CN112717093A - Mongolian medicine, namely six-ingredient costus root granules and preparation method thereof - Google Patents
Mongolian medicine, namely six-ingredient costus root granules and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Mongolian medicine, namely a six-ingredient costustoot granule and a preparation method thereof, and relates to the technical field of Mongolian medicines. The Mongolian medicine, namely the six-ingredient costustoot granules comprise the following raw materials: radix aucklandiae, fructus Gardeniae, fructus Punicae Granati, flos Rhododendri mollis, fructus Amomi rotundus, fructus Piperis Longi and adjuvants; the auxiliary materials capable of improving the taste of the original six-ingredient costustoot powder are adopted, the drug effect of the original six-ingredient costustoot powder is not influenced, and the compliance of taking by patients is enhanced. In addition, the invention also provides a preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules, which comprises the following steps: grinding and crushing the raw materials except the auxiliary materials to obtain coarse powder, sterilizing the coarse powder and primarily sieving to obtain refined powder, mixing the refined powder and the auxiliary materials, adding the mixture into a granulator, uniformly mixing to obtain a soft material, granulating, drying, grading, secondarily sieving the soft material, and mixing in a mixer to obtain Mongolian medicine, namely the six-ingredient costustoot granules; not only can ensure that the medicine property in the medicinal materials is not easy to lose, but also the Mongolian medicine, namely the six-ingredient costustoot granules are convenient to take and quick to absorb.
Description
Technical Field
The invention relates to the technical field of Mongolian medicines, and particularly relates to Mongolian medicine Liuwei Muxiang granules and a preparation method thereof.
Background
The six ingredients aucklandia root powder is recorded in the pharmacopoeia of 2015 edition of Chinese pharmacopoeia and is an proved prescription of Mongolian medicine. The original preparation is characterized in that all the medicinal materials in the prescription are directly crushed and subpackaged to prepare the traditional Chinese medicine preparation. The dosage is not accurate, the process is simple, and only the raw materials are crushed and mixed, so that the defects of bitter, spicy, sour and large dosage of finished products, strong irritation to the pharynx and the esophagus, difficulty in swallowing and the like are caused, patients feel afraid of taking medicines, particularly children are not facilitated to take medicines, the compliance of the medicines is greatly reduced, the 'difficulty in drinking' seems to become a pronoun of Mongolian medicines, and the development and the application of the Mongolian medicines are restricted to a certain extent.
The traditional decoction, powder and capsule have simple and easy preparation method, but need to be prepared when being used, are easy to go mouldy and inconvenient to carry if being placed for a long time, are inconvenient to take if a patient goes out, have large taking volume and bitter taste, are especially difficult to take by children, and are difficult to extract fat-soluble and insoluble components in the medicinal materials completely.
Disclosure of Invention
The invention aims to provide Mongolian medicine six-ingredient costus root granules, namely granules for promoting qi circulation and relieving pain, wherein the Mongolian medicine six-ingredient costus root granules adopt auxiliary materials capable of improving the taste of the original six-ingredient costus root powder, do not influence the drug effect of the original six-ingredient costus root powder and enhance the compliance of patients taking.
The invention also aims to provide a preparation method of the Mongolian medicine six-ingredient costustoot granules, which can ensure that the medicine property of the medicinal materials is not easy to lose, and the produced Mongolian medicine six-ingredient costustoot granules can be directly taken with warm water, are convenient to take, are easier to disintegrate in the stomach compared with capsules, take effect faster and are easier to absorb. In addition, compared with decoction and powder, the produced Mongolian medicine Liuwei Muxiang granules have smaller irritation, higher administration compliance of patients, difficult moisture absorption and mildewing after long-term storage and more convenient carrying.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
On one hand, the embodiment of the application provides Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following raw materials in parts by weight: 150 portions of costustoot, 100 portions of gardenia, 200 portions of pomegranate, 50 to 150 portions of Chinese azalea flower, 50 to 150 portions of round cardamom, 50 to 150 portions of long pepper and 350 portions of auxiliary material.
On the other hand, the embodiment of the application provides a preparation method of Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following steps: grinding and crushing the raw materials except the auxiliary materials to obtain coarse powder, sterilizing the coarse powder and primarily sieving to obtain refined powder, mixing the refined powder and the auxiliary materials, adding the mixture into a granulator, uniformly mixing to prepare soft materials, granulating, drying, grading, secondarily sieving the soft materials, and mixing in a mixer to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
the embodiment of the invention provides Mongolian medicine six-ingredient costustoot granules, which take Mongolian medicine theory as guidance, take compound Mongolian medicine decoction pieces as raw materials, add auxiliary materials capable of improving the taste and shape of the traditional six-ingredient costustoot powder, improve the taste of the original six-ingredient costustoot powder, change the shape of the traditional six-ingredient costustoot powder, avoid traditional decoction, powder, capsules and the like, are convenient to take, have good absorption effect and convenient to store, and the content of each bag of granules is fixed, so that the dosage is convenient to calculate.
In addition, the embodiment of the invention also provides a preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules, and production processes such as crushing, granulating and the like are adopted, so that the processes of heating, concentrating, extracting and the like in decoction and powder are abandoned, and the property of the medicine in the medicinal materials is ensured not to be easily lost. The Mongolian medicine, namely the six-ingredient costustoot granules can be directly taken with warm water, are convenient to take, are easier to disintegrate in the stomach compared with capsules, take effect more quickly and are easier to absorb. In addition, compared with decoction and powder, the produced Mongolian medicine Liuwei Muxiang granules have smaller irritation, higher administration compliance of patients, difficult moisture absorption and mildewing after long-term storage and more convenient carrying.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a thin layer chromatogram of a test solution I and a reference solution I in test example 1 of the present invention;
FIG. 3 is a thin layer chromatogram (under an ultraviolet lamp) of a test solution I and reference solutions II, III, and IV in test example 1 according to the present invention;
FIG. 4 is a thin layer chromatogram (under sunlight) of a test solution I and control solutions II, III and IV in test example 1 of the present invention;
FIG. 5 is a thin layer chromatogram of a test solution II and a control solution V in test example 1 of the present invention;
FIG. 6 is a liquid chromatogram of control solutions VI and VII in test example 1;
FIG. 7 is a liquid chromatogram of test solution III in test example 1 of the present invention;
FIG. 8 is a liquid chromatogram of a control solution VIII in test example 1 of the present invention;
FIG. 9 is a liquid chromatogram of test solution four in test example 1 of the present invention;
FIG. 10 is a liquid chromatogram of a control solution nine in test example 1 of the present invention;
FIG. 11 is a liquid chromatogram of test solution five in test example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The embodiment of the application provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following raw materials in parts by weight: 150 portions of costustoot, 100 portions of gardenia, 200 portions of pomegranate, 50 to 150 portions of Chinese azalea flower, 50 to 150 portions of round cardamom, 50 to 150 portions of long pepper and 350 portions of auxiliary material. The auxiliary materials capable of adjusting the taste and the mouthfeel of the six-ingredient costustoot powder and improving the form are added into the traditional formula of the six-ingredient costustoot powder, compared with the original decoction, the six-ingredient costustoot powder is smaller in taking volume and easier to carry, is taken by directly flushing water, is more convenient to take, has fixed content of each bag of granules, and cannot cause indefinite taking dose because the granules need to be decocted into the decoction. Compared with the original powder, the granule has the advantages of no segregation of various components, reduced dispersibility, adhesiveness, agglomeration, and hygroscopicity, and convenient storage. Compared with capsules, the granules can be directly absorbed by human bodies after being taken, beneficial components in the granules are not needed to be absorbed by the human bodies after the outer-layer coating is disintegrated like capsules, the absorption speed is higher, the granules are easier to be absorbed by the human bodies, and the loss of the beneficial components in the granules is avoided.
In some embodiments of the present invention, the Mongolian medicine, namely the six-ingredient costustoot granules, comprise the following raw materials by weight: 200 parts of costustoot, 150 parts of gardenia, 100 parts of pomegranate, 100 parts of Chinese azalea flower, 100 parts of round cardamom, 100 parts of long pepper and 300 parts of auxiliary materials.
The embodiment is a better formula of the Mongolian medicine, namely the six-ingredient costustoot granules, so that the medicine properties of the medicinal materials can be better cooperated with each other, and the medicinal materials are not influenced with each other. In addition, the prepared Mongolian medicine of six ingredients of costustoot granules has better taste and more stable shape.
In some embodiments of the invention, the adjuvant comprises one or more of sucrose, starch, a flavoring agent, a disintegrating agent, and a wetting agent. The sucrose can increase sweetness of Mongolian medicine of six ingredients of radix aucklandiae granules, improve taste of Mongolian medicine of six ingredients of radix aucklandiae granules, and the sucrose also has hygroscopicity, so as to avoid deliquescence of Mongolian medicine of six ingredients of radix aucklandiae granules. The starch can bond various raw materials in the Mongolian medicine Liuwei Muxiang granules together, so that the raw materials are better prepared into granules, preferably 10% starch slurry is used, and the bonding effect is better. The flavoring agent can improve the smell and taste of Mongolian medicine, such as LIUWEIMUXIANG granule, and reduce its bitter taste. The disintegrating agent can make Mongolian medicine Liuwei Muxiang granule disintegrate more quickly, and is helpful for human body absorption. The wetting agent can reduce the surface tension of Mongolian medicine of six ingredients of costus root granules, so that the Mongolian medicine of six ingredients of costus root granules can be better dissolved and absorbed by human body.
In addition, the invention also provides a preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules, which comprises the following steps: grinding and crushing the raw materials except the auxiliary materials to obtain coarse powder, sterilizing the coarse powder and primarily sieving to obtain refined powder, mixing the refined powder and the auxiliary materials, adding the mixture into a granulator, uniformly mixing to prepare soft materials, granulating, drying, grading, secondarily sieving the soft materials, and mixing in a mixer to obtain the Mongolian medicine, namely the six-ingredient costustoot granules. The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules, does not comprise the steps of decoction, concentration, paste collection and the like in the traditional powder and decoction, simplifies the operation steps, and avoids the loss of medicine properties in the traditional Chinese medicinal materials or the denaturation of beneficial components in the traditional Chinese medicinal materials due to high temperature in the processes of decoction, concentration and paste collection.
In some embodiments of the invention, the sterilizing and primary sieving comprises heating the crude powder to 50-60 deg.C, maintaining for 1-3h, and sieving with 100 mesh sieve to obtain refined powder. Wherein preferentially put into foraminiferous tray with coarse powder and heat in, guarantee that coarse powder process can the thermally equivalent, effectively kill most miscellaneous fungus, get rid of the bold impurity in the coarse powder process after sieving, avoid fashioned granule not full, not mellow and full.
In some embodiments of the present invention, the granulator is a wet mixing granulator, and the mixing time is 25-35 min. Compared with other granulators, the wet mixing granulator can complete the procedures of mixing, humidifying, granulating and the like at one time, does not need to be operated step by step, simplifies the operation steps and reduces the difficulty of operators. The processing time interval can fully and uniformly mix the refined powder, and avoid the formed particles from being unsaturated and not round.
In some embodiments of the present invention, the granulating and drying comprises the steps of sieving the soft material through a 12-14 mesh sieve to obtain wet granules, and drying the wet granules in an oven at 50-60 ℃ for 2-4h to obtain dried granules. Wherein 10% starch slurry is added when preparing soft material, and sieving is carried out when the soft material is held by hand to be agglomerated and loosened. And drying the wet particles to ensure that the formed particles have stable structures and can not collapse in the subsequent preparation process.
In some embodiments of the invention, the granulating comprises the steps of placing the dried granulation in a swing granulator, sieving through a 14-16 mesh sieve and sieving the granules. The swing granulator is preferably a YK160 swing granulator, the YK160 swing granulator is compact in structure and simple in operation mode, meshes and sieve meshes can be automatically adjusted according to requirements of customers, and whether a screen is damaged or not needs to be checked before use. During screening, particles without black spots and foreign matters are selected.
In some embodiments of the present invention, the secondary sieving comprises the steps of placing the prepared granules in a rotary vibrating sieve for sieving to obtain intermediate granules, and sieving the intermediate granules to obtain qualified granules. Wherein, when the intermediate granules are sieved, the intermediate granules which can pass through the first sieve but cannot pass through the fifth sieve are qualified granules, and the eliminated intermediate granules during sieving are not more than 15% of the total number, otherwise, the intermediate granules are unqualified.
In some embodiments of the present invention, the coarse mesh and the fine mesh in the aforementioned rotary vibration sieve are 10 meshes and 60 meshes; and (3) placing the qualified granules into a mixer to mix for 10-20min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules. The coarse screen in the rotary vibration screen is arranged on the upper layer of the rotary vibration screen and used for removing large-sized substances in the upper layer, and the fine screen is arranged on the lower layer and used for screening out fine powder.
After the Mongolian medicine, namely the six-ingredient costus root granules are prepared, the Mongolian medicine, namely the six-ingredient costus root granules are subpackaged and packaged. During subpackaging, the packaging amount is adjusted according to the required weight of each bag, the operation is carried out according to the particle subpackaging post SOP and the particle subpackaging post standard operating regulation, the packaging amount is pumped every 10min in the subpackaging process, the result is flexibly checked, and the packaging amount of each bag is ensured to be within the control range. The bagged granules are put into a special container (4 g in each bag, which is equivalent to 3g of raw medicinal materials), and subpackaging is completed.
During packaging, the operation is carried out according to standard operating rules of label sticking and packaging posts, and small boxes, large boxes, anti-counterfeiting trademarks, batch numbers and outer boxes are filled in the packaging process. And placing a product certificate in the outer box, sealing by using a sealing adhesive tape, and bundling firmly to finish packaging.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following components: 150g of costustoot, 100g of gardenia, 50g of pomegranate, 50g of Chinese azalea flower, 50g of round cardamom, 50g of long pepper, 150g of cane sugar and 100g of starch.
The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules comprises the following steps: grinding and crushing raw materials except the sucrose and the starch to obtain coarse powder, heating the coarse powder to 50 ℃, keeping the temperature for 1h, and then sieving the coarse powder through a 100-mesh sieve to obtain refined powder, mixing the refined powder and the sucrose, adding the mixture into a wet mixing granulator, uniformly mixing for 25min, adding 10% starch slurry prepared from the starch during the mixing, preparing into a soft material, and taking out the soft material when the soft material is held by hands to be agglomerated and is loosened by loose hands. Sieving the soft material with 12 mesh sieve to obtain wet granules, and drying the wet granules in an oven at 50 deg.C for 2 hr to obtain dry granules. The dried granules were put into a YK160 swing granulator for granulation and sieved through a 14-mesh sieve to select the finished granules without foreign matter and black spots. And (3) putting the prepared granules into a rotary vibration sieve for sorting to obtain intermediate granules, sorting the intermediate granules to obtain qualified granules which can pass through a first sieve and can not pass through a fifth sieve, and calculating whether the ratio of the eliminated intermediate granules to the total amount exceeds 15%. And (3) placing the qualified granules into a mixer to mix for 10min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Example 2
The embodiment provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following components: 250g of costustoot, 200g of gardenia, 150g of pomegranate, 150g of Chinese azalea flower, 150g of round cardamom, 150g of long pepper, 200g of cane sugar, 100g of starch, 10g of flavoring agent, 10g of disintegrating agent and 30g of wetting agent.
The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules comprises the following steps: grinding and crushing raw materials except the sucrose and the starch to obtain coarse powder, heating the coarse powder to 60 ℃, keeping the temperature for 3 hours, then sieving the coarse powder by a 100-mesh sieve to obtain refined powder, mixing the refined powder with the sucrose, the flavoring agent, the disintegrating agent and the wetting agent, adding the mixture into a wet mixing granulator, uniformly mixing for 35 minutes, adding 10% starch slurry prepared from the starch during the mixing, preparing into a soft material, and taking out the soft material when the soft material is held into a mass by hands and is loosened by hands. Sieving the soft material with 14 mesh sieve to obtain wet granule, and drying in 60 deg.C oven for 4 hr to obtain dry granule. The dried granules were put into a YK160 swing granulator for granulation and sieved through a 16-mesh sieve to select the finished granules without foreign matter and black spots. And (3) putting the prepared granules into a rotary vibration sieve for sorting to obtain intermediate granules, sorting the intermediate granules to obtain qualified granules which can pass through a first sieve and can not pass through a fifth sieve, and calculating whether the ratio of the eliminated intermediate granules to the total amount exceeds 15%. And (3) placing the qualified granules into a mixer to mix for 20min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Example 3
The embodiment provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following components: 200g of costustoot, 150g of gardenia, 100g of pomegranate, 100g of Chinese azalea flower, 100g of round cardamom, 100g of long pepper, 150g of cane sugar, 100g of starch, 10g of flavoring agent, 10g of disintegrating agent and 30g of wetting agent.
The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules comprises the following steps: grinding and crushing raw materials except the sucrose and the starch to obtain coarse powder, heating the coarse powder to 55 ℃, keeping the temperature for 2 hours, then sieving the coarse powder by a 100-mesh sieve to obtain refined powder, mixing the refined powder with the sucrose, the flavoring agent, the disintegrating agent and the wetting agent, adding the mixture into a wet mixing granulator, uniformly mixing for 30 minutes, adding 10% starch slurry prepared from the starch during the mixing, preparing into a soft material, and taking out the soft material when the soft material is held into a mass by hands and is loosened by hands. Sieving the soft material with 13 mesh sieve to obtain wet granule, and drying in oven at 55 deg.C for 3 hr to obtain dry granule. The dried granules were put into a YK160 swing granulator for granulation and sieved through a 15-mesh sieve to select the finished granules without foreign matter and black spots. And (3) putting the prepared granules into a rotary vibration sieve for sorting to obtain intermediate granules, sorting the intermediate granules to obtain qualified granules which can pass through a first sieve and can not pass through a fifth sieve, and calculating whether the ratio of the eliminated intermediate granules to the total amount exceeds 15%. And (3) placing the qualified granules into a mixer to mix for 15min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Example 4
The embodiment provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following components: 180g of costustoot, 130g of gardenia, 80g of pomegranate, 80g of Chinese azalea flower, 80g of round cardamom, 80g of long pepper, 150g of cane sugar, 80g of starch, 10g of flavoring agent, 10g of disintegrating agent and 30g of wetting agent.
The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules comprises the following steps: grinding and crushing raw materials except the sucrose and the starch to obtain coarse powder, heating the coarse powder to 53 ℃, keeping the temperature for 1.5h, and then sieving by a 100-mesh sieve to obtain refined powder, mixing the refined powder with the sucrose, the flavoring agent, the disintegrating agent and the wetting agent, adding the mixture into a wet mixing granulator, uniformly mixing for 28min, adding 10% starch slurry prepared from the starch during the mixing, preparing into a soft material, and taking out the soft material when the soft material is held by hands to be agglomerated and is loosened by hands. Sieving the soft material with 13 mesh sieve to obtain wet granule, and drying the wet granule in an oven at 53 deg.C for 2.5 hr to obtain dry granule. The dried granules were put into a YK160 swing granulator for granulation and sieved through a 15-mesh sieve to select the finished granules without foreign matter and black spots. And (3) putting the prepared granules into a rotary vibration sieve for sorting to obtain intermediate granules, sorting the intermediate granules to obtain qualified granules which can pass through a first sieve and can not pass through a fifth sieve, and calculating whether the ratio of the eliminated intermediate granules to the total amount exceeds 15%. And (3) putting the qualified granules into a mixer to mix for 13min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Example 5
The embodiment provides a Mongolian medicine, namely a six-ingredient costustoot granule, which comprises the following components: 220g of costustoot, 170g of gardenia, 120g of pomegranate, 120g of Chinese azalea flower, 120g of cardamom, 120g of long pepper, 170g of cane sugar, 100g of starch, 10g of flavoring agent, 10g of disintegrating agent and 30g of wetting agent.
The preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules comprises the following steps: grinding and crushing raw materials except the sucrose and the starch to obtain coarse powder, heating the coarse powder to 57 ℃, keeping the temperature for 2.5 hours, and then sieving the coarse powder through a 100-mesh sieve to obtain refined powder, mixing the refined powder with the sucrose, the flavoring agent, the disintegrating agent and the wetting agent, adding the mixture into a wet mixing granulator, uniformly mixing for 32 minutes, adding 10% starch slurry prepared from the starch during the mixing, preparing into a soft material, and taking out the soft material when the soft material is held into a mass by hands and is loosened by hands. Sieving the soft material with 13 mesh sieve to obtain wet granule, and drying the wet granule in oven at 57 deg.C for 3.5 hr to obtain dry granule. The dried granules were put into a YK160 swing granulator for granulation and sieved through a 15-mesh sieve to select the finished granules without foreign matter and black spots. And (3) putting the prepared granules into a rotary vibration sieve for sorting to obtain intermediate granules, sorting the intermediate granules to obtain qualified granules which can pass through a first sieve and can not pass through a fifth sieve, and calculating whether the ratio of the eliminated intermediate granules to the total amount exceeds 15%. And (3) placing the qualified granules into a mixer to mix for 17min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
Test example 1
The Mongolian medicine Liuwei Muxiang granules prepared in the example 3 are taken to carry out quality standard inspection, wherein the quality standard mainly comprises a character index, a microscopic identification index, a thin-layer chromatography identification index and a content determination index. Wherein the trait indicators include: the Mongolian medicine, namely the six-ingredient costus root granules are yellow or tawny granules, and have fragrant smell, pungent taste and bitter taste; the microscopic identification indexes comprise: the Mongolian medicine, namely the six-ingredient costus root granules have microscopic characteristics of gardenia, costus root, pomegranate, round cardamom and long pepper under microscopic observation; the thin-layer chromatography identification indexes comprise: the chromatogram of the test sample of Mongolian medicine, namely the six-ingredient costus root granules, and the corresponding positions of the chromatograms of the jasminoidin, the costustoot, the rhododendron molle and the long pepper contrast medicinal materials show spots with the same color; the content determination indexes comprise: each 1g of Mongolian medicine, LIUWEIMUXIANG granule, comprises costunolide and dehydrocostunolide above 3.7mg, jasminoidin above 13.5mg and piperine above 18 mg. The instrument and the reagent mainly used in the method comprise the following instruments: microscope, micrometer, mortar, glass slide, cover glass, alcohol lamp, graduated flask, round flask, straight condenser tube, electric heating jacket, filter, tray balance, evaporating dish, spotter, silica gel G thin layer plate, ultraviolet sample application analyzer, chromatography cylinder, oven, high performance liquid chromatograph, analytical balance, pipette, ultrasonic cleaner, conical flask with plug, volumetric flask and microfiltration membrane (0.45 um). The method comprises the following reagents: chloral hydrate solution, diethyl ether, ethyl acetate, ethanol, acetone, formic acid, sulfuric acid, n-butanol, cyclohexane, methanol, antimony trichloride, chloroform, acetonitrile (chromatographically pure), water (double-distilled water) and methanol (chromatographically pure).
Detecting character indexes: takes Mongolian medicine of six ingredients of costus root granules, looks the shape, smells the smell and tastes the taste.
(II) microscopic identification index detection: taking Mongolian medicine, namely six-component costus root particles, grinding and crushing the Mongolian medicine, then loading the Mongolian medicine into tablets by using a chloral hydrate solution, and observing the tablets under a microscope.
And (III) detecting identification indexes of thin-layer chromatography: collecting product lg, adding diethyl ether 18ml, shaking for 12min, discarding ethyl ether solution, volatilizing diethyl ether from residue, adding ethyl acetate 18ml, heating and refluxing in water bath for 70min, filtering, evaporating filtrate, and dissolving with ethanol 2.5ml to obtain sample solution I. Taking jasminoidin reference substance, adding ethanol to obtain 4.5mg/ml solution as reference substance solution I. Performing thin layer chromatography (general rule 0502) test, sucking 5ul of the above two solutions, respectively dropping on the same silica gel G thin layer plate, developing with ethyl acetate-acetone-formic acid-water (10:7:2:0.5) as developing agent one, taking out, air drying, spraying with 10% sulfuric acid-ethanol solution, and heating until the spots are clearly developed. And observing whether spots with the same color appear on the first chromatogram of the test solution at the positions corresponding to the first chromatogram of the reference solution.
Collecting radix aucklandiae control material and fructus Piperis Longi control material 0.5g respectively, adding diethyl ether 10ml respectively, shaking for 8min, discarding diethyl ether solution, removing diethyl ether from residue, adding ethyl acetate 12ml, heating and refluxing in water bath for 70min, filtering, evaporating filtrate, and adding ethanol 2.5ml to dissolve to obtain control solutions II and III. Adding ethanol into piperine control to obtain 1.2mg/ml solution as control solution IV. Performing thin layer chromatography (general rule 0502) test, sucking 5ul of the first sample solution and the second, third and fourth reference solutions, respectively, dropping on the same silica gel G thin layer plate, developing with cyclohexane-acetone (10:3) as developing agent II, taking out, air drying, spraying 10% sulfuric acid-ethanol solution, air drying, and inspecting under ultraviolet lamp (365 nm). Observing whether fluorescent spots with the same color appear in the positions corresponding to the positions of the second chromatogram and the fourth chromatogram of the reference solution in the chromatogram of the test solution I; heating until the spots are clearly developed, and inspecting in sunlight to determine whether spots of the same color appear in the first chromatogram of the test solution at the positions corresponding to the third chromatogram of the control solution.
Taking 3g of the product, adding 28ml of water-saturated n-butanol, performing ultrasonic treatment for 35min, filtering the filtrate, evaporating to dryness, and adding 2.5ml of absolute ethanol for dissolving to obtain a sample solution II. Preparing control solution five by the same method with flos Rhododendri mollis 0.5g as control medicinal material. Performing thin layer chromatography (general rule 0502) test, sucking the two solutions, respectively dripping each l0ul on the same silica gel G thin layer plate, making into strip, developing with cyclohexane-ethyl acetate-methanol (5:4:1) as developing agent III, taking out, air drying, spraying 10% antimony trichloride-trichloromethane solution, heating until the spots are clearly developed, and inspecting under ultraviolet lamp (365 nm). And observing whether the positions of the second chromatogram of the test solution and the fifth chromatogram of the reference solution show fluorescence spots with the same color.
And (IV) content determination index detection: taking appropriate amount of costunolide and dehydrocostuslactone as reference substances, precisely weighing, and adding methanol to obtain 62ug/ml mixed solution to obtain six and seven reference substances. Precisely weighing about lg of the product, placing the weighed product in a conical flask with a plug, precisely adding 55ml of methanol, sealing the plug, weighing, standing overnight, ultrasonically treating for 35 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a test solution III. Precisely sucking 10ul of each of the six and seven reference solutions and the three test solutions, and injecting into a high performance liquid chromatograph (using octadecylsilane chemically bonded silica as filler, methanol-water (65:35) as mobile phase, and detection wavelength of 225nm) to measure content.
Taking a proper amount of geniposide reference substance, precisely weighing, and adding methanol to obtain a solution of 28ug/ml, to obtain a reference substance solution eight. Weighing 0.6g of the powder, accurately weighing, placing in a conical flask with a plug, accurately adding 30ml of methanol, weighing, ultrasonically treating for 25 minutes, cooling, weighing again, supplementing the weight loss with methanol, shaking up, and filtering. Precisely measuring 10ml of the subsequent filtrate, placing the subsequent filtrate in a 25ml measuring flask, adding methanol to the scale, and shaking up to obtain a test sample solution IV. Precisely sucking 10 μ l of each of the eight reference solutions and the four test solutions, and measuring the content in a high performance liquid chromatograph (using octadecylsilane chemically bonded silica as filler, acetonitrile-water (15:85) as mobile phase, and detection wavelength of 238 nm).
Taking a proper amount of piperine reference substance, precisely weighing, placing into a brown measuring flask, and adding anhydrous ethanol to prepare solutions of 22ug/ml each to obtain a reference substance solution nine. Taking 0.1g of the powder in the product, precisely weighing, placing in a 50ml brown measuring flask, adding 45ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 35 minutes, cooling, adding absolute ethyl alcohol to the scale, shaking up, filtering, precisely measuring 10ml of subsequent filtrate, placing in a 25ml brown measuring flask, adding absolute ethyl alcohol to the scale, shaking up, filtering, and taking the subsequent filtrate to obtain a sample solution V. Precisely sucking 10 μ l of each of the nine reference solutions and the five test solutions, and measuring the content in high performance liquid chromatograph (using octadecylsilane chemically bonded silica as filler, methanol-water (77:23) as mobile phase, and detecting wavelength 343 nm).
In the detection of character identification indexes, the Mongolian medicine Liuwei Muxiang granules prepared in the example 3 are yellow granules, fragrant, pungent and bitter in taste and meet the standard.
In the microscopic identification index detection, the pericarp stone cells of the Mongolian medicine Liuwei Muxiang granules prepared in the example 3 are observed to be yellow or light brown, are broken more, are complete and are in long polygonal shapes, rectangular shapes or irregular shapes, have large circular holes in wall thickness and have brownish red cellular cavities, and the microscopic characteristics of the cape jasmine are obtained. The pericarp stone cell is colorless, oval or round-like, the wall thickness and the pore ditch are fine, and the microscopic characteristic of the pomegranate is obtained. The cells of the sclerite sclerenchyma are yellow brown or brownish red, the surface appearance is similar to a polygon, the wall thickness and the cavities contain siliceous blocks, namely the microscopic characteristics of the cardamom. The pericyte is reddish brown, is in a long polygonal shape, and is thickened in a shape of a mural pearl, namely the microscopic characteristic of the long pepper. The diameter of the reticulated duct is 32-90pm, which is the microscopic characteristic of costus root. The pollen grains are in a tetrahedron shape and have 3 germination holes, namely the microscopic characteristics of the rhododendron molle, and the rhododendron molle accords with the standard.
The results of the thin layer chromatography identification index detection are shown in fig. 2-5, wherein 1 in fig. 2 is a reference solution one, and 2, 3 and 4 are test solution one. In fig. 3, 1 is the second control solution, 2 is the third control solution, 3 is the fourth control solution, and 4-6 are the first test solution. In fig. 4, 1-3 are the first sample solution, 4 is the fourth control solution, 5 is the second control solution, and 6 is the fourth control solution. In FIG. 5, 1 is a fifth reference solution, and 2-4 are second test solutions. The development positions of the Mongolian medicine Liuwei Muxiang granules prepared in the example 3 are basically similar to those of the reference substance, which shows that the Mongolian medicine Liuwei Muxiang granules contain geniposide, radix aucklandiae, flos Rhododendri mollis and fructus Piperis Longi and meet the standard.
The results of the content determination index detection are shown in fig. 6-11, where 1 in fig. 6 is reference solution 6, and 2 is reference solution seven. In FIG. 7, 1 is the absorption peak of dehydrocostuslactone in the third sample solution, and 2 is the absorption peak of costuslactone in the third sample solution. By the formula "AFor supplying to×CTo pair/(ATo pair×mFor supplying to/VFor supplying to) "calculated, every 1g of the Mongolian medicine Liuwei Muxiang Keli prepared in example 3 comprises more than 3.7mg of costunolide and dehydrocostunolide, more than 13.5mg of geniposide and more than 18mg of piperine. Wherein, CTo pairConcentration of control solution (. mu.g/ml), ATo pairAs the average peak area of the control solution, mFor supplying toThe sample volume (g), A, is taken of the test sampleFor supplying toIs the average value of the peak area of the test solution, VFor supplying toThe volume (ml) of the test solution is in accordance with the standard.
In summary, the Mongolian medicine six-ingredient costustoot granule provided by the embodiment of the invention takes Mongolian medicine theory as guidance, takes compound Mongolian medicine decoction pieces as raw materials, and adds auxiliary materials capable of improving the taste and shape of the traditional six-ingredient costustoot powder, so that the taste of the original six-ingredient costustoot powder is improved, the shape of the traditional six-ingredient costustoot powder is changed, the traditional decoction, powder, capsule and the like are not needed, the administration is more convenient, the absorption effect is good, the storage is more convenient, in addition, the content of each bag of granules is fixed, and the dosage is convenient to calculate.
In addition, the embodiment of the invention also provides a preparation method of the Mongolian medicine, namely the six-ingredient costustoot granules, and production processes such as crushing, granulating and the like are adopted, so that the processes of heating, concentrating, extracting and the like in decoction and powder are abandoned, and the property of the medicine in the medicinal materials is ensured not to be easily lost. The Mongolian medicine, namely the six-ingredient costustoot granules can be directly taken with warm water, are convenient to take, are easier to disintegrate in the stomach compared with capsules, take effect more quickly and are easier to absorb. In addition, compared with decoction and powder, the produced Mongolian medicine Liuwei Muxiang granules have smaller irritation, higher administration compliance of patients, difficult moisture absorption and mildewing after long-term storage and more convenient carrying. The content of the beneficial components in the Mongolian medicine Liuwei Muxiang granules is high, the characteristics of various beneficial components are also included, and the Mongolian medicine Liuwei Muxiang granules can have a treatment effect on a human body.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. A Mongolian medicine, namely six-ingredient costustoot granules is characterized by comprising the following raw materials in parts by weight: 150 portions of costustoot, 100 portions of gardenia, 200 portions of pomegranate, 50 to 150 portions of Chinese azalea flower, 50 to 150 portions of round cardamom, 50 to 150 portions of long pepper and 350 portions of auxiliary material.
2. The Mongolian medicine, namely the six-ingredient costus root granules according to claim 1, is characterized by comprising the following raw materials in parts by weight: 200 parts of costustoot, 150 parts of gardenia, 100 parts of pomegranate, 100 parts of Chinese azalea flower, 100 parts of round cardamom, 100 parts of long pepper and 300 parts of auxiliary materials.
3. The Mongolian medicine, six-ingredient costus root granules according to claim 1 or 2, wherein the auxiliary materials comprise one or more of sucrose, starch, flavoring agent, disintegrating agent and wetting agent.
4. A process for the preparation of the mongolian medicine liuweixiang granules according to any one of claims 1 to 3, characterized by comprising the following steps: grinding and crushing the raw materials except the auxiliary materials to obtain coarse powder, sterilizing and primarily sieving the coarse powder to obtain refined powder, mixing the refined powder and the auxiliary materials, adding the mixture into a granulator, uniformly mixing the mixture to prepare soft materials, granulating, drying, grading, secondarily sieving the soft materials, and mixing the soft materials in a mixer to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
5. The method for preparing the Mongolian medicine Liuwei Muxiang granules as claimed in claim 4, wherein the sterilizing and primary sieving comprises the steps of heating the crude powder to 50-60 ℃, keeping the temperature for 1-3h and then sieving the crude powder with a 100-mesh sieve to obtain the refined powder.
6. The method for preparing the Mongolian medicine Liuwei Muxiang granules according to claim 5, wherein the granulator is a wet mixing granulator, and the time for mixing is 25-35 min.
7. The method for preparing the Mongolian medicine Liuwei Muxiang granules as claimed in claim 6, wherein the granulating and drying comprises the steps of sieving the soft material through a 12-14-mesh sieve to obtain wet granules, and drying the wet granules in an oven at 50-60 ℃ for 2-4h to obtain the dry granules.
8. The method for preparing the Mongolian medicine Liuwei Muxiang granules according to claim 7, wherein the granulating comprises the steps of placing the dried granules in a swing granulator, sieving with a 14-16 mesh sieve and screening the granules.
9. The method for preparing the Mongolian medicine Liuwei Muxiang granules according to claim 8, wherein the secondary sieving comprises the steps of placing the prepared granules in a rotary vibration sieve for granule selection to obtain intermediate granules, and then sieving the intermediate granules to obtain qualified granules.
10. The method for preparing the Mongolian medicine Liuwei Muxiang granules according to claim 9, wherein the coarse mesh and the fine mesh in the rotary vibrating sieve are 10 meshes and 60 meshes respectively; and (3) mixing the qualified granules in a mixer for 10-20min to obtain the Mongolian medicine, namely the six-ingredient costustoot granules.
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