CN105147800B - Detection method of ephedra, apricot, gypsum and licorice decoction formula granules - Google Patents
Detection method of ephedra, apricot, gypsum and licorice decoction formula granules Download PDFInfo
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Abstract
The invention discloses a preparation method and a quality control method of a Maxingshigan decoction formula particle, wherein the preparation method comprises the following steps: boiling water 5-15 times of the total amount of the raw materials, adding herba Ephedrae, semen Armeniacae amarum, and radix Glycyrrhizae Preparata decoction pieces, adding Gypsum Fibrosum decoction pieces, decocting and extracting for 2 times, mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure, spray drying the concentrated solution, and dry granulating. The quality control method comprises infrared fingerprint spectrum, thin layer qualitative identification and HPLC content determination. The preparation process can furthest retain the effective components in the compound, fully exert the advantages of the compatibility of the traditional Chinese medicines, embody the concept of the whole traditional Chinese medicine, establish the perfect quality standard of the formula granules of the ephedra, apricot, gypsum and licorice decoction and effectively control the quality of the compound granules.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine formula granules, and particularly relates to a preparation method and a quality control method of a ephedra, apricot, gypsum and licorice decoction formula granule.
Background
The decoction is prepared from herba Ephedrae, semen Armeniacae amarum, Gypsum Fibrosum, and radix Glycyrrhizae Preparata. Has effects in dispersing stagnated heat, clearing lung-heat, and relieving asthma. The recipe is derived from Shang Han Lun (treatise on Cold-induced diseases) of Zhang Zhongjing, which is a modified prescription of Ma Huang Tang. That is, the pungent-cool method is used to treat the syndrome of gypsum which is apt to make cassia twig and warm. The syndrome of the recipe is caused by external attack of wind pathogen, pathogenic heat blocking the lung, or wind pathogen transforming into heat entering the interior, heat obstructing the lung, so the recipe uses fever and cough and asthma as the basis to clear lung qi. The formula uses the ephedra as a monarch to ventilate the lung and relieve asthma, uses the gypsum as a minister in an amount which is more than that of the ephedra and is used together with the ephedra to clear away stagnated heat in the lung, and uses cold and heat to treat the lung without heat assistance and clear away the lung-heat without pathogenic factors, uses bitter temperature of the almond as an assistant to ventilate the lung and lower qi, not only helps the weight reduction of the gypsum to be reduced, but also assists the light diffusion of the ephedra to reduce the lung-heat to be performed in a way of reducing the lung-heat to be performed in a way of relieving asthma and stopping cough, and uses the honey-fried licorice root to tonify qi and harmonize the body fluid.
Modern researches show that the ephedra, apricot kernel, gypsum and licorice decoction has various pharmacological effects of relieving fever, relieving cough, eliminating phlegm, relieving asthma, resisting inflammation, resisting virus, regulating immunologic function and the like, and is widely used for treating various diseases such as upper respiratory tract infection, acute and chronic bronchitis, bronchial asthma, pneumonia, nasosinusitis, wind-heat type common cold and the like clinically.
The traditional Chinese medicine decoction is used as a main dosage form of traditional Chinese medicine clinical medication, has the advantages of addition and subtraction according to symptoms, flexible formula, easy absorption, quick response and the like, and is deeply trusted by patients. But can not meet the living requirements of modern people due to the defects of easy mildew, spoilage, bitter taste, large amount and the like of blending, carrying, temporary decoction and long-term storage. In order to keep the advantages of the decoction and overcome the various defects of the decoction, the traditional Chinese medicine is taken without decoction. The traditional Chinese medicine formula granules are prepared by scientifically processing traditional Chinese medicine decoction pieces under the guidance of the traditional Chinese medicine theory and refining by a modern technology, and compared with the traditional decoction pieces, the traditional Chinese medicine formula granules have the advantages of stable quality, convenient and accurate preparation, convenient carrying and storage and the like, and compared with traditional decoction, the traditional Chinese medicine formula granules have the following extraction characteristics: 1. multi-component extraction is carried out, the multi-drug property is kept, and each traditional Chinese medicine usually contains multiple components; 2. the multi-component process is adopted, the multi-drug effect of a single drug is kept, and the effective components of the drug are retained to the maximum extent; 3. the characteristics of the traditional Chinese medicine decoction are kept by imitating the decocting mode of the traditional Chinese medicine decoction, and the characteristics of the traditional Chinese medicine decoction are reflected.
In China, hundreds of single-ingredient formula granules are on the market, but because the traditional Chinese medicine formula granules are all single-ingredient traditional Chinese medicine extracts at present, people worry about the difference problem of 'common decoction' and 'separate decoction' when the traditional Chinese medicine formula granules are used for 'single-ingredient extraction and mixed taking with water'. The difference between the 'common decoction' and 'separate decoction' provides a new choice for clinical medication of the compound formula granules.
Solves the problem of dispute of single formula granules, fully exerts the advantages of compatibility of the traditional prescription and achieves the effects of attenuation and synergy, and is particularly important. The compound formula particle not only inherits the advantages of the single traditional Chinese medicine formula particle, but also considers the interaction of decoction pieces in the decoction process, conforms to the traditional Chinese medicine theory, and has great value.
Disclosure of Invention
The invention aims to provide a preparation method and a quality control method of a Maxingshigan decoction formula particle.
The invention is realized by the following technical scheme:
a preparation method of a ephedra, almond, gypsum and honey-fried licorice root decoction formula particle is characterized in that the formula particle is prepared from ephedra, bitter almond, gypsum and honey-fried licorice root decoction pieces in a mass ratio of 1-5:1-5:5-10:1-5, and comprises the following steps:
a. boiling water 5-15 times of the total amount of the raw materials, adding herba Ephedrae, semen Armeniacae amarum, and radix Glycyrrhizae Preparata decoction pieces, adding Gypsum Fibrosum decoction pieces, and decocting for 0.5-2 hr to obtain first decoction; adding water with 5-10 times of the total amount of the raw materials into the residues after the first decoction, and decocting and extracting for 0.5-2 hours to obtain a second decoction;
b. combining the two decocted filtrates, filtering, and concentrating the filtrate under vacuum and reduced pressure to obtain a concentrated solution with the relative density of 1.00-1.16;
c. spray drying the concentrated solution to obtain spray dried powder, adding maltodextrin into the spray dried powder, and performing dry granulation to obtain 16-40 mesh Maxingshigan decoction formula granule.
Preferably, the preparation method of the ephedra, apricot kernel, gypsum and licorice decoction formula particle comprises the following steps:
a. boiling water with the weight 10 times of the total feeding amount, adding herba Ephedrae, semen Armeniacae amarum, and radix Glycyrrhizae Preparata decoction pieces, adding Gypsum Fibrosum decoction pieces, extracting for 1 hr, and decocting; adding water with the weight 8 times of the total feed amount into the residues after the first decoction, boiling, and extracting for 1 hour to obtain second decoction;
b. mixing the two decoction filtrates, filtering, and concentrating under vacuum reduced pressure to obtain a concentrated solution with a relative density of 1.02-1.06;
c. spray drying the concentrated solution to obtain spray dried powder, adding maltodextrin into the spray dried powder, and performing dry granulation to obtain 16-40 mesh Maxingshigan decoction formula granule.
In the step c, the addition amount of the maltodextrin accounts for 0-25% of the weight of the spray-dried powder.
In the step c, the spray drying process parameters are as follows: the air inlet temperature is controlled to be 170-185 ℃, and the air outlet temperature is controlled to be 85-95 ℃.
The invention also provides a quality control method of the ephedra, apricot kernel, gypsum and licorice decoction formula granules prepared by the preparation method, which comprises one or more of the following methods:
(1) the quality control method by using the infrared fingerprint spectrum comprises the following steps:
and (3) extracting a sample: taking a proper amount of ephedra, apricot kernel, gypsum and licorice decoction formula particles, grinding, taking 0.5g, adding 20ml of absolute ethyl alcohol, heating and refluxing for 20 minutes, filtering, and evaporating filtrate to dryness to obtain an absolute ethyl alcohol extract;
infrared spectrum detection: measuring with Fourier transform infrared spectrometer at 4000cm-1－400cm-1DTGS Detector, resolution 4cm-1Scanning for 16 times, deducting interference of water and carbon dioxide in the scanning process, and detecting by a potassium bromide tabletting method, wherein the relative humidity of the environment is lower than 60%; the infrared fingerprint spectrum of the Maxingshigan decoction formula particle is shown in figure 1, and has the following characteristics: strongest peak: peak position 1074.91cm-1The second intensity peak: peak position 2926.73cm-1The stronger peak: peak position 1384.38cm-1It must have 2855.30cm in addition to the above peaks-1、1745.97cm-1、1638.42cm-1、594.15cm -14 peaks;
the infrared fingerprint spectrum of the invention can be an infrared fingerprint spectrum with the correlation reaching more than 90 percent.
(2) Qualitative identification by thin-layer chromatography:
taking a proper amount of formula granules of the ephedra, apricot, gypsum and licorice decoction, grinding, taking 0.5g, adding a plurality of drops of concentrated ammonia test solution, adding 10ml of trichloromethane, heating and refluxing for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution; adding methanol into ephedrine hydrochloride reference to obtain 1mg solution per 1ml as reference solution; performing thin-layer chromatography (appendix VI B of 2010 version of Chinese pharmacopoeia), sucking the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, developing with chloroform-methanol-concentrated ammonia solution (20: 5: 0.5) as developing agent, taking out, air drying, spraying with ninhydrin solution, and heating at 105 deg.C until the spots are clearly developed; displaying the same red spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution;
(3) qualitative identification by thin-layer chromatography:
taking a proper amount of formula granules of the ephedra, apricot kernel, gypsum and licorice decoction, grinding, taking 1.5g, adding 50ml of 45% ethanol solution of 7% sulfuric acid (the volume ratio of concentrated sulfuric acid to 45% ethanol is 7: 100), heating and refluxing for 1 hour, cooling, shaking and extracting for 2 times (20 ml each time) by using petroleum ether (60-90 ℃), combining the petroleum ether solution, evaporating to dryness, and adding 1ml of methanol to dissolve the petroleum ether solution to obtain a sample solution; adding methanol into glycyrrhetinic acid control to obtain 1mg solution per 1ml as control solution; according to a thin-layer chromatography (appendix VI B of the 2010 version of Chinese pharmacopoeia), 10 mul of a sample solution and 5 mul of a reference solution are respectively spotted on the same silica gel GF254And (3) spreading petroleum ether (30-60 ℃) -toluene-ethyl acetate-glacial acetic acid (1: 20: 7: 0.5) serving as a developing agent on the thin-layer plate, taking out, airing, and inspecting under an ultraviolet lamp 254 nm. Spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
(4) the content determination of the Maxingshigan decoction formula particles adopts a high performance liquid chromatography, and comprises the following specific steps:
chromatographic conditions and system applicability test chromatography columns: polar ether is connected with phenyl bonded silica gel as a filling agent; mobile phase: acetonitrile (A) -0.1% phosphoric acid solution (B) was subjected to gradient elution, the procedure of which is shown in the following Table; flow rate: 1 ml/min; detection wavelength: 207 nm; the column temperature is 30 ℃; sample introduction amount: 10 mu l; the number of theoretical plates is not less than 3000 calculated according to ephedrine hydrochloride peak;
preparing reference solution by precisely weighing appropriate amount of ephedrine hydrochloride reference, pseudoephedrine hydrochloride reference, and amygdalin reference, and adding methanol to obtain mixed solution containing 0.1mg of each 1 ml;
preparing a test solution, namely taking a proper amount of the test solution, grinding the test solution into fine powder, taking 0.2g of the test solution, precisely weighing the test solution, placing the test solution in a conical flask with a plug, precisely adding 25ml of aqueous solution, weighing the test solution, carrying out ultrasonic treatment (the power is 200W and the frequency is 25 kHz) for 30 minutes, cooling the test solution, weighing the test solution again, supplementing the weight lost by water, shaking the test solution uniformly, filtering the test solution, and taking a subsequent filtrate to obtain the test solution;
precisely sucking 10 mul of each of the reference solution and the test solution by the measuring method, injecting the solution into a liquid chromatograph, and measuring to obtain the test solution;
the content of herba Ephedrae in 1g granule is not less than 3mg and 1mg calculated by ephedrine hydrochloride and pseudoephedrine hydrochloride, and the content of semen Armeniacae amarum is not less than 15mg calculated by amygdalin.
Compared with the prior art, the invention has the following beneficial effects:
(1) the ephedra, apricot, gypsum and licorice decoction is decocted into the compound formula granules according to the traditional method, compared with the existing single formula granules, the traditional Chinese medicine compatibility advantages can be fully exerted by simply adding the medicines when the granules are taken, the concept of the whole traditional Chinese medicine is reflected, the purposes of reducing toxicity and improving efficacy are ensured, and a new choice is provided for clinical medication;
(2) the main effective component of the bitter almond is amygdalin which gradually generates trace hydrocyanic acid under the action of gastric acid in the digestive tract and has the effect of calming nerve centers, so that respiratory movement tends to be quiet and the effect of relieving cough and asthma is achieved, but the bitter almond is hydrolyzed into prunasin and glucose by the amygdalin at proper water temperature and then further hydrolyzed into hydrocyanic acid, benzaldehyde and glucose, and the hydrocyanic acid which has the effect of relieving cough is taken as gas, so that the hydrocyanic acid gas can be volatilized in the process of slowly decocting by adding water, and the drug effect of the product is directly reduced;
(3) the process adopts the gypsum with heavy weight for final feeding, can reduce the floating of the ephedra which is a light medicinal material, and can prevent the gypsum from sinking to the bottom of the tank to cause insufficient decoction and influence on drug effect, and the gypsum has more bacteria content and cannot kill bacteria due to insufficient decoction;
(4) the invention establishes the technological conditions and the perfect quality standard of the ephedra, apricot, gypsum and licorice decoction formula granules, and can effectively control the quality of the compound granules.
Drawings
Fig. 1 shows a standard infrared fingerprint spectrum of the ephedra, apricot kernel, gypsum and licorice decoction formula granules.
Fig. 2 shows an infrared fingerprint spectrum of the ephedra, apricot kernel, gypsum and licorice decoction formula granules in example 1.
FIG. 3 is a thin layer chromatogram of example 2, wherein 1-3 are Maxingshigan decoction formula granules, 4 is ephedrine hydrochloride, and 5 is a negative sample of Maxingshigan decoction formula granules lacking herba Ephedrae.
Fig. 4 is a thin layer chromatogram of example 3, wherein 1-3 are Maxingshigan decoction formula granules, 4 is glycyrrhetinic acid, and 5 is a Maxingshigan decoction formula granule negative sample lacking radix Glycyrrhizae Preparata.
FIG. 5 is an HPLC chromatogram of the control solution of example 4.
Fig. 6 is an HPLC chromatogram of a sample solution of the ephedra, apricot, gypsum and licorice decoction formulation of example 4.
FIG. 7 is an HPLC chromatogram of the ephedra negative sample solution lacking the ephedra decoction formula of example 4.
FIG. 8 is an HPLC chromatogram of a almond-deficient negative sample solution of the Maxingshigan decoction formula of example 4.
Wherein, the No. 1 peak is ephedrine hydrochloride, the No. 2 peak is pseudoephedrine hydrochloride, and the No. 3 peak is amygdalin.
Detailed Description
The present invention is further illustrated by the following specific embodiments, which are not intended to limit the scope of the invention.
Example 1:
a preparation method of a Maxingshigan decoction formula particle comprises the following steps:
a. boiling 49.9kg of water, adding 1070g of ephedra herb, 1070g of bitter apricot seed and 710g of honey-fried licorice root, adding 2140g of gypsum, and decocting and extracting for 1 hour to obtain first decoction; adding 44.91kg of water into the residues after the first decoction, and decocting and extracting for 1 hour to obtain a second decoction;
b. mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure to obtain concentrated solution with relative density of 1.04 at 95 deg.C;
c. spray drying the concentrated solution, controlling the air inlet temperature at 175-185 deg.C and the air outlet temperature at 85-95 deg.C to obtain spray dried powder, adding appropriate amount of maltodextrin, and dry granulating to obtain MA XING SHI GAN TANG granule with particle size of 16-40 mesh and uniform color.
After preparation, infrared fingerprint spectrum qualitative identification is adopted for the formula granules, and the specific method comprises the following steps:
grinding appropriate amount of the extract, adding 0.5g of anhydrous ethanol 20ml, heating and refluxing for 20 min, filtering, and evaporating the filtrate to dryness to obtain anhydrous ethanol extract; the absolute ethyl alcohol extract is subjected to quality identification by adopting an infrared fingerprint spectrum, and the infrared fingerprint spectrum identification method comprises the following steps: measuring with Fourier transform infrared spectrometer at 4000cm-1~400cm-1DTGS Detector, resolution 4cm-1Scanning for 16 times, deducting interference of water and carbon dioxide in the scanning process, and detecting by a direct potassium bromide tabletting method, wherein the relative humidity of the environment is lower than 60%; maxingshigan decoctionThe infrared fingerprint of the square particles is shown in figure 2 and has the following characteristics: strongest peak: peak position 1074.91cm-1The second intensity peak: peak position 2926.73cm-1The stronger peak: peak position 1384.38cm-1Meanwhile, 1745.97cm appears from high to low according to peak intensity-1、2855.30cm-1、1638.42cm-1、594.15cm -14 peaks.
Example 2:
a preparation method of a Maxingshigan decoction formula particle comprises the following steps:
a. boiling 31.88kg of water, adding 535g of ephedra, 535g of bitter almond and 355g of honey-fried licorice root, adding 700g of gypsum, and decocting and extracting for 1.5 hours to obtain first decoction; adding 21.25kg of water into the residues after the first decoction, and decocting and extracting for 1 hour to obtain a second decoction;
b. mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure to obtain concentrated solution with relative density of 1.02 at 95 deg.C;
c. spray drying the concentrated solution, controlling the air inlet temperature at 175-185 deg.C and the air outlet temperature at 85-95 deg.C to obtain spray dried powder, adding appropriate amount of maltodextrin, and dry granulating to obtain MA XING SHI GAN TANG granule with particle size of 16-40 mesh and uniform color.
After preparation, the formula particles are qualitatively identified by adopting thin-layer chromatography, and the specific method is as follows:
taking a proper amount of the product, grinding, taking 0.5g, adding a plurality of drops of concentrated ammonia test solution, adding 10ml of trichloromethane, heating and refluxing for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution. Adding methanol into ephedrine hydrochloride control to obtain 1mg solution per 1ml as control solution. According to a test of thin-layer chromatography (appendix VI B of the first part of the Chinese pharmacopoeia 2010 edition), 5 mu l of each of the two solutions is absorbed, respectively spotted on the same silica gel G thin-layer plate, a trichloromethane-methanol-concentrated ammonia test solution (20: 5: 0.5) is used as a developing agent, developed, taken out, dried, sprayed with a ninhydrin test solution, and heated at 105 ℃ until spots are clearly developed. The same red spot appears on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution.
Example 3:
a preparation method of a Maxingshigan decoction formula particle comprises the following steps:
a. boiling 14.97kg of water, adding 321g of ephedra, 321g of bitter almond and 213g of honey-fried licorice root, adding 642g of gypsum, and decocting for 2 hours to obtain first decoction; adding 7.49kg of water into the residues after the first decoction, and decocting and extracting for 0.5 hour to obtain a second decoction;
b. mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure to obtain concentrated solution with relative density of 1.06 at 95 deg.C;
c. spray drying the concentrated solution, controlling the air inlet temperature at 175-185 deg.C and the air outlet temperature at 85-95 deg.C to obtain spray dried powder, adding appropriate amount of maltodextrin, and dry granulating to obtain MA XING SHI GAN TANG granule with particle size of 16-40 mesh and uniform color.
After preparation, qualitative identification is carried out on the formula particles by adopting thin-layer chromatography, and the specific method comprises the following steps:
taking 1.5g of the product, adding 50ml of 45% ethanol solution of 7% sulfuric acid, heating and refluxing for 1 hour, cooling, extracting with petroleum ether (60-90 ℃) for 2 times and 20ml each time by shaking, combining the petroleum ether solution, evaporating to dryness, and adding 1ml of methanol to dissolve to obtain a sample solution. Adding methanol into glycyrrhetinic acid control to obtain 1mg solution per 1ml, and making into control solution. According to a thin-layer chromatography (appendix VI B of the 2010 version of Chinese pharmacopoeia), 10 mul of a sample solution and 5 mul of a reference solution are respectively spotted on the same silica gel GF254And (3) developing the thin-layer plate by using petroleum ether (30-60 ℃), toluene, ethyl acetate and glacial acetic acid (1: 20: 7: 0.5) as a developing agent, taking out, airing, and inspecting under an ultraviolet lamp (254 nm). Spots of the same color appear in the chromatogram of the test solution at positions corresponding to those in the chromatogram of the control solution.
Example 4:
a preparation method of a Maxingshigan decoction formula particle comprises the following steps:
a. boiling 34.93kg of water, adding 749g of ephedra herb, 749g of bitter almond and 497g of honey-fried licorice root, adding 1498g of gypsum, and decocting and extracting for 1 hour to obtain first decoction; adding 27.94kg of water into the residues after the first decoction, and decocting and extracting for 1 hour to obtain a second decoction;
b. mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure to obtain concentrated solution with relative density of 1.05 at 95 deg.C;
c. spray drying the concentrated solution, controlling the air inlet temperature at 175-185 deg.C and the air outlet temperature at 85-95 deg.C to obtain spray dried powder, adding appropriate amount of maltodextrin, and dry granulating to obtain MA XING SHI GAN TANG granule with particle size of 16-40 mesh and uniform color.
After the preparation, the content of the formula particles is measured by adopting a high performance liquid chromatography, and the method comprises the following specific steps:
chromatographic conditions and system applicability test chromatography columns: polar ether is connected with phenyl bonded silica gel as a filling agent; mobile phase: acetonitrile (A) -0.1% phosphoric acid solution (B) was subjected to gradient elution, the procedure of which is shown in the following Table; flow rate: 1 ml/min; detection wavelength: 207 nm; the column temperature is 30 ℃; sample introduction amount: 10 mu l; the number of theoretical plates is not less than 3000 calculated according to ephedrine hydrochloride peak;
preparing reference solution by precisely weighing appropriate amount of ephedrine hydrochloride reference, pseudoephedrine hydrochloride reference, and amygdalin reference, and adding methanol to obtain mixed solution containing 0.1mg of each 1 ml;
preparing a test solution, namely taking a proper amount of the test solution, grinding the test solution into fine powder, taking 0.2g of the test solution, precisely weighing the test solution, placing the test solution in a conical flask with a plug, precisely adding 25ml of aqueous solution, weighing the test solution, carrying out ultrasonic treatment (the power is 200W and the frequency is 25 kHz) for 30 minutes, cooling the test solution, weighing the test solution again, supplementing the weight lost by water, shaking the test solution uniformly, filtering the test solution, and taking a subsequent filtrate to obtain the test solution;
precisely sucking 10 mul of each of the control solution and the test solution by the measuring method, injecting the control solution and the test solution into a liquid chromatograph, and measuring to obtain the test solution, wherein the obtained results are shown in the following table;
each 1g of the product contains ephedrine hydrochloride 4.495mg, pseudoephedrine hydrochloride 2.177mg, and amygdalin 33.071 mg.
Comparative example:
a preparation method of a Maxingshigan decoction formula particle comprises the following steps:
decocting herba Ephedrae 749g, semen Armeniacae amarum 749g, radix Glycyrrhizae Preparata 497g, and Gypsum Fibrosum 1498g with water twice, adding 34.93kg of water for the first time, and decocting for 1 hr to obtain a decoction; adding 27.94kg of water into the residues after the first decoction, and decocting and extracting for 1 hour to obtain a second decoction; mixing the two decoctions, filtering, vacuum concentrating the filtrate under reduced pressure to obtain concentrated solution with relative density of 1.05 at 95 deg.C; spray drying the concentrated solution, controlling the air inlet temperature at 175-185 deg.C and the air outlet temperature at 85-95 deg.C to obtain spray dried powder, adding appropriate amount of maltodextrin, and dry granulating to obtain MA XING SHI GAN TANG granule with particle size of 16-40 mesh and uniform color.
The samples of example 4 and comparative example were subjected to content measurement according to the content measurement method in the above quality control method, and the measurement results are shown in the following table 1:
TABLE 1 test results of amygdalin content in example 4 and comparative examples
As can be seen from the above table, after the preparation method adopts boiling water feeding, the content of the active ingredient amygdalin is obviously higher than that of the comparative example, which shows that the preparation method of the invention can furthest reserve the active ingredient amygdalin in the formula.
Claims (4)
1. A detection method of the Maxingshigan decoction formula particles is characterized by comprising the following steps:
(1) the infrared fingerprint spectrum is adopted for detection, and the method comprises the following steps:
and (3) extracting a sample: taking a proper amount of ephedra, apricot kernel, gypsum and licorice decoction formula particles, grinding, taking 0.5g, adding 20ml of absolute ethyl alcohol, heating and refluxing for 20 minutes, filtering, and evaporating filtrate to dryness to obtain an absolute ethyl alcohol extract;
infrared spectrum detection: measuring with Fourier transform infrared spectrometer at 4000cm-1－400cm-1DTGS Detector, resolution 4cm-1Scanning for 16 times, deducting interference of water and carbon dioxide in the scanning process, and detecting by a potassium bromide tabletting method, wherein the relative humidity of the environment is lower than 60%; the infrared fingerprint spectrum of the Maxingshigan decoction formula particle has the following characteristics: strongest peak: peak position 1074.91cm-1The second intensity peak: peak position 2926.73cm-1The stronger peak: peak position 1384.38cm-1It must have 2855.30cm in addition to the above peaks-1、1745.97cm-1、1638.42cm-1、594.15cm-14 peaks;
(2) taking a proper amount of formula granules of the ephedra, apricot, gypsum and licorice decoction, grinding, taking 0.5g, adding a plurality of drops of concentrated ammonia test solution, adding 10ml of trichloromethane, heating and refluxing for 30 minutes, filtering, evaporating filtrate to dryness, and adding 1ml of methanol to dissolve residues to obtain a test solution; adding methanol into ephedrine hydrochloride reference to obtain 1mg solution per 1ml as reference solution; according to a test of an appendix VI B of the first part of the version 2010 of the thin-layer chromatography, sucking 5 mu l of each of the two solutions, respectively dropping the two solutions on the same silica gel G thin-layer plate, taking a chloroform-methanol-concentrated ammonia test solution of which the ratio is 20: 5: 0.5 as a developing agent, developing, taking out, drying in the air, spraying a ninhydrin test solution, and heating at 105 ℃ until spots are clearly developed; displaying the same red spot on the chromatogram of the test solution at the position corresponding to the chromatogram of the control solution;
(3) taking a proper amount of formula granules of the ephedra, apricot kernel, gypsum and licorice decoction, grinding, taking 1.5g, adding 50ml of 45% ethanol solution of 7% sulfuric acid, heating and refluxing for 1 hour, cooling, shaking and extracting for 2 times by 20ml of petroleum ether at the temperature of 60-90 ℃, combining the petroleum ether solution, evaporating to dryness, and adding 1ml of methanol to dissolve to obtain a sample solution; adding methanol into glycyrrhetinic acid control to obtain 1mg solution per 1ml as control solution; according to a thin-layer chromatography (Chinese pharmacopoeia 2010 edition I appendix VI B test), 10 mu l of a sample solution and 5 mu l of a reference solution are respectively spotted on the same silica gel GF254On the thin-layer plate, mixing petroleum ether-toluene-ethyl acetate-glacial acetic acid 1: 20: 7: 0.5 is a developing agent, developingTaking out, air drying, and inspecting under 254nm ultraviolet lamp; spots with the same color appear on the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
(4) the content determination of the Maxingshigan decoction formula particles adopts a high performance liquid chromatography, and comprises the following specific steps:
chromatographic conditions and system applicability test chromatography columns: polar ether is connected with phenyl bonded silica gel as a filling agent; mobile phase: gradient elution is carried out on acetonitrile A-0.1 percent phosphoric acid solution B, and the gradient elution procedure is shown in the following table; flow rate: 1 ml/min; detection wavelength: 207 nm; the column temperature is 30 ℃; sample introduction amount: 10 mu l; the number of theoretical plates is not less than 3000 calculated according to ephedrine hydrochloride peak;
Preparing reference solution by precisely weighing appropriate amount of ephedrine hydrochloride reference, pseudoephedrine hydrochloride reference, and amygdalin reference, and adding methanol to obtain mixed solution containing 0.1mg of each 1 ml;
preparing a test solution by taking a proper amount of the formula granules of the ephedra, apricot, gypsum and licorice decoction, grinding, taking 0.2g of the formula granules, precisely weighing, placing the formula granules in a conical flask with a plug, precisely adding 25ml of aqueous solution, weighing, ultrasonically treating for 30 minutes, cooling, weighing again, supplementing the weight loss by water, shaking up, filtering, and taking a subsequent filtrate;
precisely sucking 10 mul of each of the reference solution and the test solution by the measuring method, injecting the solution into a liquid chromatograph, and measuring to obtain the test solution;
the product contains herba Ephedrae (calculated as ephedrine hydrochloride and pseudoephedrine hydrochloride) at a ratio of not less than 3mg and not less than 1mg per 1g granule, and semen Armeniacae amarum (calculated as amygdalin) at a ratio of not less than 15 mg;
the ephedra, almond, gypsum and honey-fried licorice root decoction piece formula particle is prepared from ephedra, bitter almond, gypsum and honey-fried licorice root decoction pieces according to the mass ratio of 1-5:1-5:5-10:1-5, and the preparation method comprises the following steps:
a. boiling water 5-15 times of the total amount of the raw materials, adding herba Ephedrae, semen Armeniacae amarum, and radix Glycyrrhizae Preparata decoction pieces, adding Gypsum Fibrosum decoction pieces, and decocting for 0.5-2 hr to obtain first decoction; adding water 5-10 times the total amount of the raw materials into the residue after the first decoction, boiling, and decocting for 0.5-2 hr to obtain second decoction;
b. combining the two decocted filtrates, filtering, and concentrating the filtrate under vacuum and reduced pressure to obtain a concentrated solution with the relative density of 1.00-1.16;
c. spray drying the concentrated solution to obtain spray dried powder, adding maltodextrin into the spray dried powder, and performing dry granulation to obtain 16-40 mesh Maxingshigan decoction formula granule.
2. The method for detecting the Maxingshigan decoction formula particle as claimed in claim 1, comprising the steps of:
a. boiling water with the weight 10 times of the total feeding amount, adding herba Ephedrae, semen Armeniacae amarum, and radix Glycyrrhizae Preparata decoction pieces, adding Gypsum Fibrosum decoction pieces, extracting for 1 hr, and decocting; adding water with the weight 8 times of the total feeding amount into the residues after the first decoction, and extracting for 1 hour to obtain second decoction;
b. mixing the two decoction filtrates, filtering, and concentrating under vacuum reduced pressure to obtain a concentrated solution with a relative density of 1.02-1.06;
c. spray drying the concentrated solution to obtain spray dried powder, adding maltodextrin into the spray dried powder, and performing dry granulation to obtain 16-40 mesh Maxingshigan decoction formula granule.
3. The method for testing the Maxingshigan decoction formula granule as claimed in claim 1 or 2, wherein in step c, the amount of maltodextrin added is 0-25% of the weight of the spray dried powder.
4. The method for detecting the ephedra, almond, gypsum and licorice formula particles as claimed in claim 1 or 2, wherein in the step c, the spray drying process parameters are as follows: the air inlet temperature is controlled to be 170-185 ℃, and the air outlet temperature is controlled to be 85-95 ℃.
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| CN105640893B (en) * | 2015-12-29 | 2019-11-12 | 广东一方制药有限公司 | A kind of preparation method and its method of quality control of Longdan Xiegan Tang granule |
| CN105535395A (en) * | 2015-12-29 | 2016-05-04 | 广东一方制药有限公司 | Preparation method and quality control method of suanzaoren decoction formula granules |
| CN105866318A (en) * | 2016-03-16 | 2016-08-17 | 保定冀中药业有限公司 | Thin-layer chromatographic detection method for ephedra stem in ephedra stem-bitter apricot kernel-gypsum-licorice root oral liquid |
| CN105911211B (en) * | 2016-05-24 | 2017-10-13 | 四川逢春制药有限公司 | The detection method of Maxing Cough Syrup |
| CN108267515B (en) * | 2016-12-30 | 2020-10-02 | 广州中医药大学第一附属医院 | Method for detecting content of D-amygdalin and/or L-amygdalin in substance to be detected |
| CN106950292A (en) * | 2017-01-17 | 2017-07-14 | 天津中新药业集团股份有限公司达仁堂制药厂 | A kind of lung-clearing anti-inflammatory ball quality standard detecting method |
| CN108896543A (en) * | 2018-08-15 | 2018-11-27 | 康美保宁（四川）制药有限公司 | A kind of qualitative checking method of FENGRE GANMAO KELI |
| CN109632992A (en) * | 2018-12-21 | 2019-04-16 | 广东方制药有限公司 | The content assaying method of D- amarogentin in a kind of peach kernel granule |
| CN111743867A (en) * | 2020-07-29 | 2020-10-09 | 四川新绿色药业科技发展有限公司 | Preparation method and quality control method of bamboo leaf and gypsum decoction formula granules |
| CN111729054A (en) * | 2020-08-19 | 2020-10-02 | 广东一方制药有限公司 | Dampness-resolving toxin-vanquishing traditional Chinese medicine composition, traditional Chinese medicine preparation, preparation method and application thereof |
| CN116139164B (en) * | 2023-04-21 | 2023-07-11 | 北京中医药大学 | Supramolecular hydrogel derived from Maxingshi Gantn decoction and having antipyretic and anti-inflammatory effects |
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| CN102846767A (en) * | 2011-06-30 | 2013-01-02 | 苏州知微堂生物科技有限公司 | Preparation process of integration-type novel formulation of MAXINGGANSHI decoction and production method thereof |
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