CN111671820A - Method for preparing belladonna fluid extract by bionic compounding - Google Patents
Method for preparing belladonna fluid extract by bionic compounding Download PDFInfo
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
The quality of the existing belladonna medicinal materials is unstable, which causes the unstable quality of belladonna liquid extract. Meanwhile, in the Chinese pharmacopoeia, the content of tropane alkaloid is required to be more than or equal to 0.30 percent in terms of hyoscyamine in the determination item of the belladonna raw medicinal material, and a scientific content interval is not set. Therefore, the belladonna liquid extract has unstable quality such as overhigh alkaloid content and the like, and the situation of unstable curative effect is caused. The invention provides a scientific bionic formula for preparing the belladonna fluid extract, realizes the stable content of each main tropane alkaloid in the belladonna fluid extract and improves the stability of the belladonna fluid extract.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a method for preparing belladonna fluid extract by bionic compounding.
Background
Belladonna, Atropa belladonna, is a perennial herb of the genus Atropa of the family Solanaceae. Belladonna native Europe, introduced to China in the 30 th 20 th century, is an unlimited growth type, perennial herb of belladonna. At present, the medicinal belladonna in China is an artificial cultivation product and is a year-old. Belladonna fluid extract is a product recorded in Chinese pharmacopoeia, has the main medicinal component of tropane alkaloid, has the effects of resisting choline medicaments, relieving smooth muscle spasm and inhibiting glandular secretion, and can be used for treating gastric and duodenal ulcer, gastrointestinal tract, kidney, biliary colic and the like.
Belladonna is a foreign species, and since the last 30 centuries, artificial cultivation has been successfully achieved in China. In recent years, with the enlargement of planting regions, on one hand, the tropine alkaloid content in the belladonna grass is in a trend of gradually decreasing due to the degeneration of germplasm; on the other hand, with the increase of planting regions, different planting conditions and climatic environments cause great difference of alkaloid content in belladonna, and the total content of belladonna is in a descending trend. Therefore, the variation range of tropane alkaloids in the belladonna fluid extract is large, and the total alkaloid content in the belladonna fluid extract cannot reach the specification of pharmacopoeia. Moreover, the difference of the contents of main alkaloids in tropane alkaloids in the belladonna fluid extract is large, and the belladonna fluid extract cannot meet the detection requirement of fingerprint spectrum method in pharmacopoeia.
The provision of Chinese pharmacopoeia indicates that the belladonna liquid extract is prepared from belladonna herbs, but in order to improve the clarity of the product, part of enterprises artificially reduce the dosage of belladonna leaves, which often causes the quality of the belladonna liquid extract to be unstable or even not reach the standard. Meanwhile, in the Chinese pharmacopoeia, the content of tropane alkaloid is required to be more than or equal to 0.30 percent in terms of hyoscyamine in the belladonna raw medicinal material content measurement item, and a scientific content interval is not set. Therefore, the belladonna liquid extract has unstable quality such as overhigh alkaloid content and the like, and the situation of unstable curative effect is caused. Similarly, the quality of belladonna fluid extract in the Chinese pharmacopoeia is regulated to be not less than 6.6mg in terms of atropine sulfate per 1mL, and no upper limit of alkaloid content is regulated. These are very disadvantageous for safe administration, and the high alkaloid content is liable to cause strong side effects, such as hyperventilation, arrhythmia, heart failure and other symptoms.
However, the alkaloid content of belladonna has a great relationship with the temperature, humidity and climate conditions of the planting field, soil fertility, illumination environment, growth period, harvest period and the like, and even plants have annual and perennial differences. In such complex growth situations, the alkaloid content of belladonna and the alkaloid content of belladonna fluid extract fluctuate greatly, resulting in unstable quality of belladonna fluid extract and poor quality stability between batches.
Meanwhile, the quality of belladonna in different producing areas is different, so that the content difference of alkaloid in the extracted fluid extract is large; the alkaloid content in the fluid extract extracted from belladonna (such as more leaves and less leaves) with different qualities even in the same producing area is greatly different; the belladonna harvested in the same producing area on the same day has different quality due to soil fertility, and the belladonna harvested in the same producing area has the same difficulty in uniformity in quality because the belladonna harvested in the same producing area ripens early in sunny slopes and ripens late in flat and low-lying areas. These all have an influence on the quality of belladonna fluid extract, and if the content of alkaloid is too low, the alkaloid does not reach the standard, and if the content of alkaloid is too high, serious adverse reaction is easily caused. Meanwhile, the existing Chinese pharmacopoeia requires that the belladonna fluid extract is extracted by using dry belladonna herbs, but the method easily causes the unqualified rate of products in the practical application process due to the large quality deviation of the belladonna herbs, for example, some belladonna herbs have poor growth and less leaves and are picked up with broken roots, and the phenomena of small rhizome, less seeds and the like caused by poor soil fertility, so the belladonna herbs can accord with the specification of the Chinese pharmacopoeia on the belladonna herbs, but the fluid extract has poor quality. Therefore, the development of a preparation method for improving the quality stability of the belladonna fluid extract is of great significance.
The bionic compound preparation method provided by the invention can improve the quality of the belladonna fluid extract and realize the stability of the content of each main tropane alkaloid in the belladonna fluid extract. In the earlier stage of the application, measurement and statistical analysis are carried out on mass samples, a scientific bionic formula for preparing the belladonna fluid extract is formulated, and the content stability of each main tropane alkaloid in the belladonna fluid extract is improved.
Disclosure of Invention
Collecting 1000 parts of belladonna samples in different producing areas (Jiangxi province, Shandong province, Hunan province and Heilongjiang province) in the harvesting period, uniformly drying, and carrying out statistical analysis on the dry weight of roots, stems, leaves and seeds in the dried whole grass to obtain the weight ratio of all parts of the belladonna whole grass, wherein the root weight is 10-25% of the whole plant, the stem weight is 40-65% of the whole plant, the leaf weight is 10-25% of the whole plant, and the seed weight is 5-15% of the whole plant.
The content of tropine alkaloid in roots, stems, leaves and seeds in 1000 samples of Jiangxi province, Shandong province, Hunan province and Heilongjiang province is detected, and the average value and the deviation of the tropine alkaloid are calculated through statistical analysis. The average content of total alkaloids in the root of belladonna is 0.56%, the average content of total alkaloids in the stem is 0.17%, the average content of total alkaloids in the leaf is 0.43%, and the average content of total alkaloids in the seed is 0.59%.
Belladonna is the main commercial cultivation medicine source of scopolamine and hyoscyamine, and is also the only medicine source plant of tropane alkaloids specified in Chinese pharmacopoeia. The belladonna contains tropane alkaloids of hyoscyamine, and mainly contains hyoscyamine (hyoscyamine, atropine, anisodamine, scopolamine and anisodamine). Generally, during the extraction process, levorotatory hyoscyamine is easy to be converted into racemate (i.e. atropine), so the content of hyoscyamine in the medicinal extract is calculated by the racemate. The three major alkaloids are structurally similar, but differ significantly in polarity. For example, the partition coefficients of anisodamine and scopolamine fatty water are 0.839 and 0.856, respectively, and the partition coefficient of anisodamine fatty water is 1.869.
In order to clearly reveal the specific distribution of tropane alkaloids in different parts of belladonna, the content difference of various alkaloids (levorotatory hyoscyamine, atropine, scopolamine, anisodamine and anisodamine) in roots, stems, leaves and seeds is respectively determined and analyzed. The research result shows that the content of various alkaloids in different parts of belladonna is greatly different. Based on the discovery, the invention provides a method for preparing the belladonna fluid extract by bionic compound preparation, and different extraction processes are developed for different parts in sequence, so that the bionic compound fluid extract prepared by the method can overcome the practical situations of different belladonna qualities and different plant qualities in different production places, and the bionic compound fluid extract has stable and reliable quality.
The bionic compounding method is based on the premise that each part of belladonna is respectively extracted to prepare a fluid extract, and all effective components of belladonna are maintained and kept stable by performing bionic compounding on the whole belladonna plant and the fluid extract of each part. The method can overcome the problem of unstable belladonna quality caused by different producing areas and different harvesting periods, and the belladonna product has high quality uniformity.
Based on the high content of atropine in roots and seeds, the invention improves the ethanol concentration of the prior production process in order to improve the content of levorotatory hyoscyamine. Weighing 1000g of roots and seeds respectively, adding 80-95% of ethanol according to the mass ratio of the material liquid to 1 (belladonna roots or seeds) to 2-5 (extracting solution), soaking for 36-72 hours at 35-45 ℃, and percolating and extracting at room temperature. And controlling the percolation speed to be 1-3 ml per minute to obtain primary percolate. Continuously percolating to obtain continuous percolate as solvent for next percolation. Recovering ethanol from the primary percolate under reduced pressure at 60 deg.C, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60-70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, collecting the upper liquid after precipitation, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain the extract of belladonna root and seed.
In addition, the contents of anisodamine and scopolamine are higher in the belladonna leaves and belladonna stems. The invention designs the following extraction process: 1000g of belladonna leaves and stems are taken, crushed, added with 50-65% of ethanol according to the mass ratio of 1 (belladonna leaves or belladonna stems) to 30-50 (extracting solution), soaked for 36-72 hours at the temperature of 35-45 ℃, then extracted under reflux for 6-12 hours, and extracted twice. Filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60-70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, collecting the upper filtrate, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract. Respectively extracting to obtain fluid extracts of leaves and stems of belladonna.
According to the weight ratio of root, stem, leaf and seed in belladonna plant, the content difference of various alkaloids in different parts, and the extract yield of each part. Through repeated blending and statistical analysis, the root fluid extract with the mass of 15-25 parts, the stem fluid extract with the mass of 45-60 parts, the leaf fluid extract with the mass of 10-15 parts and the seed fluid extract with the mass of 10-15 parts are uniformly mixed, a proper amount of 85% ethanol is added, and the mixture is diluted with water, so that the alkaloid and ethanol content meets the requirements, the mixture is kept stand, cleared and filtered, and the bionic compound fluid extract is obtained.
The bionic compound fluid extract comprises 0.043-0.051 mg/mL of scopolamine, 0.022-0.029 mg/mL of atropine and 0.410-0.450 mg/mL of scopoletin; the content of the total alkaloids is 7.6-8.1 mg/mL calculated by henbane.
The invention separately extracts different parts of belladonna, and then designs reasonable compounding proportion based on the weight ratio of each part of the whole plant and the content of each main alkaloid, and the obtained belladonna fluid extract has the main advantages that:
1. the phenomenon of sudden reduction or deletion of certain parts in the entire belladonna plants in different harvesting periods in actual production is avoided, for example, the phenomenon that leaves in the late harvesting period are greatly reduced, the content of seeds in the early harvesting period is low, and even no seeds exist, so that the fluid extract extracted from belladonna in different growth periods and different growth vigors can achieve the effect of stable quality, and the effect of high-quality belladonna can be achieved through bionic compounding;
2. the problem of large quality variation of the fluid extract caused by different quality of belladonnas produced in different regions is avoided, so that the fluid extract extracted from the belladonnas in different producing areas can achieve the effect of stable quality;
3. the regulation of the current pharmacopoeia only regulates the lower limit of each alkaloid content in the belladonna fluid extract, but does not regulate the upper limit of each alkaloid, so that the phenomenon that the alkaloid content of a part of batches is overhigh is often caused, and the fluid extract obtained by the compounding proportion can maximally realize the stability of quality on the current level;
4. different extraction processes are designed by analyzing the content difference of alkaloids in different parts, so that the extraction rate of the alkaloids is improved more effectively and pertinently, and the drug effect of belladonna is improved;
5. although the belladonna fluid extract is prepared from belladonna dry herbs in Chinese pharmacopoeia, the alkaloid contained in belladonna has strong parasympathetic nerve inhibiting effect and strong stimulating effect on respiration and heartbeat, the existing quality standard of the belladonna fluid extract is only specified by the lower limit of the content of the alkaloid, and does not have the upper limit limitation and the batch stability specification, which is very unfavorable for safe medication and is easy to cause strong side reactions, such as symptoms of hyperventilation, arrhythmia, heart failure and the like, the invention can effectively improve the quality stability and the batch stability of the belladonna fluid extract, can effectively reduce the occurrence of adverse reactions, and is powerful improvement and supplement for the prior art and the standard;
6. the method can be suitable for the belladonna grass raw materials in various growing environments, the influence of the quality difference of the raw materials on the quality of the fluid extract is reduced to the minimum, the belladonna grass which is not good in growth and has few leaves and broken roots in picking and has small rhizome, few seeds and the like caused by poor soil fertility can be utilized and prepared into the qualified fluid extract, the utilization rate of the belladonna grass is improved, and the method has obvious effect compared with the method for preparing the fluid extract by using the whole grass.
Detailed Description
Example 1
Extracting root and seed of belladonna separately:
in the preparation process of the intermediate extract of belladonna root or seed, adding 95% ethanol into 2 (extract) according to the mass ratio of 1 (belladonna root or seed) and soaking at 45 deg.C for 36 hr, and percolating at room temperature to extract; controlling the percolation speed to be 1ml per minute to obtain primary percolate; continuously percolating to obtain a continuous percolate as a solvent for the next percolation; recovering ethanol from the primary percolate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, sucking the upper liquid, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain the soft extract of belladonna root and seed.
Extracting belladonna leaf and belladonna stem respectively:
pulverizing belladonna leaf or belladonna stem, adding 65% ethanol into 30 (extractive solution) according to the material liquid mass ratio of 1 (belladonna leaf or belladonna stem), soaking at 45 deg.C for 36 hr, reflux extracting for 6 hr, and repeating the extraction twice; filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, collecting the upper filtrate, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract of leaves and stems of Atropa belladonna;
bionic compound fluid extract
Uniformly mixing 25 parts by mass of root fluid extract, 45 parts by mass of stem fluid extract, 10 parts by mass of leaf fluid extract and 10 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 1:
example 2
Extracting root and seed of belladonna separately:
in the preparation process of the intermediate extract of belladonna root or seed, adding 85% ethanol into 3 (extract) according to the mass ratio of 1 (belladonna root or seed) of the liquid, soaking at 40 deg.C for 54 hr, and percolating at room temperature to extract; controlling the percolation speed at 2ml per minute to obtain primary percolate; continuously percolating to obtain a continuous percolate as a solvent for the next percolation; recovering ethanol from the primary percolate under reduced pressure at 60 deg.C, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 65 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, sucking the upper liquid, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain the extract of belladonna root and seed.
Extracting belladonna leaf and belladonna stem respectively:
pulverizing belladonna leaf or belladonna stem, adding 55% ethanol into 40 (extractive solution) at 40 deg.C, soaking at 40 deg.C for 54 hr, reflux extracting for 9 hr, and repeating the extraction twice; filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 65 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, collecting the upper filtrate, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract of leaves and stems of Atropa belladonna;
bionic compound fluid extract
Uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 2:
example 3
Extracting root and seed of belladonna separately:
in the preparation process of the intermediate extract of belladonna root or seed, adding 80% ethanol into 5 (extract) of belladonna root or seed at a material liquid mass ratio of 1, soaking at 35 deg.C for 72 hr, and percolating at room temperature to extract; controlling the percolation speed to be 3ml per minute to obtain primary percolate; continuously percolating to obtain a continuous percolate as a solvent for the next percolation; recovering ethanol from the primary percolate under reduced pressure at 60 deg.C, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, sucking the upper liquid, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain the extract of belladonna root and seed.
Extracting belladonna leaf and belladonna stem respectively:
pulverizing belladonna leaf or belladonna stem, adding 50% ethanol into 50 (extractive solution) at a mass ratio of 1 (belladonna leaf or belladonna stem), soaking at 35 deg.C for 72 hr, reflux-extracting for 12 hr, and repeating the extraction twice; filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, collecting the upper filtrate, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract of leaves and stems of Atropa belladonna;
bionic compound fluid extract
Uniformly mixing 15 parts by mass of root fluid extract, 60 parts by mass of stem fluid extract, 15 parts by mass of leaf fluid extract and 15 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 3:
comparative example 1
The whole belladonna plant is sampled for extraction, the extraction method is the same as that of the root and the seed in the example 2, and the preparation of the bionic compound fluid extract is the same as that in the example 2.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 4:
comparative example 2
The whole belladonna plant is sampled for extraction, the extraction method is the same as that of the leaves and stems in the example 2, and the preparation of the bionic compound fluid extract is the same as that in the example 2.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 5:
comparative example 3
Extracting root and seed of belladonna separately:
in the preparation process of the intermediate extract of belladonna root or seed, 70% ethanol is added into 1.5 (extract) of belladonna root or seed in the material liquid mass ratio of 1, and the extract is soaked for 24 hours at 50 ℃ and percolated and extracted at room temperature; controlling the percolation speed to be 5ml per minute to obtain primary percolate; continuously percolating to obtain a continuous percolate as a solvent for the next percolation; recovering ethanol from the primary percolate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 75 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, sucking the upper liquid, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain the extract of belladonna root and seed.
Extracting belladonna leaf and belladonna stem respectively:
pulverizing belladonna leaf or belladonna stem, adding 75% ethanol into 20 (extractive solution) at a mass ratio of 1 (belladonna leaf or belladonna stem), soaking at 50 deg.C for 24 hr, reflux-extracting for 5 hr, and repeating the extraction twice; filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 75 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, precipitating completely, collecting the upper filtrate, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract of leaves and stems of Atropa belladonna;
bionic compound fluid extract
Uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 6:
comparative example 4:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 14 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 7:
comparative example 5:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: the bionic compound fluid extract is prepared by uniformly mixing 26 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 8:
comparative example 6:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 42 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 9:
comparative example 7:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 63 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 10:
comparative example 8:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 9 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 11:
comparative example 9:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 16 parts by mass of leaf fluid extract and 12 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 12:
comparative example 10:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 9 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 13:
comparative example 11:
the method for extracting the root, the seed, the leaf and the stem of the belladonna is as in example 2, the bionic compound fluid extract is respectively compounded by four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna, and the compounding ratio of the four intermediate extracts of the root, the stem, the leaf and the seed of the belladonna is as follows: uniformly mixing 20 parts by mass of root fluid extract, 50 parts by mass of stem fluid extract, 12 parts by mass of leaf fluid extract and 16 parts by mass of seed fluid extract, adding a proper amount of 85% ethanol, and diluting with water to obtain the bionic compound fluid extract.
The alkaloid content of the bionic compound fluid extract prepared by the steps is measured by liquid chromatography by using belladonna produced in Jiangxi province, Shandong province, Hunan province and Heilongjiang province as raw materials, and the results are shown in Table 14:
to summarize: from the above results, it can be seen that belladonna quality varies from region to region, resulting in unstable quality of the fluid extract. Moreover, if the whole plant is used for extraction, the alkaloid content in the extract is greatly different, and like the comparative example 1 and the comparative example 2, the whole plant causes the belladonna fluid extract quality in different producing areas to be greatly different, which is not beneficial to the stability of belladonna products. The scientific bionic formula for preparing the belladonna fluid extract improves the quality of the belladonna fluid extract and realizes the stability of the content of each main tropine alkane alkaloid in the belladonna fluid extract. In the bionic compound fluid extract extracted from belladonna produced in each region of examples 1-3, the content of scopolamine is 0.043-0.051 mg/mL, the content of atropine is 0.022-0.029 mg/mL, and the content of scopoletin is 0.410-0.450 mg/mL; the content of total alkaloids is 7.6-8.1 mg/mL calculated by henbane, the distribution interval is small, the quality fluctuation is small, and the quality is more stable.
From the comparison example 1 (whole plant extraction) and the comparison example 2 (whole plant extraction), the bionic compound fluid extracts extracted from belladonna in different areas have different alkaloid contents and large total alkaloid content difference, and the comparison example 3 (different parameters) reduces the alkaloid contents, which shows that the extraction process of the root, the seed, the stem and the leaf of the belladonna is effective and optimized. Meanwhile, the root, the seed, the stem and the leaf of the belladonna are extracted and proportioned separately, so that the bionic compound fluid extract extracted from the belladonna with different growth vigors and different growth periods is favorable for stable quality. The content deviation of the total alkaloids in comparative examples 4-11 (different fluid extract ratios) is large, and the quality of the bionic compound fluid extract is unstable.
The above examples and comparative examples are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention has been described in detail by the above examples and comparative examples, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the present invention as defined by the claims.
Claims (2)
1. A method for preparing belladonna fluid extract by bionic compound preparation is characterized in that:
the preparation method of the intermediate extract of belladonna root, seed, leaf and stem has the following characteristics:
(1) in the preparation process of the intermediate extract of the belladonna root or the belladonna seed, the extract is prepared by the following steps: adding 80-95% ethanol into the extracting solution according to the material-liquid mass ratio of 1: 2-5, soaking for 36-72 hours at 35-45 ℃, and percolating and extracting at room temperature; controlling the percolation speed to be 1-3 ml per minute to obtain primary percolate; continuously percolating to obtain a continuous percolate as a solvent for the next percolation; recovering ethanol from the primary percolate under reduced pressure at 60 deg.C, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60-70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, collecting the upper liquid after precipitation, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain belladonna root and seed extracts;
(2) after the belladonna leaves or belladonna stems are crushed, the weight ratio of the belladonna leaves or belladonna stems is as follows: adding 50-65% ethanol into the extracting solution according to the material-liquid mass ratio of 1: 30-50, soaking for 36-72 hours at 35-45 ℃, then performing reflux extraction for 6-12 hours, and repeating the extraction twice; filtering, recovering ethanol from the filtrate at 60 deg.C under reduced pressure, cooling to room temperature, separating to remove chlorophyll, filtering, steaming the filtrate at 60-70 deg.C to obtain soft extract, adding 10 times of 85% ethanol, stirring, standing, collecting the upper liquid after precipitation, recovering ethanol at 60 deg.C under reduced pressure, and concentrating to obtain soft extract of leaves and stems of Atropa belladonna;
(3) the bionic compound fluid extract is respectively compounded by four intermediate extracts of belladonna root, stem, leaf and seed, and the compounding proportion of the four intermediate extracts of the belladonna root, stem, leaf and seed is as follows: the mass of the plant extract is 15-25 parts of root fluid extract, 45-60 parts of stem fluid extract, 10-15 parts of leaf fluid extract and 10-15 parts of seed fluid extract.
2. A bionic compound fluid extract prepared by the preparation method of claim 1 is characterized in that: wherein the content of scopolamine is 0.043-0.051 mg/mL, the content of atropine is 0.022-0.029 mg/mL, and the content of scopoletin is 0.410-0.450 mg/mL; the content of the total alkaloids is 7.6-8.1 mg/mL calculated by henbane.
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|---|---|---|---|---|
| CN113274436A (en) * | 2021-04-06 | 2021-08-20 | 福建力传生物有限公司 | Belladonna extract preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104013729A (en) * | 2014-06-20 | 2014-09-03 | 安徽安科余良卿药业有限公司 | Arthralgia relieving gel and preparation method thereof |
| CN104840603A (en) * | 2015-05-29 | 2015-08-19 | 重庆希尔安药业有限公司 | Belladonna extract and preparation method thereof |
| CN106620008A (en) * | 2017-01-18 | 2017-05-10 | 石药集团江西金芙蓉药业股份有限公司 | Process for preparing belladonna liquid extract by ultrasonic dynamic multi-stage countercurrent extraction |
-
2020
- 2020-07-22 CN CN202010707813.XA patent/CN111671820A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104013729A (en) * | 2014-06-20 | 2014-09-03 | 安徽安科余良卿药业有限公司 | Arthralgia relieving gel and preparation method thereof |
| CN104840603A (en) * | 2015-05-29 | 2015-08-19 | 重庆希尔安药业有限公司 | Belladonna extract and preparation method thereof |
| CN106620008A (en) * | 2017-01-18 | 2017-05-10 | 石药集团江西金芙蓉药业股份有限公司 | Process for preparing belladonna liquid extract by ultrasonic dynamic multi-stage countercurrent extraction |
Non-Patent Citations (4)
| Title |
|---|
| 中国医学科学院药物研究所编: "《中草药栽培技术》", 30 June 1979, 人民卫生出版社 * |
| 国家药典委员会编: "《中华人民共和国药典：2010年版.1部》", 31 January 2010, 中国医药科技出版社 * |
| 庄果 等: "RP-HPLC法同时测定颠茄草5个部位中2种成分", 《中成药》 * |
| 药学教研组编: "《药剂学》", 31 December 1975, 广西卫生学校 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113274436A (en) * | 2021-04-06 | 2021-08-20 | 福建力传生物有限公司 | Belladonna extract preparation method |
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