CN108969567B - Preparation method of traditional Chinese medicine composition containing rock fat - Google Patents
Preparation method of traditional Chinese medicine composition containing rock fat Download PDFInfo
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Abstract
The invention relates to the technical field of traditional Chinese medicine extraction, and particularly relates to a preparation method of a traditional Chinese medicine composition containing dangshi. The preparation method of the traditional Chinese medicine composition comprises the following steps: crushing the mirabilite powder and 140-180 parts of poria cocos to obtain raw medicinal powder; extracting herba Cephalanoploris and folium Pyrrosiae with ethanol to obtain extractive solution and residue; extracting the residues, the rest of Poria cocos, piemarker seed, pumice, clam shell, achyranthes and licorice with water to obtain water extract; mixing the extractive solution and water extractive solution, concentrating, and mixing the obtained extract and original medicinal powder to obtain the Chinese medicinal composition. The invention breaks through the conventional preparation method, firstly extracts the active ingredients of the common cephalanoplos herb and the pyrrosia lingua, and then combines the extract with other medicinal materials for extraction, and the method can greatly improve the transfer rate of the linarin from the existing 5 percent to more than 50 percent, thereby improving the curative effect of the product.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine extraction, and particularly relates to a preparation method of a traditional Chinese medicine composition containing dangshi.
Background
The ZHUANSHI Capsule is prepared from Abutilon, kurtosis, Pumex, Concha Meretricis Seu Cyclinae, Poria, herba Cephalanoploris, Natrii sulfas, Achyranthis radix, and Glycyrrhrizae radix. Has effects of clearing heat, promoting urination, and treating urinary system calculus such as renal calculus, ureter and bladder etc. The product is a hard capsule, and the content is brown granules; slightly fragrant smell, slightly salty taste. The product is a national standard product, is loaded in the 2015 edition pharmacopeia, and has a variety approval document number of national drug standard Z20090335.
The existing extraction method of the dangshi capsule comprises the following steps: 125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice. Pulverizing the above nine ingredients, the glauber salt and 160g of poria cocos into fine powder, sieving, decocting the rest poria cocos and the rest seven ingredients such as chingma abutilon seed and the like twice with water, decocting for 1.5 hours with 10 times of water for the first time, decocting for 1 hour with 8 times of water for the second time, mixing decoctions, filtering, concentrating the filtrate to obtain a relative density of 1.30-1.32 (measured at 60 ℃), mixing with the glauber salt and the like uniformly, granulating, drying, and encapsulating to obtain 1000 capsules.
One of the effective components in the ZHUANSHI Capsule is linarin, has a structural formula shown in formula I, and has antiaging, anoxia resisting, adverse irritation resisting, organism bidirectional regulating, fatigue resisting, and blood sugar increase inhibiting effects.
However, the existing method for extracting the dangshi capsule has low extraction transfer rate of the linarin. Therefore, it is necessary to develop a method for effectively improving the extraction and transfer rate of linarin.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a traditional Chinese medicine composition containing the rocks. The preparation method can greatly improve the extraction transfer rate of linarin and chlorogenic acid.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a traditional Chinese medicine composition, which is prepared from the following raw materials in parts by weight: 100-150 parts of chingma abutilon seed, 80-120 parts of pyrrosia lingua, 100-150 parts of pumice, 100-150 parts of clam shell, 200-280 parts of poria cocos, 100-150 parts of field thistle, 60-100 parts of glauber salt, 100-150 parts of achyranthes bidentata and 40-60 parts of liquorice; the preparation method comprises the following steps:
crushing the mirabilite powder and 140-180 parts of poria cocos to obtain raw medicinal powder;
cold-soaking herba Cephalanoploris and folium Pyrrosiae with 70% ethanol to obtain extractive solution and residue;
extracting the residues, the rest of Poria cocos, piemarker seed, pumice, clam shell, achyranthes and licorice with water to obtain water extract;
mixing the extractive solution and water extractive solution, concentrating, and mixing the obtained extract and original medicinal powder to obtain the Chinese medicinal composition.
Preferably, the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 125 parts of chingma abutilon seed, 100 parts of pyrrosia lingua, 125 parts of pumice, 125 parts of clam shell, 240 parts of poria cocos, 125 parts of field thistle, 83 parts of glauber salt, 125 parts of achyranthes bidentata and 50 parts of liquorice.
Preferably, the cold-leaching extraction of the common cephalanoplos herb and the pyrrosia lingua by using 70% ethanol is as follows: extracting with 8-20 times of ethanol by weight of common cephalanoplos herb and pyrrosia lingua for 2-4 times, wherein the extraction time is 1-3 h each time, and combining filtrates.
Preferably, the extraction of herba Cirsii and folium Pyrrosiae with ethanol is: extracting with ethanol 10 times the weight of herba Cephalanoploris and folium Pyrrosiae for 2 times, extracting for 2 hr for the first time, extracting for 1 hr for the second time, and mixing filtrates.
Preferably, the aqueous extraction is: extracting 8-20 times of water by weight of raw materials except the mirabilite and 140-180 parts of poria cocos for 2-4 times, wherein the extraction time is 1-3 h each time, and combining filtrates.
Preferably, the aqueous extraction is: extracting with water for 2 times, the first time with 10 times of water for 1.5 hr, the second time with 8 times of water for 1 hr, and mixing filtrates.
Preferably, the relative density after concentration is 1.30-1.32; the relative density was measured at 60 ℃.
Preferably, the concentration is a concentration under reduced pressure.
Preferably, the step of pulverizing the mirabilite and 140 to 180 parts of the poria cocos is to pulverize the mirabilite and the poria cocos into superfine powder.
Preferably, the Chinese medicinal composition is in the form of capsules, tablets, granules or pills.
The invention also provides a method for extracting the herba cepbalanoplosis segeti and the pyrrosia lingua, which comprises the following steps: extracting herba Cephalanoploris and folium Pyrrosiae with ethanol to obtain extractive solution and residue;
extracting the dregs with water to obtain water extract;
mixing the extractive solution and water extractive solution to obtain extract.
Preferably, the extraction of herba Cirsii and folium Pyrrosiae with ethanol is: extracting with 8-20 times of ethanol by weight of common cephalanoplos herb and pyrrosia lingua for 2-4 times, wherein the extraction time is 1-3 h each time, and combining filtrates.
Preferably, the extraction of herba Cirsii and folium Pyrrosiae with ethanol is: extracting with ethanol 10 times the weight of herba Cephalanoploris and folium Pyrrosiae for 2 times, extracting for 2 hr for the first time, extracting for 1 hr for the second time, and mixing filtrates.
Preferably, the aqueous extraction is: extracting with water which is 8-20 times the weight of the common cephalanoplos herb and the pyrrosia lingua for 2-4 times, wherein the extraction time is 1-3 h each time, and combining the filtrates.
Preferably, the aqueous extraction is: extracting with water for 2 times, the first time with 10 times of water for 1.5 hr, the second time with 8 times of water for 1 hr, and mixing filtrates.
Preferably, the step of combining the extract and the aqueous extract further comprises concentrating.
The invention provides a preparation method of a traditional Chinese medicine composition containing Chinese medicine of land rockvine. The traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 100-150 parts of chingma abutilon seed, 80-120 parts of pyrrosia lingua, 100-150 parts of pumice, 100-150 parts of clam shell, 200-280 parts of poria cocos, 100-150 parts of field thistle, 60-100 parts of glauber salt, 100-150 parts of achyranthes bidentata and 40-60 parts of liquorice; the preparation method comprises the following steps: crushing the mirabilite powder and 140-180 parts of poria cocos to obtain raw medicinal powder; extracting herba Cephalanoploris and folium Pyrrosiae with ethanol to obtain extractive solution and residue; extracting the residues, the rest of Poria cocos, piemarker seed, pumice, clam shell, achyranthes and licorice with water to obtain water extract; mixing the extractive solution and water extractive solution, concentrating, and mixing the obtained extract and original medicinal powder to obtain the Chinese medicinal composition. The invention has the technical effects that:
the invention breaks through the conventional preparation method, firstly extracts the active ingredients of the common cephalanoplos herb, and then combines the common cephalanoplos herb with other medicinal materials for extraction, and the method can greatly improve the transfer rate of the linarin from the existing 5 percent to more than 50 percent, thereby improving the curative effect of the product.
Detailed Description
The invention discloses a preparation method of a traditional Chinese medicine composition containing traditional Chinese medicine of land stone, and the technical personnel in the field can appropriately improve the technological parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The raw materials or auxiliary materials used in the preparation method of the traditional Chinese medicine composition provided by the invention can be purchased from the market.
The invention is further illustrated by the following examples:
example 1
The formula of the rock swinging capsule in the embodiment is as follows:
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
The process for preparing the rock swinging capsule of the embodiment is as follows:
1. pulverizing Natrii sulfas and Poria 160g into fine powder, and sieving;
2. cold-soaking herba Cephalanoploris and folium Pyrrosiae in 10 times of 70% ethanol for two times (2 hr for the first time and 1 hr for the second time), and filtering to obtain filtrate;
3. decocting the residue and the rest of pulverized Poria and semen Abutili in water twice, decocting with 10 times of water for 1.5 hr for the first time, decocting with 8 times of water for 1 hr for the second time, filtering, and mixing the filtrate with the above filtrate;
4. concentrating under reduced pressure to relative density of 1.30-1.32 (measured at 60 deg.C), and mixing with the above Natrii sulfas;
5. granulating, drying, and making into capsule 1000.
Example 2
The formula of the rock swinging capsule in the embodiment is as follows:
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
The process for preparing the rock swinging capsule of the embodiment is as follows:
1. pulverizing Natrii sulfas and Poria 160g into fine powder, and sieving;
2. cold soaking herba Cephalanoploris and folium Pyrrosiae in 8 times of 70% ethanol for four times (2 hr for the first time, 1 hr for the second time, 1 hr for the third time, and 1 hr for the fourth time), and filtering to obtain filtrate;
3. decocting the residue and the rest of pulverized Poria and semen Abutili with water for four times, decocting with 8 times of water for 1.5 hr for the first time, 8 times of water for 1 hr for the second time, 8 times of water for 1 hr for the third time, 8 times of water for 1 hr for the fourth time, filtering, and mixing the filtrate with the above filtrate;
4. concentrating under reduced pressure to relative density of 1.30-1.32 (measured at 60 deg.C), and mixing with the above Natrii sulfas;
5. granulating, drying, and making into capsule 1000.
Example 3
The formula of the rock swinging capsule in the embodiment is as follows:
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
The process for preparing the rock swinging capsule of the embodiment is as follows:
1. pulverizing Natrii sulfas and Poria 160g into fine powder, and sieving;
2. cold soaking herba Cephalanoploris and folium Pyrrosiae in 20 times of 70% ethanol for two times (3 hr for the first time and 1 hr for the second time), and filtering to obtain filtrate;
3. decocting the residue and the rest of pulverized Poria and semen Abutili in water twice, decocting with 20 times of water for 1.5 hr for the first time, decocting with 10 times of water for 1 hr for the second time, filtering, and mixing the filtrate with the above filtrate;
4. concentrating under reduced pressure to relative density of 1.30-1.32 (measured at 60 deg.C), and mixing with the above Natrii sulfas;
5. granulating, drying, and making into capsule 1000.
Comparative example 1
The existing extraction method of the dangshi capsule comprises the following steps:
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
Pulverizing the above nine ingredients, the glauber salt and 160g of poria cocos into fine powder, sieving, decocting the rest poria cocos and the rest seven ingredients such as chingma abutilon seed and the like twice with water, decocting for 1.5 hours with 10 times of water for the first time, decocting for 1 hour with 8 times of water for the second time, mixing decoctions, filtering, concentrating the filtrate to obtain a relative density of 1.30-1.32 (measured at 60 ℃), mixing with the glauber salt and the like uniformly, granulating, drying, and encapsulating to obtain 1000 capsules.
Comparative example 2
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
The nine ingredients, the mirabilite and 160g of tuckahoe are crushed into fine powder and sieved for standby. Extracting herba cepbalanoplosis segeti and pyrrosia lingua twice with 8 times of ethanol for 2 hours each time, decocting residues and the rest five materials such as poria cocos and abutilon seed twice with water, decocting the residues and the rest five materials with 10 times of water for 1.5 hours for the first time, decocting the residues and the rest five materials with 8 times of water for 1 hour for the second time, merging decoction, filtering, concentrating the filtrate to obtain the relative density of 1.30-1.32 (measured at 60 ℃), mixing the filtrate with the glauber salt and the like uniformly, granulating, drying, and encapsulating to obtain 1000 granules.
Comparative example 3
125g of chingma abutilon seed, 100g of pyrrosia lingua, 125g of pumice, 125g of clamshell, 240g of poria cocos, 125g of field thistle, 83g of glauber salt, 125g of achyranthes bidentata and 50g of liquorice.
The nine ingredients, the mirabilite and 160g of tuckahoe are crushed into fine powder and sieved for standby. Extracting herba cepbalanoplosis segeti and pyrrosia lingua twice with ethyl acetate in an amount which is 8 times that of the herba cepbalanoplosis segeti for 2 hours each time, decocting residues and the rest five medicines such as poria cocos, chingma abutilon seed and the like twice with water, decocting the residues and the rest five medicines with water in an amount which is 10 times that of the residues and the rest five medicines with water in an amount which is 8 times that of the residues and the rest five medicines with water in the first time for 1.5 hours and the rest five medicines with water in an amount which is 8 times that of the residues and the rest five.
Test example 1 determination of linarin content
The capsules of examples 1-3 and comparative example were tested for the linarin extraction transfer rate by the following specific test method:
the detection method of linarin comprises the following steps:
chromatographic conditions and system applicability tests, and octadecylsilane chemically bonded silica is used as a filler; methanol-water (47:53) is used as a mobile phase; the detection wavelength was 326 nm. The number of theoretical plates is not less than 2000 calculated according to the linarin peak.
Taking a sample, grinding, precisely weighing about 1.5g, placing in a conical flask with a plug, precisely adding 25ml of methanol, sealing the plug, carrying out ultrasonic treatment (power 250W and frequency 40kHz) for 45 minutes, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking a subsequent filtrate as a test solution. Taking a proper amount of linarin control, precisely weighing, and adding methanol to obtain a solution containing 20 μ g of linarin per 1ml as control solution. Precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and calculating linarin content by external standard method.
The extraction transfer rate was calculated as follows:
the extraction transfer rate is equal to the content of the finished product of the linarin multiplied by 2.4/the content of the linarin in the field thistle medicinal material multiplied by 100%
The detection method of chlorogenic acid comprises the following steps:
chromatographic conditions and system applicability tests, and octadecylsilane chemically bonded silica is used as a filler; acetonitrile-0.4% phosphoric acid solution (10:90) is used as a mobile phase; the detection wavelength was 327 nm. The number of theoretical plates is not less than 1000 calculated according to chlorogenic acid peak.
Taking a sample, grinding, taking about 1g, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of 50% methanol, sealing the plug, carrying out ultrasonic treatment (power 250W, frequency 33kHz) for 30 minutes, weighing again, supplementing the lost weight with 50% methanol, shaking up, filtering, and taking a subsequent filtrate as a test solution. Taking a proper amount of chlorogenic acid reference substance, precisely weighing, placing into a brown measuring flask, adding 50% methanol to obtain a solution containing 10 μ g of chlorogenic acid per 1ml, and using as a test solution. Precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and calculating chlorogenic acid content by external standard method.
The extraction transfer rate was calculated as follows:
the extraction transfer rate is equal to the content of chlorogenic acid in the finished product multiplied by 3/the content of chlorogenic acid in the pyrrosia lingua medicinal material multiplied by 100%
The content detection results are as follows:
TABLE 1 extraction transfer rate of linarin in each group of capsules
The invention breaks through the conventional preparation method, firstly extracts the active ingredients of the common cephalanoplos herb, and then combines the common cephalanoplos herb with other medicinal materials for extraction, and the method can greatly improve the transfer rate of the linarin from the existing 5 percent to more than 50 percent, thereby improving the curative effect of the product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The preparation method of the traditional Chinese medicine composition is characterized in that the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 100-150 parts of chingma abutilon seed, 80-120 parts of pyrrosia lingua, 100-150 parts of pumice, 100-150 parts of clam shell, 200-280 parts of poria cocos, 100-150 parts of field thistle, 60-100 parts of glauber salt, 100-150 parts of achyranthes bidentata and 40-60 parts of liquorice; the preparation method comprises the following steps:
crushing the mirabilite powder and 140-180 parts of poria cocos to obtain raw medicinal powder;
cold-soaking herba cepbalanoplosis segeti and pyrrosia lingua in 70% ethanol 8-20 times of the weight of the herba cepbalanoplosis segeti, extracting for 2-4 times, wherein the extraction time is 1-3 h each time, and combining filtrates to obtain an extracting solution and dregs;
extracting the residues, the rest of poria cocos, abutilon seed, pumice, clam shell, achyranthes and liquorice with water to obtain water extract; the water extraction comprises the following steps: extracting 8-20 times of water by weight of raw materials except the mirabilite and 140-180 parts of poria cocos for 2-4 times, wherein the extraction time is 1-3 h each time, and combining filtrates;
and combining the extracting solution and the water extract, concentrating, and mixing the obtained extract with the original medicine powder to obtain the traditional Chinese medicine composition.
2. The preparation method according to claim 1, characterized in that the traditional Chinese medicine composition is prepared from the following raw materials in parts by weight: 125 parts of chingma abutilon seed, 100 parts of pyrrosia lingua, 125 parts of pumice, 125 parts of clam shell, 240 parts of poria cocos, 125 parts of field thistle, 83 parts of glauber salt, 125 parts of achyranthes bidentata and 50 parts of liquorice.
3. The process according to claim 1, wherein the extraction of the Cirsium setosum and Pyrrosia with ethanol is: extracting with ethanol 10 times the weight of herba Cephalanoploris and folium Pyrrosiae for 2 times, extracting for 2 hr for the first time, extracting for 1 hr for the second time, and mixing filtrates.
4. The method of preparation according to claim 3, characterized in that said aqueous extraction is: extracting with water for 2 times, the first time with 10 times of water for 1.5 hr, the second time with 8 times of water for 1 hr, and mixing filtrates.
5. The production method according to claim 1, wherein the relative density after the concentration is 1.30 to 1.32; the relative density is detected at 60 ℃; the concentration is a reduced pressure concentration.
6. The method according to claim 1, wherein the step of pulverizing Matrii sulfas exsiccatus and 140-180 parts of Poria cocos is carried out by micronization.
7. The preparation method according to claim 1, wherein the dosage form of the Chinese medicinal composition is capsules, tablets, granules or pills.
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| HPLC法测定金银花中绿原酸的含量;石连成等;《黑龙江医药》;20021231;第15卷(第2期);第92-94页 * |
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