CN111803463A - Tibetan medicine compound Ruteng capsule and preparation method and quality standard detection method thereof - Google Patents
Tibetan medicine compound Ruteng capsule and preparation method and quality standard detection method thereof Download PDFInfo
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- CN111803463A CN111803463A CN202010559457.1A CN202010559457A CN111803463A CN 111803463 A CN111803463 A CN 111803463A CN 202010559457 A CN202010559457 A CN 202010559457A CN 111803463 A CN111803463 A CN 111803463A
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- A—HUMAN NECESSITIES
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- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
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Abstract
The invention belongs to the technical field of medicines, and particularly relates to a Tibetan medicine compound Ruteng capsule, a preparation method thereof and a quality standard detection method. The preparation method of the Tibetan medicine compound Ruteng capsule comprises the following steps: mixing fructus Chebulae, semen Cassiae, semen Abutili, caulis tinosporae, radix Lamiophlomidis Rotatae, and herba Kyllingae, adding ethanol solution, reflux-extracting for several times, mixing filtrates, concentrating under reduced pressure to obtain concentrated solution, drying, and pulverizing to obtain first mixed fine powder; mixing the obtained first mixed fine powder with Olibanum, adding calcium hydrogen phosphate, pulverizing to obtain second mixed fine powder, drying, sieving, adding silica gel micropowder and magnesium stearate, mixing, and making into capsule. The preparation method provided by the invention improves the compliance of the medicament, is reasonable and feasible, has scientific and controllable quality standard, and has good economic and social benefits.
Description
Technical Field
The invention relates to the technical field of medicines, in particular to a Tibetan medicine compound Ruteng capsule, a preparation method and a quality standard detection method thereof.
Background
Rheumatoid arthritis, which is considered by modern medical theory as a chronic, inflammatory and multisystemic autoimmune disease, is clinically characterized by symmetrical and progressive polyarthritis, and the main pathology of the rheumatoid arthritis is changed into the formation of chronic joint synovium inflammation and the destruction of articular cartilage and bone, which finally result in serious joint deformity and dysfunction. The rheumatoid arthritis has the characteristics of difficult cure, easy relapse, high disability rate and the like, the etiology and pathogenesis of the rheumatoid arthritis are not completely clear at present, and the rheumatoid arthritis is a difficult and difficult disease worldwide. The rheumatoid arthritis is called 'Zhebu' in Tibetan medicine, and belongs to the category of 'yellow water disease'. The Tibetan medicine theory considers that when the external environment influence or the internal environment change of the human body causes the digestive system disorder and the three major factors of dragon, gibba and bacon of the body are abnormal in function to cause imbalance, the dominated yellow water is also directly influenced, so that the quality, quantity and physiological function of the yellow water are all abnormal, and the yellow water disease is formed. Due to the unique geographical environment of high altitude and high cold in Tibetan regions, the Tibetan medicine accumulates abundant experience on the treatment of rheumatoid arthritis, and develops a plurality of compound combinations which are rich in characteristics and have good effects.
At present, the traditional dosage forms of decoction, powder, pills and the like are commonly used in clinic of the Tibetan medicine, the compliance of patients is not good, and the clinical application range of the Tibetan medicine is limited.
Disclosure of Invention
In view of the above, the invention provides a Tibetan medicine compound Ruteng capsule, a preparation method and a quality standard detection method thereof.
The invention provides a Tibetan medicine compound Ruteng capsule which comprises main materials and auxiliary materials, wherein the main materials comprise the following raw materials in parts by mass: 80-120 parts of frankincense, 80-120 parts of myrobalan, 60-100 parts of semen cassiae, 60-100 parts of abelmoschus manihot, 30-70 parts of tinospora sinensis, 30-70 parts of lamiophlomis rotate and 20-60 parts of fleshy aster; the auxiliary materials comprise the following raw materials: calcium hydrogen phosphate, aerosil and magnesium stearate.
The invention also provides a preparation method of the Tibetan medicine compound Ruteng capsule, which comprises the following steps: mixing fructus Chebulae, semen Cassiae, semen Abutili, caulis tinosporae, radix Lamiophlomidis Rotatae, and herba Kyllingae, adding ethanol solution, reflux-extracting for several times, mixing filtrates, concentrating under reduced pressure to obtain concentrated solution, drying, and pulverizing to obtain first mixed fine powder; mixing the obtained first mixed fine powder with Olibanum, adding calcium hydrogen phosphate, pulverizing to obtain second mixed fine powder, drying, sieving, adding silica gel micropowder and magnesium stearate, mixing, and making into capsule.
Furthermore, the usage amount of the calcium hydrophosphate is 20 to 40 percent of the total mass of the first mixed fine powder and the frankincense, the usage amount of the superfine silica powder is 0.3 to 0.8 percent of the mass of the second mixed fine powder, and the usage amount of the magnesium stearate is 0.3 to 0.8 percent of the mass of the second mixed fine powder.
The invention also provides a quality standard detection method of the Tibetan medicine compound masturbation capsule, which specifically comprises the steps of carrying out qualitative identification on frankincense and cassia seed by using a thin-layer chromatography and carrying out quantitative determination on 8-O-acetyl shanzhiside methyl ester by using a high performance liquid chromatography;
the qualitative identification of frankincense comprises the following steps: taking 0.3g of the content of the product, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a test solution; taking 0.2g of frankincense control medicinal material, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a control medicinal material solution; sucking 10 μ L of a test solution and 5 μ L of a control solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether (60-90 deg.C) -ethyl acetate as developing agent at a volume ratio of 19:1, taking out, air drying, spraying with 5% vanillin-sulfuric acid solution, and heating at 105 deg.C until the spots are clearly developed; in the chromatogram of the test solution, main spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
the qualitative identification of the cassia seeds comprises the following steps: taking 3g of the content of the product, adding 30mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20mL of water into the residue for dissolving, adding 2mL of hydrochloric acid, heating in a water bath for 30 minutes, immediately cooling, shaking and extracting with diethyl ether for 2 times, wherein 20mL of the extraction solution is added each time, combining the diethyl ether extraction solutions, volatilizing, and adding 1mL of methanol into the residue for dissolving to obtain a sample solution; adding 10mL of methanol into 1g of semen Cassiae reference material, soaking for 1 hour, filtering, evaporating filtrate to dryness, dissolving the residue in 10mL of water, adding 1mL of hydrochloric acid, heating in water bath for 30 minutes, cooling immediately, shaking with diethyl ether for 2 times, each time extracting for 20mL, mixing diethyl ether extractive solutions, volatilizing, and dissolving the residue in 1mL of methanol to obtain a reference material solution; taking an aurantio-obtusin reference substance, and adding methanol to prepare a solution containing 0.5mg of aurantio-obtusin per 1mL, wherein the solution is used as a reference substance solution; sucking 8 mu L of each of the three solutions, respectively dropping on the same silica gel H thin layer plate, developing by using petroleum ether (30-60 ℃) and acetone as developing agents in a volume ratio of 3:1, taking out, airing, fumigating in ammonia until spots are clearly developed, and observing under sunlight to display spots with the same color in a sample chromatogram at positions corresponding to a reference medicinal material solution chromatogram and a reference substance solution chromatogram;
the quantitative determination of the 8-O-acetyl shanzhiside methyl ester comprises the following steps:
(1) preparation of control solutions: precisely weighing 8-O-acetyl shanzhiside methyl ester reference substance, and adding methanol to obtain solution containing 8-O-acetyl shanzhiside methyl ester 30 μ g per 1 mL;
(2) preparing a test solution: precisely weighing 1.0g of the content of the product, placing the product in a conical flask with a plug, precisely adding 25mL of 70% methanol, sealing the plug, weighing, ultrasonically treating for 40 minutes, cooling, weighing again, supplementing the loss weight with 70% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product;
(3) precisely sucking 10 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Further, in the step (3), the chromatographic conditions of the liquid chromatograph are as follows: octadecyl bonded phase silica gel is used as a filling agent; taking acetonitrile as a mobile phase A and water as a mobile phase B, and performing gradient elution: 0-10 min, 12% of mobile phase A; 10-20 min, 12% mobile phase A → 10% mobile phase A; 20-70 min, 10% of mobile phase A; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the detection wavelength is 235 nm; the theoretical plate number is not less than 4000 calculated according to 8-O-acetyl shanzhiside methyl ester.
Furthermore, the content of 8-O-acetyl shanzhiside methylester in each gram of the content is not less than 0.5 mg.
The technical scheme provided by the invention has the beneficial effects that:
1. the formula of the Tibetan medicine compound milk vine capsule provided by the invention is guided by Tibetan medicine theory, the change rule of compatibility of Tibetan medicine prescription is explored, and the formula is performed by organically combining six ingredients, eight ingredients, seventeen ingredients and three ingredients, so that the Tibetan medicine compound milk vine capsule has the characteristics of multiple target points, multiple links and overall regulation of organisms, and is mainly used for treating the yellow water disease;
2. the preparation method of the Tibetan medicine compound Ruteng capsule provided by the invention ensures the quality of Tibetan medicine, combines the traditional Tibetan medicine with the modern preparation technology, develops the Tibetan medicine into a safe, effective, quality-controllable, convenient-to-take and carry modern preparation form, can improve the compliance of patients, and expands the clinical application range of the compound Ruteng capsule;
3. the invention provides a quality standard detection method of Tibetan medicine compound Ruteng capsules, which accords with relevant regulations of 'Chinese pharmacopoeia' 2015 edition and has scientific and controllable quality standard.
Drawings
Fig. 1 is a flow chart of a preparation method of a Tibetan medicine compound milk vine capsule of the invention.
Fig. 2 is a thin layer chromatogram of frankincense in the Tibetan medicine compound milk vine capsule prepared in example 1 of the invention.
Fig. 3 is a thin layer chromatogram of cassia seed in the Tibetan medicine compound milk vine capsule prepared in example 1 of the present invention.
Fig. 4 is a high performance liquid chromatogram for measuring the content of the Tibetan medicine compound milk vine capsule prepared in the embodiment 1 of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the following examples and accompanying drawings.
Example 1:
weighing 100g of myrobalan, 80g of semen cassiae, 80g of radix mallow, 50g of tinospora sinensis, 50g of lamiophlomis rotata and 40g of fleshy ardisia herb, mixing, performing reflux extraction for 3 times by using 12 times of 60% ethanol, performing 1.5 hours each time, combining filtrates, performing reduced pressure concentration to obtain a concentrated solution, drying at 80 ℃, and crushing to obtain first mixed fine powder; and (3) uniformly mixing the first mixed fine powder with 100g of frankincense, adding calcium hydrogen phosphate accounting for 30% of the total weight of the first mixed fine powder and the frankincense, crushing to obtain second mixed fine powder, drying at 60 ℃, sieving by a 16-mesh sieve, adding micro-powder silica gel accounting for 0.5% of the weight of the second mixed fine powder and 0.5% of magnesium stearate, uniformly mixing, and encapsulating to obtain the Tibetan medicine compound mastra lactea capsule.
The flow chart of the preparation method is shown in figure 1.
In example 1, one part of the Tibetan medicine compound Ruteng capsule is prepared into 650 granules per 1 g.
And (3) identification:
the thin-layer chromatography is utilized to qualitatively identify the frankincense in the Tibetan medicine compound milk rattan capsule prepared in the embodiment 1, and the method specifically comprises the following steps: taking 0.3g of the content of the product, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a test solution; taking 0.2g of frankincense control medicinal material, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a control medicinal material solution; performing thin-layer chromatography (0502 of the four ministerial general rules of the design reside in the Chinese pharmacopoeia 2015), sucking 10 μ L of a sample solution and 5 μ L of a reference medicinal material solution, respectively dropping the sample solution and the reference medicinal material solution on the same silica gel G thin-layer plate, developing by using petroleum ether (60-90 ℃) and ethyl acetate as developing agents in a volume ratio of 19:1, taking out, drying in the air, spraying a 5% vanillin sulfuric acid solution, and heating at 105 ℃ until spots are clearly developed; the main spot with the same color appears on the chromatogram of the test solution at the position corresponding to the chromatogram of the reference solution.
The thin layer chromatogram of the frankincense in the Tibetan medicine compound milk vine capsule prepared in the example 1 is shown in figure 2, and in the figure 2, 1-3 represent a test solution; 4 represents a reference solution of Olibanum; 5 represents a negative sample lacking mastic gum.
The method for qualitatively identifying the cassia seeds in the Tibetan medicine compound milk vine capsule prepared in the embodiment 1 by utilizing the thin-layer chromatography comprises the following steps: taking 3g of the content of the product, adding 30mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20mL of water into the residue for dissolving, adding 2mL of hydrochloric acid, heating in a water bath for 30 minutes, immediately cooling, shaking and extracting with diethyl ether for 2 times, wherein 20mL of the extraction solution is added each time, combining the diethyl ether extraction solutions, volatilizing, and adding 1mL of methanol into the residue for dissolving to obtain a sample solution; adding 10mL of methanol into 1g of semen Cassiae reference material, soaking for 1 hour, filtering, evaporating the filtrate to dryness, dissolving the residue in 10mL of water, adding 1mL of hydrochloric acid, heating in water bath for 30 minutes, immediately cooling, shaking with diethyl ether for 2 times (20 mL each time), mixing the diethyl ether extractive solutions, volatilizing, and dissolving the residue in 1mL of methanol to obtain a reference material solution; taking an aurantio-obtusin reference substance, and adding methanol to prepare a solution containing 0.5mg of aurantio-obtusin per 1mL, wherein the solution is used as a reference substance solution; performing thin-layer chromatography (0502 of the four ministry of the national pharmacopoeia 2015), sucking 8 μ L of each of the three solutions, respectively dropping on the same silica gel H thin-layer plate, developing with petroleum ether (30-60 deg.C) -acetone as developing agent at a volume ratio of 3:1, taking out, air drying, fumigating in ammonia gas until the spots are clear, inspecting under sunlight, and displaying spots of the same color in the chromatogram of the sample at the positions corresponding to the chromatogram of the reference medicinal solution and the chromatogram of the reference solution.
The thin-layer chromatogram of semen Cassiae in the Tibetan medicine compound Ruteng capsule prepared in example 1 is shown in FIG. 3, wherein 1-3 in FIG. 3 represent the test solution; 4 orange obtusin reference; 5 represents semen Cassiae reference material; 6 represents a negative sample lacking cassia seed.
The inspection method of the Tibetan medicine compound Ruteng capsule prepared in the embodiment 1 is carried out according to the following steps:
moisture content: checking according to water content determination method (0832 in the four departments of the version of Chinese pharmacopoeia 2015), wherein the water content is not more than 0.9%;
the difference of the loading amount: checking according to general rules of capsules (0103 in the four-part general rules of 2015 pharmacopoeia);
disintegration time limit: the composition can be completely disintegrated within 30 minutes according to disintegration time limit examination method (0921 in 2015 th four-department general rules of pharmacopoeia of China);
the microbial limit: examine according to general rules of capsules (0103 in the four-department general rules of 2015 pharmacopoeia).
Content determination: the determination is carried out according to high performance liquid chromatography (0512 in the four-department general regulation of the national pharmacopoeia 2015 edition), which comprises the following steps:
chromatographic conditions and system applicability test: octadecyl bonded phase silica gel is used as a filling agent; taking acetonitrile as a mobile phase A and water as a mobile phase B, and performing gradient elution: 0-10 min, 12% of mobile phase A and 88% of mobile phase B; 10-20 min, 12% of mobile phase A → 10% of mobile phase A, 88% of mobile phase B → 90% of mobile phase B; 20-70 min, 10% of mobile phase A and 90% of mobile phase B; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the detection wavelength is 235 nm; the theoretical plate number is not less than 4000 calculated according to 8-O-acetyl shanzhiside methyl ester;
preparation of control solutions: taking a proper amount of 8-O-acetyl shanzhiside methyl ester reference substance, precisely weighing, and adding methanol to prepare a solution containing 30 μ g of 8-O-acetyl shanzhiside methyl ester per 1 mL;
preparation of a test solution: precisely weighing 1.0g of the content of the product, placing the product in a conical flask with a plug, precisely adding 25mL of 70% methanol, sealing the plug, weighing, ultrasonically treating for 40 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product;
and (3) determination: precisely sucking 10 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Per gram of the product contains 8-O-acetyl shanzhiside methyl ester (C)19H28O12) The content should not be less than 0.5 mg.
The high performance liquid chromatogram for measuring the content of the Tibetan medicine compound milk vine capsule prepared in the example 1 is shown in fig. 4, peak 1 represents 8-O-acetyl shanzhiside methyl ester, fig. 4A is the high performance liquid chromatogram of a blank sample (methanol) solution, fig. 4B is the high performance liquid chromatogram of a reference solution, fig. 4C is the high performance liquid chromatogram of a negative sample solution, and fig. 4D is the high performance liquid chromatogram of a test solution.
Example 2:
weighing 90g of myrobalan, 65g of semen cassiae, 85g of abelmoschus manihot, 65g of tinospora sinensis, 55g of lamiophlomis rotata and 50g of fleshy ardisia herb, mixing, performing reflux extraction for 3 times by using 12 times of 60% ethanol, performing 1.5 hours each time, combining filtrates, performing reduced pressure concentration to obtain a concentrated solution, drying at 80 ℃, and crushing to obtain first mixed fine powder; and uniformly mixing the first mixed fine powder with 90g of frankincense, adding calcium hydrogen phosphate accounting for 35% of the total weight of the first mixed fine powder and the frankincense, crushing to obtain second mixed fine powder, drying at 60 ℃, sieving by a 16-mesh sieve, adding micro-powder silica gel accounting for 0.6% of the weight of the second mixed fine powder and 0.6% of magnesium stearate, uniformly mixing, and encapsulating to obtain the Tibetan medicine compound mastra lactea capsule.
In example 2, one part of the Tibetan medicine compound Ruteng capsule is prepared into 650 granules per 1 g.
The identification, inspection and content determination processes of the Tibetan medicine compound Ruteng capsule prepared in the embodiment 2 are the same as those of the embodiment 1.
Example 3:
weighing 110g of myrobalan, 95g of semen cassiae, 70g of radix mallow, 40g of tinospora sinensis, 35g of lamiophlomis rotata and 35g of fleshy ardisia herb, mixing, performing reflux extraction for 3 times by using 12 times of 60% ethanol, performing 1.5 hours each time, combining filtrates, performing reduced pressure concentration to obtain a concentrated solution, drying at 80 ℃, and crushing to obtain first mixed fine powder; and (3) uniformly mixing the first mixed fine powder with 100g of frankincense, adding calcium hydrogen phosphate accounting for 30% of the total weight of the first mixed fine powder and the frankincense, crushing to obtain second mixed fine powder, drying at 60 ℃, sieving by a 16-mesh sieve, adding micro-powder silica gel accounting for 0.5% of the weight of the second mixed fine powder and 0.5% of magnesium stearate, uniformly mixing, and encapsulating to obtain the Tibetan medicine compound mastra lactea capsule.
In example 3, 650 grains of the Tibetan medicine compound milk vine capsule are prepared in each 1 g.
The identification, inspection and content determination processes of the Tibetan medicine compound Ruteng capsule prepared in the embodiment 3 are the same as those of the embodiment 1.
And (3) composition analysis: the frankincense is astringent and bitter in taste, warm in nature, light in effect, dry and acute, and mainly treats the yellow water disease, the dragon disease and the like; the myrobalan balances three factors, namely dragon, red bara and bacon, and plays a role in harmonizing and balancing; caulis tinosporae sinensis is sweet, bitter, astringent and pungent in flavor, moist, cool and warm in nature, sweet in flavor and sour in nature, and is commonly used for treating dragon and red barbiers complications, bacon disease, febrile dragon disease, rheumatism and the like; the fleshy chrysanthemum is cool in nature and bitter in taste, and is used for treating headache and dry yellow water; the lamiophlomis rotata is warm in nature, sweet and astringent in taste, and mainly treats inflammation caused by various reasons, bone and joint pain, trauma and fracture caused by traumatic injury; semen Cassiae has bitter and astringent taste, is cool and effective in dryness after digestion, can guide yellow water, and can be used for treating yellow water disease, hysteria, epilepsia, intractable skin tinea, etc.; the malva verticillata seeds are bitter in taste, bitter in taste after being digested, cool in nature, coarse in effect, capable of astringing yellow water, and used for treating yellow water diseases, skin diseases, insect diseases and the like.
And (3) analyzing characters: examples 1-3 the product obtained was a hard capsule, the contents being a tan powder; slightly fragrant smell, bitter and astringent taste.
The product of the Tibetan medicine compound milk vine capsule prepared in example 1-example 3 is illustrated as follows:
the functions and indications are as follows: dispelling pathogenic wind and removing dampness, and "dry yellow water", can be used for treating eczema, rheumatoid arthritis, gout, and other arthralgia syndrome, "yellow water disease", and dermatosis.
The application and dosage are as follows: oral administration, following the medical advice;
specification: each grain is filled with 0.35g, 15 grains are multiplied by 2 plates/boxes;
and (3) storage: sealing, and standing in a cool and dry place.
The invention utilizes modern preparation theory and technology to carry out modern research and development on the Tibetan medicine with unique curative effect, and develops the Tibetan medicine compound Ruteng capsule into a safe, effective, quality-controllable and portable modern preparation form through the preparation method and the quality standard research of the Tibetan medicine compound Ruteng capsule, thereby having good economic benefit and social significance and also providing reference for exploring the modern research and development application of the Tibetan medicine compound.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The Tibetan medicine compound Ruteng capsule is characterized by comprising main materials and auxiliary materials, wherein the main materials comprise the following raw materials in parts by mass: 80-120 parts of frankincense, 80-120 parts of myrobalan, 60-100 parts of semen cassiae, 60-100 parts of abelmoschus manihot, 30-70 parts of tinospora sinensis, 30-70 parts of lamiophlomis rotate and 20-60 parts of fleshy aster; the auxiliary materials comprise the following raw materials: calcium hydrogen phosphate, aerosil and magnesium stearate.
2. The preparation method of the Tibetan medicine compound Ruteng capsule as claimed in claim 1, which is characterized by comprising the following steps: mixing fructus Chebulae, semen Cassiae, semen Abutili, caulis tinosporae, radix Lamiophlomidis Rotatae, and herba Kyllingae, adding ethanol solution, reflux-extracting for several times, mixing filtrates, concentrating under reduced pressure to obtain concentrated solution, drying, and pulverizing to obtain first mixed fine powder; mixing the obtained first mixed fine powder with Olibanum, adding calcium hydrogen phosphate, pulverizing to obtain second mixed fine powder, drying, sieving, adding silica gel micropowder and magnesium stearate, mixing, and making into capsule.
3. The preparation method of a Tibetan medicine compound Ruteng capsule as claimed in claim 2, wherein the usage amount of calcium hydrogen phosphate is 20% -40% of the total mass of the first mixed fine powder and Olibanum, the usage amount of aerosil is 0.3% -0.8% of the mass of the second mixed fine powder, and the usage amount of magnesium stearate is 0.3% -0.8% of the mass of the second mixed fine powder.
4. The quality standard detection method of the Tibetan medicine compound milk rattan capsule prepared by the preparation method of claim 2 is characterized in that the qualitative identification of frankincense and cassia seed is carried out by using thin-layer chromatography, and the quantitative determination of 8-O-acetyl shanzhiside methyl ester is carried out by using high performance liquid chromatography;
the qualitative identification of frankincense comprises the following steps: taking 0.3g of the content of the product, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a test solution; taking 0.2g of frankincense control medicinal material, adding 5mL of methanol, carrying out ultrasonic treatment for 10 minutes, and filtering to obtain filtrate as a control medicinal material solution; sucking 10 μ L of test solution and 5 μ L of control solution, respectively dropping on the same silica gel G thin layer plate, developing with petroleum ether-ethyl acetate as developing agent, taking out, air drying, spraying 5% vanillin-sulfuric acid solution, and heating at 105 deg.C until the spots are clearly developed; in the chromatogram of the test solution, main spots with the same color appear at the corresponding positions of the chromatogram of the reference solution;
the qualitative identification of the cassia seeds comprises the following steps: taking 3g of the content of the product, adding 30mL of methanol, carrying out ultrasonic treatment for 30 minutes, filtering, evaporating the filtrate to dryness, adding 20mL of water into the residue for dissolving, adding 2mL of hydrochloric acid, heating in a water bath for 30 minutes, immediately cooling, shaking and extracting with diethyl ether for 2 times, wherein 20mL of the extraction solution is added each time, combining the diethyl ether extraction solutions, volatilizing, and adding 1mL of methanol into the residue for dissolving to obtain a sample solution; adding 10mL of methanol into 1g of semen Cassiae reference material, soaking for 1 hour, filtering, evaporating filtrate to dryness, dissolving the residue in 10mL of water, adding 1mL of hydrochloric acid, heating in water bath for 30 minutes, cooling immediately, shaking with diethyl ether for 2 times, each time extracting for 20mL, mixing diethyl ether extractive solutions, volatilizing, and dissolving the residue in 1mL of methanol to obtain a reference material solution; taking an aurantio-obtusin reference substance, and adding methanol to prepare a solution containing 0.5mg of aurantio-obtusin per 1mL, wherein the solution is used as a reference substance solution; sucking the three solutions with each volume of 8 μ L, respectively dropping on the same silica gel H thin layer plate, spreading with petroleum ether-acetone as developing agent, taking out, air drying, fumigating in ammonia gas until the spots are clearly developed, and observing under sunlight to show spots with the same color in the chromatogram of the sample at the positions corresponding to the chromatogram of the reference medicinal solution and the chromatogram of the reference solution;
the quantitative determination of the 8-O-acetyl shanzhiside methyl ester comprises the following steps:
(1) preparation of control solutions: precisely weighing 8-O-acetyl shanzhiside methyl ester reference substance, and adding methanol to obtain solution containing 8-O-acetyl shanzhiside methyl ester 30 μ g per 1 mL;
(2) preparing a test solution: precisely weighing 1.0g of the content of the product, placing the product in a conical flask with a plug, precisely adding 25mL of 70% methanol, sealing the plug, weighing, ultrasonically treating for 40 minutes, cooling, weighing again, supplementing the loss weight with 70% methanol, shaking up, filtering, and taking the subsequent filtrate to obtain the product;
(3) precisely sucking 10 μ L of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
5. The quality standard detection method of the Tibetan medicine compound milk vine capsule as claimed in claim 4, wherein in step (3), the chromatographic conditions of a liquid chromatograph are as follows: octadecyl bonded phase silica gel is used as a filling agent; taking acetonitrile as a mobile phase A and water as a mobile phase B, and performing gradient elution: 0-10 min, 12% of mobile phase A; 10-20 min, 12% mobile phase A → 10% mobile phase A; 20-70 min, 10% of mobile phase A; the flow rate is 1.0 mL/min; the column temperature is 30 ℃; the detection wavelength is 235 nm; the theoretical plate number is not less than 4000 calculated according to 8-O-acetyl shanzhiside methyl ester.
6. The quality standard detection method of the Tibetan medicine compound milk vine capsule as claimed in claim 4, wherein the content of 8-O-acetyl shanzhiside methyl ester in each gram of the content is not less than 0.5 mg.
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Application publication date: 20201023 |