak position 1023cm
-1, have 1078cm
-1, 1152cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1629cm
-1, with 1726cm
-1, 1514cm
-1Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762m
-1, 843cm
-1Respectively has a peak; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peaks.
Claims (6)
1, a kind of Chinese ephedra prescription particle is characterized in that the every gram of this Chinese ephedra prescription particle contains suitable crude drug amount 10 grams; Determination of Ephedrine Hydrochloride is not less than 3.0% in the granule; Measure its Infrared fingerprint spectra with Fourier transform infrared spectrometer, measurement result is: highest peak: peak position 1023cm
-1, at 1078cm
-1, 1152cm
-1Have two peaks and form peak bunch with it; Inferior strong peak: peak position 1629cm
-1With 1726cm
-1, 1514cm
-11Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762cm
-1, 843cm
-1A peak is respectively arranged; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peaks;
Its Infrared fingerprint spectra condition determination: instrument is a Fourier transform infrared spectrometer, measurement range 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.
2, the preparation method of Chinese ephedra prescription particle as claimed in claim 1 is characterized in that this method is:
The raw material Herba Ephedrae adopts Infrared fingerprint spectra to carry out quality discrimination, and the Infrared fingerprint spectra discrimination method is: use Fourier transform infrared spectrometer, measurement range 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; Herba Ephedrae HERBA EPHEDRAE standard Infrared fingerprint spectra has following feature: highest peak: peak position 1623cm
-1, have 1547cm
-1The peak forms peak bunch with it; Inferior strong peak: peak position 1032cm
-1, have 1103cm
-1The peak forms peak bunch with it; Strong peak: peak position 2922cm
-1, at 2851cm
-1There is a peak to form peak bunch with it; Intensity according to the peak has 1317cm from height successively to hanging down in addition
-1, 1384cm
-1, 1443cm
-1, 1240cm
-1Peak that forms bunch and 516cm
-1, 780cm
-1Two peaks;
Get the hydrochloric acid that above-mentioned raw materials Herba Ephedrae chopping back adds the 1%-2% of 1-2 times of weight portion, soaked into 4-8 hour, add the water extraction one time of 4-8 times of weight portion of raw material Herba Ephedrae again, promptly one fry in shallow oil extraction time 1.5-2 hour; One fries in shallow oil the water that the back medical material adds 6-8 times of weight portion of raw material Herba Ephedrae, promptly two fries in shallow oil, and extracts 1-1.5 hour; Two liquid of boiling medicine merge, and are evaporated to relative density 1.05-1.15, concentrated solution; The concentrated solution spray drying gets the Herba Ephedrae spray drying powder; Xeraphium is directly granulated or add adjuvant dextrin or the lactose of himself weight portion 0%-20% in the Herba Ephedrae spray drying powder; Dry granulation gets Chinese ephedra prescription particle.
3, the preparation method of Chinese ephedra prescription particle as claimed in claim 2, it is characterized in that this method is: get 1.5% the hydrochloric acid that raw material Herba Ephedrae chopping back adds 1.5 times of weight portions, soaked into 6 hours, add the water extraction one time of 6 times of weight portions of raw material Herba Ephedrae again, promptly one fry in shallow oil 2 hours extraction times; One fries in shallow oil the water that the back medical material adds 7 times of weight portions of raw material Herba Ephedrae, promptly two fries in shallow oil, and extracts 1.5 hours; Two liquid of boiling medicine merge, and are evaporated to relative density 1.10, concentrated solution; The concentrated solution spray drying gets the Herba Ephedrae spray drying powder; Xeraphium is directly granulated or add the adjuvant dextrin or the lactose of himself weight portion 10% in the Herba Ephedrae spray drying powder; Dry granulation gets Chinese ephedra prescription particle.
4, as the preparation method of claim 2 or 3 arbitrary described Chinese ephedra prescription particles, it is characterized in that the drying process with atomizing parameter is in this method: the medicinal liquid preheat temperature is lower than 60 ℃; 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.
5, as the preparation method of claim 2 or 3 arbitrary described Chinese ephedra prescription particles, it is characterized in that the granulation parameter is in this method: main pinch roller pressure: 4-6MPa; Side pressure wheel pressure: 0.4-0.6MPa; The speed of mainshaft: 300-500 rev/min; Feed voltage: 100-150V; Granular size: 20-60 order.
6, the method for quality control of Chinese ephedra prescription particle as claimed in claim 1 is characterized in that comprising in the following method one or more:
A. the quality control of Herba Ephedrae spray drying powder: the Herba Ephedrae spray drying powder adopts Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra of Herba Ephedrae spray drying powder is characterized as:
Highest peak: peak position 1616cm
-1, have 1727cm
-1, 1515cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1076cm
-1Strong peak: peak position 1384cm
-1, at 1407cm
-1Have a peak and form peak bunch with it; Intensity according to the peak has 621cm from height successively to hanging down in addition
-1, 703cm
-1Two peaks;
B. the quality control of Chinese ephedra prescription particle: Chinese ephedra prescription particle adopts Fourier transform infrared spectrometer, measurement range 4000cm
-1-400cm
-1, DTGS detector, resolution 4cm
-1, scanning times 16 times is deducted water and carbon dioxide constantly and is disturbed in the scanning process, and envionmental humidity is lower than 60%, and the potassium bromide direct compression process detects; The standard Infrared fingerprint spectra of Chinese ephedra prescription particle is characterized as:
Highest peak: peak position 1023cm
-1, have 1078cm
-1, 1152cm
-1Peak bunch is formed at two peaks with it; Inferior strong peak: peak position 1629cm
-1, with 1726cm
-1, 1514cm
-1Form peak bunch; Strong peak: peak position 575cm
-1, at 526cm
-1, 704cm
-1, 762cm
-1, 843cm
-1Respectively has a peak; Intensity according to the peak has 2931cm from height successively to hanging down in addition
-1, 1430cm
-1, 1338cm
-1, 1236cm
-1Four peaks.
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|---|---|---|---|
| CN 200710118746 CN101342199B (en) | 2007-07-13 | 2007-07-13 | Chinese ephedra prescription particle, preparation method and quality control method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102512324A (en) * | 2012-01-07 | 2012-06-27 | 贵阳新天药业股份有限公司 | Dry granulation method for cold and cough relieving capsules |
| CN104122221A (en) * | 2014-08-03 | 2014-10-29 | 北京康仁堂药业有限公司 | On-line ultraviolet analysis method for dynamic tendency during extraction process of traditional Chinese medicines |
| CN106267314A (en) * | 2016-10-09 | 2017-01-04 | 常州亚环环保科技有限公司 | A kind of preparation method of antibacterial corrosion-resistant bearing hydrocolloid dressing |
| CN109001143A (en) * | 2018-08-01 | 2018-12-14 | 重庆医科大学 | A kind of mid-infrared light spectrometry of sensitive prediction Chinese ephedra quality characteristic |
| CN112326592A (en) * | 2020-09-16 | 2021-02-05 | 广东一方制药有限公司 | Quality control method of dampness-resolving and toxin-vanquishing composition based on near infrared spectrum |
-
2007
- 2007-07-13 CN CN 200710118746 patent/CN101342199B/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102512324A (en) * | 2012-01-07 | 2012-06-27 | 贵阳新天药业股份有限公司 | Dry granulation method for cold and cough relieving capsules |
| CN104122221A (en) * | 2014-08-03 | 2014-10-29 | 北京康仁堂药业有限公司 | On-line ultraviolet analysis method for dynamic tendency during extraction process of traditional Chinese medicines |
| CN104122221B (en) * | 2014-08-03 | 2016-04-20 | 北京康仁堂药业有限公司 | The online ultra-violet analysis method of extraction of traditional Chinese medicine dynamic trend |
| CN106267314A (en) * | 2016-10-09 | 2017-01-04 | 常州亚环环保科技有限公司 | A kind of preparation method of antibacterial corrosion-resistant bearing hydrocolloid dressing |
| CN109001143A (en) * | 2018-08-01 | 2018-12-14 | 重庆医科大学 | A kind of mid-infrared light spectrometry of sensitive prediction Chinese ephedra quality characteristic |
| CN112326592A (en) * | 2020-09-16 | 2021-02-05 | 广东一方制药有限公司 | Quality control method of dampness-resolving and toxin-vanquishing composition based on near infrared spectrum |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101342199B (en) | 2011-03-02 |
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