CN114652799B - Sanjin traditional Chinese medicine composition and preparation method thereof - Google Patents
Sanjin traditional Chinese medicine composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Sanjin traditional Chinese medicine composition and a preparation method thereof, wherein the Sanjin traditional Chinese medicine composition comprises the following components in parts by weight: 14.5-20.6 parts of cherokee rose root dry extract, 9.6-16 parts of chinaroot greenbrier rhizome dry extract, 11-16.8 parts of sheep opening dry extract, 3.48-7.57 parts of jinsha vine dry extract and 6.5-13.8 parts of centella asiatica dry extract. The preparation method comprises the following steps: the preparation method comprises the steps of respectively and independently preparing dry extracts of cherokee rose root, chinaroot greenbrier rhizome, sheep's mouth, jinshu vine and asiatic centella herb materials according to the prescription amount, crushing, and mixing the dry extract powders of the components according to the mass ratio. The three-gold traditional Chinese medicine composition comprises dry extracts prepared by respectively extracting five medicinal materials of cherokee rose root, chinaroot greenbrier rhizome, sheep mouth, jinsha vine and centella asiatica, and the optimal dry extract preparation process is optimized according to the characteristics of the medicinal materials, so that the loss of active ingredients is less, the content of the active ingredients in the composition is high, and the uniformity of the mass of the composition is better.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicines, and particularly relates to a Sanjin traditional Chinese medicine composition and a preparation method thereof.
Background
The Sanjin preparation is a traditional Chinese medicine preparation prepared by extracting and processing five traditional Chinese medicinal materials of cherokee rose root, chinaroot greenbrier rhizome, sheep opening, jinshu vine and centella asiatica, and has the effects of clearing away heat and toxic materials, promoting diuresis, treating stranguria and tonifying kidney; is mainly used for treating heat stranguria, oliguria with reddish urine, dribbling and pain and urgent micturition frequency caused by damp-heat in lower jiao; acute and chronic pyelonephritis, cystitis and urinary tract infection with the symptoms; chronic abacterial prostatitis with kidney deficiency and damp-heat downward flow.
The Sanjin preparation is currently prepared into various dosage forms, for example, the prescription and quality control method of Sanjin tablets are already listed in the Chinese pharmacopoeia of 2000 edition, and the content measurement items are added in the amendment of 2003. The preparation method of the Sanjin tablet in the pharmacopoeia is described as follows: decocting the above five materials with water twice for 2 hr for 1 hr, filtering, mixing filtrates, concentrating to appropriate amount, spray drying, adding appropriate amount of adjuvant, mixing, granulating, drying, and pressing into 1000 (small) or 600 (large) pieces, and sugar coating or film coating.
It can be known that the existing extraction mode of Sanjin preparation generally comprises mixing five medicinal materials, decocting with water, and extracting. The inventor finds that the following problems easily exist due to different effective active ingredients contained in cherokee rose root, chinaroot greenbrier rhizome, sheep's mouth, jinsha vine and centella asiatica in the way of decoction, firstly the condition can not fully extract the effective ingredients of each medicinal material, and secondly the five medicinal materials can be mutually influenced in the common decoction process.
Therefore, how to provide a Sanjin traditional Chinese medicine composition and a preparation method which can fully extract and utilize the effective components in five medicinal materials is a problem to be solved.
The present invention has been made in view of this.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing a Sanjin traditional Chinese medicine composition and a preparation method thereof. The three-gold traditional Chinese medicine composition comprises dry extracts prepared by respectively extracting five medicinal materials of cherokee rose root, chinaroot greenbrier rhizome, sheep mouth, jinsha vine and centella asiatica, and the optimal dry extract preparation process is optimized according to the characteristics of the medicinal materials, so that the loss of active ingredients is less, the content of the active ingredients in the composition is high, and the uniformity of the mass of the composition is better.
In order to solve the technical problems, the invention adopts the basic conception of the technical scheme that:
the invention provides a Sanjin traditional Chinese medicine composition, which comprises the following components in parts by weight:
14.5-20.6 parts of cherokee rose root dry extract, 9.6-16 parts of chinaroot greenbrier rhizome dry extract, 11-16.8 parts of sheep opening dry extract, 3.48-7.57 parts of jinsha vine dry extract and 6.5-13.8 parts of centella asiatica dry extract.
In the three-gold traditional Chinese medicine composition, five medicinal materials of cherokee rose root, chinaroot greenbrier rhizome, sheep mouth, jinshug vine and centella asiatica are respectively and independently extracted to prepare dry paste. Compared with the method of extracting the medicinal materials together to prepare the ointment after mixing, the method adopts the optimized method to prepare the active ingredient extract in the mode of dry ointment respectively, has little loss and high content of the active ingredient in the composition, thereby improving the quality of the traditional Chinese medicine composition.
The further scheme comprises the following components in parts by weight:
14.5-18 parts of cherokee rose root dry paste, 9.6-12 parts of chinaroot greenbrier dry paste, 12-15 parts of sheep opening dry paste, 4.1-6.8 parts of gold Sha Tenggan paste and 7-12 parts of centella dry paste.
In a further scheme, the preparation method of the cherokee rose root dry paste comprises the following steps: soaking radix Rosae Laevigatae in 2 times of hot water at 60-100deg.C for 10-30min, decocting with 4 times of water for 1.5 hr, filtering, extracting residues with water twice, mixing filtrates, concentrating, and drying to obtain radix Rosae Laevigatae dry extract;
preferably, the mixture is soaked in hot water at 85 ℃ for 20min;
preferably, the water is added for extraction in the last two times, the water adding amount is 5 times and 4 times respectively, and the decoction time is 1 hour.
In the invention, cherokee rose root medicinal material is soaked in 2 times of hot water for 20 minutes and then is decocted with water for three times, the extraction rate of total glycosides in the first decoction can reach 18.92%, the extraction rate of total glycosides in the second extraction can reach 18.34%, the extraction rate of total glycosides in the third extraction is 9.49%, the total extraction rate in the extraction stage can reach more than 46.75%, and the dry paste rate is 10.32%, which means that the saponins can be extracted by three times of water extraction.
Further, the preparation method of the smilax glabra dry paste comprises the following steps: soaking rhizoma Smilacis chinensis in 2 times of hot water at 60-100deg.C for 10-30min, decocting in 4 times of water, controlling temperature at 70deg.C, extracting for 2 hr, filtering, extracting residues with water twice, and mixing filtrates; concentrating, and drying to obtain rhizoma Smilacis chinensis dry extract;
preferably, the mixture is soaked in hot water at 85 ℃ for 20min;
preferably, in the latter two times of water extraction, the water addition amount is 5 times and 4 times respectively, and the micro-boiling decoction time is 1.5 hours and 1 hour respectively.
In the invention, the chinaroot greenbrier medicinal material is subjected to enzyme deactivation and glycoside preservation and then is extracted by water for three times, the extraction rate of chlorogenic acid extracted by water for the first time can reach 64.43 percent, the extraction rate of the longan glycoside is 17.86 percent, the extraction rate of chlorogenic acid extracted by water for the second time is 31.57 percent, and the extraction rate of the longan glycoside is 9.0 percent; the extraction rate of chlorogenic acid extracted for the third time is 7.5%, the extraction rate of the longan aril is 2.85%, the total extraction rate of chlorogenic acid in the extraction stage can reach more than 98%, and the dry paste rate is 16.02%, which indicates that the components to be detected can be completely extracted by the second water extraction.
Further, the preparation method of the sheep opening dry paste comprises the following steps: extracting sheep opening with 6 times of alkaline water with pH of 8-10 for 1.5 hr, filtering, extracting residues with water twice, filtering, and mixing filtrates; concentrating, and drying to obtain sheep opening dry extract;
preferably, when water is added for extraction in the latter two times, the water adding amount is 5 times and 4 times, and the decoction time is 1.5 hours and 1 hour respectively;
preferably, the alkaline water comprises sodium bicarbonate solution, sodium carbonate solution, sodium hydroxide solution and lime water.
Preferably, the pH of the alkaline water is 8.5.
In the specific embodiment of the invention, the sodium hydroxide solution with the pH of 8.5 is adopted, and can be replaced by other alkaline water, so that the extraction effect is similar.
In the invention, the sheep opening medicinal material is extracted three times by adding water, the extraction rate of extracting gallic acid by adding a small amount of alkali for the first time is 41.2%, the extraction rate of extracting gallic acid by adding water for the second time is 25.49%, the extraction rate of extracting gallic acid for the third time is 11.51%, and the total extraction amount of the three times reaches 88%, which indicates that the extraction can be basically completed.
Further, the preparation method of the sargentgloryvine stem paste comprises the following steps: extracting radix seu herba Kadsurae Longipedunculatae with water twice (8 times and 6 times of water), decocting for 1 hr, filtering, and mixing filtrates; concentrating, and drying to obtain the dry extract of the sargentgloryvine stem.
In the invention, the total extraction rate of main saponins in the extraction stage of the sargentgloryvine stem medicinal material can reach more than 70% through two water extractions, which shows that after steam, the saponins can be basically extracted through the two water extractions.
Further, the preparation method of the centella asiatica dry extract comprises the following steps: steaming herba Centellae with water for 15-40min, decocting with water for 3 times, mixing filtrates, concentrating, and drying to obtain herba Centellae dry extract;
preferably, 8 times of water is added for the first time, the decoction is decocted for 1.5 hours, filtering is carried out, the decoction dregs are extracted twice by adding water, the water adding amount is 6 times and 3 times of water respectively, and the decoction time is 1 hour.
Preferably, the asiatic herb material is steamed with water vapor for 25min, and then decocted with water for 3 times.
In the invention, centella asiatica medicinal materials are steamed for 25min by steam and then are decocted by adding water, the extraction rate of total glycosides in the first decoction can reach 52.76%, the extraction rate of total glycosides in the second extraction can reach 16.5%, the extraction rate of total glycosides in the third extraction can reach 5.97%, the total extraction rate of main saponins in the extraction stage can reach 77%, and the dry extract rate is 20.23%, which indicates that the saponin components can be basically extracted by three water extractions.
In a further scheme, the preparation process of the dry paste of each component further comprises a purification process: mixing the filtrates, concentrating to relative density of 1.12-1.15, and directly drying to obtain dry extract; or precipitating with 80% ethanol, recovering ethanol from ethanol solution, and concentrating to relative density of 1.1-1.2; drying to obtain dry extract.
In the invention, an alcohol precipitation process can be further adopted, so that the paste amount can be properly reduced, and active substances can be reserved.
In a further scheme, the Sanjin traditional Chinese medicine composition is prepared into a conventional dosage form;
preferably, the dosage forms comprise granules, pills, powder, capsules and tablets.
The second purpose of the invention is to provide a preparation method of the three-gold traditional Chinese medicine composition according to any one or combination scheme, wherein the Chinese medicinal composition is prepared by respectively and independently preparing dry extracts of cherokee rose root, chinaroot greenbrier rhizome, sheep mouth, jinsha vine and asiatic centella herb materials according to prescription, crushing the dry extracts, and mixing dry extract powders of the components according to mass ratio. Wherein, cherokee rose root dry paste, chinaroot greenbrier dry paste, sheep opening dry paste, gold Sha Tenggan paste and centella dry paste are separately prepared by adopting the method described above.
After the technical scheme is adopted, compared with the prior art, the invention has the following beneficial effects:
1. the three-gold traditional Chinese medicine composition comprises dry extracts prepared by respectively extracting five medicinal materials of cherokee rose root, chinaroot greenbrier rhizome, sheep mouth, jinsha vine and centella asiatica, and the optimal dry extract preparation process is optimized according to the characteristics of the medicinal materials, so that the loss of active ingredients is less, and the content of the active ingredients in the composition is high.
2. Aiming at the characteristics of different medicinal materials, the extraction mode aiming at each medicinal material is optimized: the cherokee rose root medicinal material and the chinaroot greenbrier medicinal material are extracted by soaking in hot water and extracting for three times; the sheep opening adopts an alkaline water extraction mode, and centella asiatica medicinal materials adopt a mode of steaming and then water extraction; thereby fully utilizing the effective components in each medicinal material and improving the content of the effective components in the traditional Chinese medicine composition.
3. After the five medicinal materials are re-extracted, the five medicinal materials can be further purified by adopting an alcohol precipitation mode, impurities can be removed, the content of active ingredients is improved, and the paste quantity can be properly reduced by adopting an alcohol precipitation process, and active substances can be reserved.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments will be clearly and completely described in conjunction with the embodiments of the present invention, and the following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
Example 1
The preparation method of the dry extract of each medicinal material comprises the following steps:
6Kg of cherokee rose root medicinal material, soaking for 20min with 2 times of hot water, adding 4 times of cold water for extraction for 1.5 hours, filtering, extracting the residues with water twice, adding 5 times of water and 4 times of water respectively, decocting for 1 hour, mixing filtrates, concentrating, and drying to obtain cherokee rose root dry extract;
preparation of chinaroot greenbrier dried paste: 9Kg of chinaroot greenbrier medicinal material, soaking for 20min with 2 times of hot water, adding 4 times of cold water for decoction, controlling the temperature to about 70 ℃, extracting for 2 hours, filtering, extracting residues with water twice, adding 5 times of water and 4 times of water respectively, boiling for 1.5 hours and 1 hour respectively, merging the filtrates, concentrating and drying to obtain chinaroot greenbrier dry paste;
preparing sheep opening dry paste: 6Kg of sheep opening medicinal material, adding 6 times of alkaline water with pH of 8.5 for one time, decocting for 1.5 hours, filtering, extracting residues with water twice, adding 5 times of water and 4 times of water for 1.5 hours and 1 hour respectively, filtering, mixing filtrates, concentrating, and drying to obtain sheep opening dry extract;
preparation of the sargentgloryvine stem dry paste: extracting 6Kg of radix seu herba Kadsurae Longipedunculatae with water twice (8 times and 6 times of water), decocting for 1 hr, filtering, mixing filtrates, concentrating, and drying to obtain radix Kadsurae Longipedunculatae dry extract.
Preparation of centella asiatica dry paste: steaming herba Centellae 6Kg for 25min with steam, adding 8 times of water, decocting for 1.5 hr, filtering, extracting the residue with water twice, adding 6 times of water and 3 times of water respectively, decocting for 1 hr, mixing filtrates, concentrating, and drying to obtain herba Centellae dry extract.
Example 2
The preparation method of the dry extract of each medicinal material comprises the following steps:
preparation of cherokee rose root dry paste: 6Kg of cherokee rose root medicinal material is soaked for 20min by 2 times of hot water, then is added with 4 times of cold water for extraction for 1.5 hours, filtered, the dregs are extracted twice by adding water, the water adding amount is 5 times and 4 times of water respectively, the decoction time is 1 hour, and the filtrates are combined; concentrating the filtrate to relative density of 1.12, adding 80% ethanol for ethanol precipitation (ethanol precipitation concentration of 40% is calculated, supernatant is measured by ethanol and the ethanol content is 14%); recovering ethanol from the ethanol solution, concentrating to about 1.10, and drying to obtain radix Rosae Laevigatae dry extract;
preparation of chinaroot greenbrier dried paste: 9Kg of chinaroot greenbrier medicinal material is soaked for 20min by 2 times of hot water, then is decocted by 4 times of cold water, the temperature is controlled to be about 70 ℃, the extracting is carried out for 2 hours, filtering is carried out, the residues are extracted twice by adding water, the water adding amount is 5 times and 4 times respectively, the micro-boiling time is 1.5 hours and 1 hour respectively, and the filtrates are combined; concentrating the filtrate to relative density of 1.15, adding 80% ethanol for ethanol precipitation (ethanol precipitation concentration of 40% is calculated, supernatant is measured by ethanol and alcohol content is 25%); recovering ethanol from the ethanol solution, concentrating to about 1.10, and drying to obtain rhizoma Smilacis chinensis dry extract;
preparing sheep opening dry paste: 6Kg of sheep opening medicinal material, adding 6 times of sodium hydroxide solution with pH of 8.5 for extraction once, decocting for 1.5 hours, filtering, extracting residues with water twice, adding 5 times of water and 4 times of water respectively, decocting for 1.5 hours and 1 hour, filtering, and mixing filtrates; concentrating the filtrate to relative density of 1.15, adding 80% ethanol for ethanol precipitation (ethanol precipitation concentration of 30% is calculated, and supernatant is measured by ethanol); recovering ethanol from the ethanol solution, concentrating to about 1.10, and drying to obtain sheep opening dry extract;
preparation of the sargentgloryvine stem dry paste: extracting 6Kg of radix seu caulis Kadsurae Longipedunculatae with water twice (8 times and 6 times of water), decocting for 1 hr, filtering, and mixing filtrates; concentrating the filtrate to relative density of 1.12, adding 80% ethanol for ethanol precipitation (ethanol precipitation concentration of 40% is calculated and added, and supernatant is measured by ethanol); recovering ethanol from the ethanol solution, concentrating to about 1.20, and drying to obtain dry extract of caulis Sargentodoxae.
Preparation of centella asiatica dry paste: steaming herba Centellae 6Kg for 25min with steam, adding 8 times of water, decocting for 1.5 hr, filtering, extracting the residue with water twice, adding 6 times of water and 3 times of water respectively, decocting for 1 hr, and mixing filtrates; concentrating the filtrate to relative density of 1.12, adding 80% ethanol for ethanol precipitation (ethanol precipitation concentration of 40% is calculated, supernatant is measured by ethanol and the ethanol content is 14%); recovering ethanol from the ethanol solution, concentrating to about 1.10, and drying to obtain herba Centellae dry extract.
Examples 3 to 6
The dry paste powder of five medicinal materials prepared in the embodiment 1 or 2 is mixed according to a proportion to obtain a three-gold traditional Chinese medicine composition, and the specific composition is shown in the following table 1, wherein the weight parts can be measured in units of gram, kilogram, ton and the like.
TABLE 1
Experimental example 1 study on extraction and purification Process of cherokee rose root
1. Cherokee rose root extraction process
6Kg of cherokee rose root medicinal material is soaked for 20min by 2 times of hot water, then is added with 4 times of cold water for extraction for 1.5 hours, filtered, the dregs are extracted twice by adding water, the water adding amount is 5 times and 4 times respectively, the decoction time is 1 hour, and the filtrates are combined and divided into two parts for standby.
2. Purification process
Concentrating and precipitating the water extract with ethanol: one part of the extract was concentrated to 1.12, and ethanol was added to 80% ethanol for ethanol precipitation (the ethanol precipitation concentration was 40% by calculation, and the content of ethanol in the supernatant was 25% as measured by alcohol).
3. The concentration process comprises the following steps: the ethanol was recovered from the ethanol solution and concentrated to about 1.10.
4. And (3) content measurement: extracting the above samples with n-butanol for three times, collecting n-butanol layer, volatilizing, dissolving in methanol, and fixing volume to 5ml; the sample of the refining process is directly diluted to 5ml by methanol for standby.
Chromatographic conditions: c18 column, mobile phase methanol-water (55:45), evaporative light scattering detector.
The peak area of each component is measured, and the calculation is carried out according to an external standard peak area logarithmic two-point method. And (5) measuring the dry paste rate of the key step, and calculating the yield. The results are shown in Table 2.
The content of the effective components in the cherokee rose root medicinal material in the test is detected by adopting the same method: 0.074% rose glycoside (4.44 g) and 0.066% rose glycoside (3.96 g).
TABLE 2 extraction yield and yield of the ingredients from each step during the cherokee rose root extraction process
From the results, the cherokee rose root medicinal material is soaked in 2 times of hot water for 20 minutes and then is decocted with water for three times, the extraction solutions are combined, the extraction rate of the rosa multiflora glucoside can reach 43.45%, the extraction rate of the rosa multiflora glucoside can reach 56.47%, and the dry paste rate is 10.32%, so that the saponin components can be extracted by three times of water extraction.
The alcohol precipitation process can reduce the amount of paste properly and retain active matters.
Experimental example 2 research on extraction and purification process of smilax china
1. Smilax extraction process
9Kg of chinaroot greenbrier medicinal material is soaked for 20min by 2 times of hot water, then is decocted by 4 times of cold water, the temperature is controlled to be about 70 ℃, the extracting is carried out for 2 hours, filtering is carried out, the residues are extracted twice by adding water, the water adding amount is 5 times and 4 times respectively, the micro-boiling decoction time is 1.5 hours and 1 hour respectively, and the filtrates are combined and divided into three parts for standby.
2. Purification process
Concentrating and precipitating the water extract with ethanol: concentrating one part of the extractive solution to 1.15, adding 80% ethanol for ethanol precipitation (40% ethanol precipitation concentration is calculated, the supernatant is measured by ethanol and the ethanol content is 25%)
3. Concentration process the ethanol solution described above was recovered and concentrated to about 1.1.
4. Content determination
Preparing the above samples for measuring flavonoid components, extracting unrefined sample with n-butanol under shaking for three times, collecting n-butanol layer, volatilizing, dissolving in methanol, and fixing volume to 5ml; the sample of the refining process is directly diluted to 5ml by methanol for standby.
Preparing chlorogenic acid-measuring samples, adjusting unrefined samples to 1.5 with hydrochloric acid, extracting with n-butanol under shaking for three times, collecting n-butanol layer, volatilizing, dissolving with methanol, and fixing volume to 5ml; the sample of the refining process is directly diluted to 5ml by methanol for standby.
Chromatographic conditions column C18 um (4.6x250 mm), mobile phase: acetonitrile as mobile phase a and 0.1% phosphoric acid solution as mobile phase B, gradient elution was performed as specified in table 3, and the detection wavelength: 290nm.
TABLE 3 elution gradient
| Time (minutes) | Mobile phase a | Mobile phase B |
| 0～20 | 5.0～9.0 | 95.0～91 |
| 25～76 | 12～17.5 | 88～82.5 |
| 78～83 | 90.0 | 10.0 |
The dry extract rate of the key step was measured, the yield thereof was calculated, and the results are shown in Table 4.
The content of the effective components in the medicinal materials in the test is detected by adopting the same method: chlorogenic acid is 0.228%, arillus longan glycoside is 0.056%, astilbin is 0.578%, resveratrol is 0.064%, and engelhardin is 0.045%.
TABLE 4 transfer rates and yields of ingredients from the various procedures during the smilax extraction Process
Results: the chinaroot greenbrier medicinal material is subjected to enzyme deactivation and glycoside preservation and then is extracted by water for three times, the extraction rate of chlorogenic acid extracted by water for the first time can reach 64.43 percent, the extraction rate of the longan glycoside is 17.86 percent, the extraction rate of chlorogenic acid extracted for the second time is 31.57 percent, and the extraction rate of the longan glycoside is 9.0 percent; the extraction rate of chlorogenic acid extracted for the third time is 7.5%, the extraction rate of the longan aril is 2.85%, the total extraction rate of chlorogenic acid in the extraction stage can reach more than 98%, and the dry paste rate is 16.02%, which indicates that the components to be detected can be completely extracted by the second water extraction.
Purifying by alcohol precipitation, wherein the transfer rate of flavone by 40% alcohol precipitation method is 6.5%, the transfer rate of chlorogenic acid is 46.9%, and the dry extract rate is 8.4%.
Experimental example 3 sheep open extraction purification process study
1. Sheep opening extraction process
6Kg of sheep opening medicinal material, adding 6 times of sodium hydroxide solution with pH of 8.5 for extraction once, decocting for 1.5 hours, filtering, extracting residues with water twice, adding 5 times of water and 4 times of water for 1.5 hours and 1 hour respectively, filtering, mixing filtrates, and dividing into two parts for later use.
2. Purification process
Concentrating and precipitating the water extract with ethanol: concentrating one part of the extractive solution to 1.15, adding 80% ethanol, and precipitating with ethanol (30% ethanol concentration is calculated, supernatant is measured by alcohol meter, and alcohol content is not measured)
3. Concentration process the ethanol solution described above was recovered and concentrated to about 1.1.
4. Content determination
Gallic acid sample treatment: taking the samples, evaporating the water extract to dryness, adding 20% methanol for dissolution, and fixing the volume to 5ml; the sample of the refining process is directly diluted to 5ml with 20% methanol for later use.
Ellagic acid sample treatment: taking the samples, evaporating the water extract to dryness, adding 80% acetone for dissolution, and fixing the volume to 5ml; the sample of the refining process is directly diluted to 5ml with 20% acetone for standby.
Chromatographic conditions C18 column, gallic acid mobile phase acetonitrile-0.1% formic acid (5:95), detection wavelength: 246nm;
ellagic acid mobile phase was acetonitrile-0.1% formic acid (26:74), detection wavelength: 270nm.
The peak area of each component was measured and calculated according to the external standard method.
And (5) measuring the dry paste rate of the key step, and calculating the yield. The results are shown in Table 5.
The content of the effective components in the medicinal materials in the test is detected by adopting the same method: gallic acid 0.05% and ellagic acid 0.067%.
TABLE 5 transfer rates and paste yields of the Process Components during the sheep opening extraction Process
Results: extracting sheep opening medicinal materials with water for three times, wherein the extraction rate of extracting gallic acid with a small amount of alkali is 41.2% in the first time, the extraction rate of extracting gallic acid with water is 25.49% in the second time, the extraction rate of extracting gallic acid is 11.51% in the third time, the extraction rate of gallic acid in mixed extracting solution after combining the three extracting solutions is 79.19%, ellagic acid is almost insoluble in water, the extraction rate is very low, and the total of three extracting solutions is less than 2%; the dry paste rate is 17.05%.
And 3, the ethanol precipitation and purification, namely, 30% ethanol precipitation has good transfer rate of two measured components, the dry paste rate is 10%, and the dry paste rate is reduced compared with 17.05% of the dry paste extracted by water.
And (3) comprehensively analyzing, extracting the sheep mouth by adopting a small amount of alkali to perform water extraction, wherein the extraction rate of the organic acid is relatively complete, the organic acid is relatively well enriched by an alcohol precipitation method, and the paste yield can be effectively controlled.
In this test example, the alkali water may be replaced with sodium bicarbonate solution, sodium carbonate solution, or lime water having a pH of 8.5, and the extraction results are similar and will not be repeated here.
Experimental example 4 research on extraction and purification process of jinsha vine
1. Process for extracting sargentgloryvine stem
6Kg of sargentgloryvine stem, extracting twice with water in an amount of 8 times and 6 times, decocting for 1 hr, filtering, mixing the filtrates, and dividing into two parts for use.
2. Purification process
Concentrating and precipitating the water extract with ethanol: concentrating one part of the extractive solution to 1.12, adding 80% ethanol, precipitating with ethanol (40% ethanol concentration is calculated, and the supernatant is measured with alcohol meter, and the ethanol content is not measured)
3. Concentrating the above ethanol solutions to recover ethanol and concentrate to 1.20.
4. Content determination
Extracting the above samples with n-butanol for three times, collecting n-butanol layer, volatilizing, dissolving in methanol, and fixing volume to 5ml; the sample of the refining process is directly diluted to 5ml by methanol for standby.
Chromatographic conditions acetonitrile-0.2% aqueous phosphoric acid (16:84), detection wavelength: 254nm.
The peak areas of the components are measured, and the peak areas are calculated according to external standards.
And (5) measuring the dry paste rate of the key step, and calculating the yield. The results are shown in Table 6.
The content of the effective components in the medicinal materials in the test is detected by adopting the same method: isoquercitrin is 0.034% and astragalin is 0.021%.
TABLE 6 transfer rates and paste yields of Process Components during the Stephania sinica Diels extraction Process
Analysis of results: the sarcandra glabra medicinal material is subjected to twice water extraction, and the extraction rate of isoquercitrin in the mixed extraction solution is 51.71% after the two extraction solutions are combined, so that the extraction rate of astragalin can reach 62.00%; after steam, the saponins can be extracted basically by two water extractions. The alcohol precipitation process can reduce the amount of paste properly and retain active matters.
Experimental example 5 study on extraction and purification Process of centella asiatica
1. Centella extraction process
6Kg of centella asiatica medicinal material is steamed for 25min by steam, 8 times of water is added for decoction for 1.5 hours, filtering is carried out, the decoction dregs are extracted twice by adding water, the water adding amount is 6 times of water and 3 times of water respectively, the decoction time is 1 hour, and the filtrates are combined and divided into three parts for standby.
2. Purification process
Concentrating and precipitating the water extract with ethanol: one part of the extract was concentrated to 1.12, and ethanol was added to 80% ethanol for ethanol precipitation (the ethanol precipitation concentration was 40% by calculation, and the content of ethanol in the supernatant was 14% as measured by alcohol meter).
3. Concentration process each of the ethanol solutions described above was recovered and concentrated to about 1.10.
4. Content determination
Taking the samples of the steps, preparing a test solution according to the content measurement items of the Sanjin tablets in the pharmacopoeia, measuring the content of asiaticoside B, madecassoside and asiaticoside according to the chromatographic condition of one-measurement-multiple-evaluation, and calculating the transfer rate.
The dry paste rate of the key step was measured, and the paste yield was calculated, and the results are shown in Table 7.
The content of the effective components in the medicinal materials in the test is detected by adopting the same method: asiaticoside B0.602% (36.12 g), madecassoside 1.53% (91.8 g), asiaticoside 0.66% (39.6 g).
TABLE 7 transfer rates and yields of ingredients from the various procedures during the centella extraction process
Analysis of results: steaming herba Centellae herb for 25min, decocting in water, mixing three extractive solutions, wherein the extraction rate of asiaticoside in the mixed extractive solution can reach 73% or more, the extraction rate of madecassoside can reach 81% or more, and the extraction rate of asiaticoside can reach 70.03% or more; the three water extractions are described to basically extract the saponins.
Test example 6
In the test example, the data of the group 1 and the group 2 are prepared from the same amount of medicinal materials in the same batch, wherein the group 1 is the content of each component in dry paste powder prepared by respectively and independently extracting five medicinal materials (refer to the method of the embodiment 1) and converting the raw measurement data (refer to the test examples 1-5) obtained by measurement into the content of each component in each three gold tablets, and the group 2 is the content of each component in dry paste powder prepared by mixing and extracting the five medicinal materials by adopting a preparation method in pharmacopoeia; groups 3-5 are the contents of each component in the three-gold-plate mixed dry paste prepared in three batches in a workshop. The results are shown in Table 8.
TABLE 8
From the data in the above table 8, the content of the effective components of centella asiatica, cherokee rose root and chinaroot greenbrier which are extracted independently and isoquercitrin in the jinsha vine are higher than that of the dry extract powder which is extracted by mixing, which shows that the single extraction has certain advantages. In addition, the gallic acid data of sheep mouth is low, probably because the compound is also present in other medicinal materials; compared with the dry extract powder extracted by mixing the three golden tablets, the centella asiatica has certain advantages in all the measured components.
The foregoing description is only illustrative of the preferred embodiment of the present invention, and is not to be construed as limiting the invention, but is to be construed as limiting the invention to any and all simple modifications, equivalent variations and adaptations of the embodiments described above, which are within the scope of the invention, may be made by those skilled in the art without departing from the scope of the invention.
Claims (10)
1. The Sanjin traditional Chinese medicine composition is characterized by comprising the following components in parts by weight:
14.5 to 20.6 parts of cherokee rose root dry extract, 9.6 to 16 parts of chinaroot greenbrier rhizome dry extract, 11 to 16.8 parts of sheep opening dry extract, 3.48 to 7.57 parts of jinsha vine dry extract and 6.5 to 13.8 parts of centella asiatica dry extract;
the preparation method of the cherokee rose root dry paste comprises the following steps: soaking radix Rosae Laevigatae in 2 times of hot water at 60-100deg.C for 10-30min, decocting with 4 times of water for 1.5 hr, filtering, extracting residues with water twice, mixing filtrates, concentrating, and drying to obtain radix Rosae Laevigatae dry extract;
the preparation method of the smilax glabra dry paste comprises the following steps: soaking rhizoma Smilacis chinensis in 2 times of hot water at 60-100deg.C for 10-30min, decocting in 4 times of cold water, controlling temperature to 50-70deg.C, extracting for 2 hr, filtering, extracting residues with water twice, and mixing filtrates; concentrating, and drying to obtain rhizoma Smilacis chinensis dry extract;
the preparation method of the sheep opening dry paste comprises the following steps: extracting sheep opening medicinal material with 6 times of alkaline water with pH of 8-10 for 1.5 hr, filtering, extracting residues with water twice, filtering, and mixing filtrates; concentrating, and drying to obtain sheep opening dry extract;
the preparation method of the sargentgloryvine stem paste comprises the following steps: extracting radix seu herba Kadsurae Longipedunculatae with water twice (8 times and 6 times of water), decocting for 1 hr, filtering, and mixing filtrates; concentrating, and drying to obtain dry extract of caulis Sargentodoxae;
the preparation method of the centella asiatica dry paste comprises the following steps: heating herba Centellae with steam for 15-40min, decocting with water for 3 times, mixing filtrates, concentrating, and drying to obtain herba Centellae dry extract;
the preparation process of the dry paste of each component further comprises a purification process: mixing filtrates, concentrating to relative density of 1.12-1.15, adding 80% ethanol for ethanol precipitation, recovering ethanol from ethanol solution, and concentrating to relative density of 1.1-1.2; drying to obtain dry extract.
2. The Sanjin traditional Chinese medicine composition according to claim 1, which is characterized by comprising the following components in parts by weight: 14.5-18 parts of cherokee rose root dry paste, 9.6-12 parts of chinaroot greenbrier dry paste, 12-15 parts of sheep opening dry paste, 4.1-6.8 parts of gold Sha Tenggan paste and 7-12 parts of centella dry paste.
3. The Sanjin traditional Chinese medicine composition according to claim 1, wherein in the preparation method of the cherokee rose root dry extract, water is added for extraction in the last two times, the water adding amount is 5 times and 4 times respectively, and the decoction time is 1 hour.
4. The Sanjin traditional Chinese medicine composition according to claim 1, wherein in the preparation method of the chinaroot greenbrier rhizome dry paste, when water is added for extraction in the last two times, the water adding amount is 5 times and 4 times, and the decoction time is 1.5 hours and 1 hour respectively.
5. The Sanjin traditional Chinese medicine composition according to claim 1, wherein in the preparation method of the sheep opening dry paste, the water adding amount is 5 times and 4 times respectively in the two later water adding extraction processes, and the decoction time is 1.5 hours and 1 hour respectively.
6. The composition of claim 5, wherein the alkaline water is selected from sodium bicarbonate solution, sodium carbonate solution, sodium hydroxide solution, lime water.
7. The Sanjin traditional Chinese medicine composition according to claim 1, wherein in the preparation method of the centella asiatica dry extract, 8 times of water is added for the first time, the centella asiatica dry extract is decocted for 1.5 hours, filtering is carried out, the dregs are extracted twice by adding water, the water adding amount is 6 times and 3 times of water adding amount respectively, and the decoction time is 1 hour.
8. The three-gold traditional Chinese medicine composition according to any one of claims 1-7, wherein the three-gold traditional Chinese medicine composition is prepared into a conventional dosage form.
9. The Sanjin traditional Chinese medicine composition of claim 8, wherein the dosage form is a granule, a pill, a powder, a capsule or a tablet.
10. A method for preparing a sanjin traditional Chinese medicine composition as claimed in any one of claims 1-7, characterized in that the prescription amount of cherokee rose root, chinaroot greenbrier rhizome, sheep's mouth, jinsha vine and asiatic centella herb materials are respectively prepared into dry paste separately, and the dry paste powder of each component is mixed according to the mass ratio.
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| CN1733273A (en) * | 2005-08-15 | 2006-02-15 | 贵阳云岩西创药物科技开发有限公司 | Pulean pharmaceutical preparation, process for preparing the same and quality controlling method thereof |
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