CN114377095A - Fructus amomi-sandalwood volatile oil extraction method, capsule for treating gastritis and preparation method of capsule - Google Patents
Fructus amomi-sandalwood volatile oil extraction method, capsule for treating gastritis and preparation method of capsule Download PDFInfo
- Publication number
- CN114377095A CN114377095A CN202210098043.2A CN202210098043A CN114377095A CN 114377095 A CN114377095 A CN 114377095A CN 202210098043 A CN202210098043 A CN 202210098043A CN 114377095 A CN114377095 A CN 114377095A
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- capsule
- mass
- fructus amomi
- sandalwood
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 46
- 238000000605 extraction Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 208000007882 Gastritis Diseases 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 47
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- 238000004821 distillation Methods 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims description 43
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- KGEKLUUHTZCSIP-HOSYDEDBSA-N [(1s,4s,6r)-1,7,7-trimethyl-6-bicyclo[2.2.1]heptanyl] acetate Chemical compound C1C[C@]2(C)[C@H](OC(=O)C)C[C@H]1C2(C)C KGEKLUUHTZCSIP-HOSYDEDBSA-N 0.000 description 7
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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- A61K35/24—Mucus; Mucous glands; Bursa; Synovial fluid; Arthral fluid; Excreta; Spinal fluid
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- A61K36/185—Magnoliopsida (dicotyledons)
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- A61K36/537—Salvia (sage)
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- A61K36/8905—Cyperus (flatsedge)
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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
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Epidemiology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Mycology (AREA)
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- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Biomedical Technology (AREA)
- Immunology (AREA)
- Inorganic Chemistry (AREA)
- Cell Biology (AREA)
- Developmental Biology & Embryology (AREA)
- Neurology (AREA)
- Virology (AREA)
- Zoology (AREA)
- Orthopedic Medicine & Surgery (AREA)
- Pain & Pain Management (AREA)
- Rheumatology (AREA)
- Hospice & Palliative Care (AREA)
- Otolaryngology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Nutrition Science (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for extracting fructus amomi-sandalwood volatile oil, a preparation method and application of a capsule for treating gastritis. The invention adopts distillation method to extract the volatile oil of fructus amomi and sandalwood, avoids the loss of the volatile oil in the direct decoction process by controlling the extraction conditions, and can improve the content of effective components and the proportion of effective substances when the fructus amomi-sandalwood volatile oil obtained by the extraction method is used for preparing the capsule for treating gastritis. The prepared new Jingzhu Weitai capsule is suitable for treating various chronic gastritis (superficial, atrophic and hypertrophic), gastric and duodenal ulcers, stomachache, fullness and distention in chest and abdomen, epigastric pain, vomiting and diarrhea, and deficiency-cold of spleen and stomach. Especially has better curative effect on the chronic atrophic gastritis and the spleen and stomach weakness than the Jingzhu Weitai capsule prepared by the original method.
Description
The application is a divisional application with application date of 2018, 11 and 21, application number of 201811391271.9, and invention name of "a capsule for treating gastritis and a preparation method thereof".
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a method for extracting fructus amomi-sandalwood volatile oil, a Tibetan medicine new medicament for treating various gastritis-Jingzhuweitai capsule and a preparation method thereof.
Background
The Jingzhu Weitai capsule is a medicine for treating various gastritis, and has the effects of strengthening spleen and stomach, promoting qi circulation and relieving pain, promoting repair and regeneration of gastric mucosa epithelium, and promoting ulcer healing; it is suitable for treating chronic gastritis (superficial, atrophic, and hypertrophic), gastric and duodenal ulcer, gastralgia, abdominal distention, gastralgia, vomiting, diarrhea, and deficiency-cold of spleen and stomach.
The existing preparation method of the Jingzhu Weitai capsule comprises the following steps: taking eight traditional Chinese medicinal materials in the prescription, grinding calcite, sandalwood and trogopterus dung into fine powder; pulverizing fructus Chebulae and fructus Amomi into coarse powder; the salvia miltiorrhiza, the prepared rhizoma cyperi and the galangal are cut into decoction pieces. Extracting Saviae Miltiorrhizae radix, rhizoma Cyperi preparata, and Oletum Trogopterori with 70% ethanol for three times, mixing extractive solutions, concentrating into paste, oven drying, and pulverizing. Decocting Mirabilitum crystallina, fructus Chebulae, lignum Santali albi, and fructus Amomi in water for three times, mixing decoctions, concentrating into paste, oven drying, and pulverizing. Mixing the ethanol extract powder, water extract powder and adjuvants, and making into capsule.
This method has drawbacks. Research shows that the fructus amomi volatile oil is the main active ingredient of fructus amomi, such as borneol acetate, linalool, limonene and the like, and can inhibit gastrointestinal motility, gastric acid secretion and pepsin activity. Similarly, the sandalwood volatile oil is the main active ingredient of sandalwood, such as alpha-santalene, santalenone and the like, and animal experiments show that the sandalwood volatile oil can antagonize small intestine movement of mice loaded with neostigmine. However, in the original preparation method, the amomum fruit volatile oil and the sandalwood volatile oil are extracted by a water decoction method, the loss of the volatile oil is great, and the extraction effect is not ideal. Therefore, the volatile oil of fructus amomi and sandalwood is separately extracted and used as a separate component for preparing the Jingzhu Weitai capsule, which can play a greater role in treatment.
In addition, the thick paste is an important intermediate of the traditional Chinese medicine preparation, and the drying process of the thick paste is one of key joints in the traditional Chinese medicine preparation process. The existing method adopts a microwave vacuum drying method to dry the alcohol extract and the water extract thick paste. Although the microwave vacuum drying method has the advantages of convenient operation, high drying speed and the like, the loss of effective components is large, and the exertion of the drug effect is not facilitated. Therefore, there is a need to reduce the loss of active ingredients during drying of alcohol and water extracts using new drying techniques.
Disclosure of Invention
The invention aims to provide a method for extracting amomum fruit-sandalwood volatile oil, a method for preparing a capsule for treating gastritis-Jingzhu stomach-Tai capsule and application thereof.
The preparation method of the Jingzhu Weitai capsule provided by the invention comprises the following steps:
1) the Chinese medicinal materials are treated as follows: grinding Mirabilitum crystallina, lignum Santali albi, and Oletum Trogopterori into fine powder; pulverizing fructus Chebulae and fructus Amomi into coarse powder respectively; cutting Saviae Miltiorrhizae radix, rhizoma Cyperi preparata, and rhizoma Alpiniae Officinarum into pieces;
2) extracting the salvia miltiorrhiza, the prepared rhizoma cyperi, the trogopterus dung and the galangal which are treated in the step 1) with 70 percent ethanol water solution for 3 times, combining the extracting solutions, concentrating into thick paste, and performing spray drying to obtain medicinal powder 1;
3) extracting volatile oil from the fructus amomi and the sandalwood processed in the step 1) by a distillation method, and respectively collecting the volatile oil, the aqueous solution and dregs;
4) decocting the dregs obtained in the step 3) and the myrobalan and the calcite treated in the step 1) with water for three times, combining the decoction and the aqueous solution obtained in the step 3), filtering, concentrating the filtrate into thick paste, and then performing spray drying to obtain medicinal powder 2;
5) primarily mixing the medicinal powder 1 and the medicinal powder 2, spraying the volatile oil obtained in the step 3), uniformly mixing, preparing granules, and filling into capsules.
Preferably, the traditional Chinese medicinal materials comprise the following raw materials in parts by mass: 400 parts of salvia miltiorrhiza bunge, 400 parts of galangal 200 bunge, 250 parts of myrobalan 150 bunge, 250 parts of gypsum rubrum 150 bunge, 250 parts of fructus amomi 150 bunge, 250 parts of prepared rhizoma cyperi 150 bunge, 140 parts of sandalwood 100 bunge and 50-150 parts of trogopterus dung; the preferred composition is: 300 parts of salvia miltiorrhiza, 300 parts of galangal, 180 parts of myrobalan, 200 parts of calcite, 200 parts of fructus amomi, 200 parts of prepared rhizoma cyperi, 120 parts of sandalwood and 100 parts of trogopterus dung.
The raw material medicines for preparing the capsule are proportioned according to parts by mass, and can be increased or decreased according to corresponding proportions during production, for example, the mass production can be in units of kilograms or tons, the small-scale production can also be in units of grams, the weight can be increased or decreased, but the mass proportioning proportion of the raw material medicines among the components is unchanged.
Preferably, in step 2), the extraction conditions are as follows: the mass of the ethanol water solution added in the first extraction is 6 times of the mass of the medicinal materials, and the extraction is carried out for 4 hours; the mass of the ethanol water solution added in the second extraction is 4 times of the mass of the medicinal materials, and the extraction is carried out for 3 hours; the mass of the ethanol water solution added in the third extraction is 4 times of the mass of the medicinal materials, and the extraction lasts 2 hours.
Preferably, in the step 2), the concentrating into the paste is specifically a thick paste obtained by concentrating the extracting solution to a relative density of 1.30-1.35 (50 ℃).
Preferably, in the step 3), the conditions for extracting the volatile oil by distillation are as follows: adding water in an amount of 90-100 times of the total mass of fructus Amomi and lignum Santali albi, soaking for 20-40 min, and distilling for 8-10 hr.
Preferably, the conditions for extracting the volatile oil by distillation are as follows: adding water 90 times of the medicinal materials, soaking for 30 min, and distilling for 8 hr.
Preferably, in step 4), the water-adding decoction conditions are as follows: the water adding amount of the three times of decoction is 7 times, 6 times and 5 times of the mass of the medicine residues, the myrobalan and the gypsum rubrum in sequence; the time for three times of decoction is 3 hours, 2 hours and 2 hours in sequence.
Preferably, in the step 4), the thick paste is thick paste with the relative density of 1.30-1.35 (50 ℃).
Preferably, in step 2) and step 4), the spray drying conditions are as follows: the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5 KPa.
The capsule for treating gastritis prepared by the method also belongs to the protection scope of the invention.
The invention improves the preparation process of the existing prescription, improves the content of effective components and improves the proportion of effective substances. The distillation method is adopted to extract the volatile oil of the amomum villosum and the sandalwood, and the volatile oil is used as a single component to be added into the medicinal powder, so that the loss of the volatile oil in the direct decoction process is avoided. Pharmacodynamic tests prove that the novel Jingzhu Weitai capsule prepared by the method is also suitable for treating various chronic gastritis (superficial, atrophic and hypertrophic), gastric and duodenal ulcers, stomachache, fullness and distention in chest and abdomen, epigastric pain, vomiting and diarrhea and deficiency-cold in spleen and stomach. Especially has better curative effect on the chronic atrophic gastritis and the spleen and stomach weakness than the Jingzhu Weitai capsule prepared by the original method.
Detailed Description
The present invention will be described below with reference to specific examples, but the present invention is not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The salvia miltiorrhiza, galangal, myrobalan, calcite, fructus amomi, prepared rhizoma cyperi, sandalwood and trogopterus dung used in the following examples all accord with the related regulations under the terms of each medicinal material in the part of Chinese pharmacopoeia (2015 edition). Before feeding, the material objects are identified to be consistent with the names of the medicinal materials, and the quality is in accordance with the standard.
In the following examples, the method for measuring the content of tanshinone IIA is high performance liquid chromatography, and the method for measuring the content of galangin is high performance liquid chromatography.
Example 1 examination of the Effect of different steam distillation conditions on active ingredients
The prescription composition is as follows:
300.0g of salvia miltiorrhiza, 300.0g of galangal, 180.0g of myrobalan, 200.0g of calcite, 200.0g of amomum villosum,
200.0g of prepared rhizoma cyperi, 120.0g of sandalwood and 100.0g of trogopterus dung.
The preparation method comprises the following steps:
1) the Chinese medicinal materials are treated as follows: grinding Mirabilitum crystallina, lignum Santali albi, and Oletum Trogopterori into fine powder; respectively pulverizing the myrobalan and the fructus amomi into coarse powder for later use; cutting the salvia miltiorrhiza, the prepared rhizoma cyperi and the galangal into decoction pieces for later use;
2) extracting the salvia miltiorrhiza, the prepared rhizoma cyperi, the trogopterus dung and the galangal which are treated in the step 1) with 70 percent ethanol water solution for 3 times (6 times of volume of ethanol is added for extraction for 4 hours for the first time, 4 times of volume of ethanol is added for extraction for 3 hours for the second time, and 4 times of volume of ethanol is added for extraction for 2 hours for the third time), combining the extracting solutions, concentrating the extracting solutions to thick paste with the relative density of 1.30-1.35 (50 ℃), and performing spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5kPa) to obtain medicinal powder 1;
3) extracting volatile oil from the fructus amomi and the sandalwood processed in the step 1) by adopting a steam distillation method, collecting the volatile oil and dregs of a decoction, and collecting the aqueous solution in another container;
4) decocting the medicine residues and the myrobalan and the gypsum rubrum treated in the step 1) with water for three times (the water adding amount is 7 times, 6 times and 5 times of the mass of the medicinal materials in sequence, and the time for the three times of decoction is 3 hours, 2 hours and 2 hours in sequence), combining decoction and the aqueous solution obtained in the step 3), filtering, concentrating the filtrate into thick paste with the relative density of 1.30-1.35 (50 ℃), and performing spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5kPa) to obtain medicine powder 2;
5) primarily mixing the medicinal powder 1 and the medicinal powder 2, spraying the volatile oil obtained in the step 3), uniformly mixing, preparing granules, and filling into capsules.
The examination conditions of the steam distillation in the step 3) are as follows: adding water in an amount which is 30 times of the amount of the medicinal materials, soaking for 30 minutes, and distilling for 4 hours; ② adding water which is 60 times of the amount of the medicinal materials, soaking for 30 minutes, and distilling for 4 hours; thirdly, the water adding amount is 90 times of the amount of the medicinal materials, the soaking time is 30 minutes, and the distillation time is 4 hours; fourthly, the water adding amount is 90 times of the amount of the medicinal materials, the soaking time is 60 minutes, and the distillation time is 4 hours; adding water in an amount which is 90 times of the amount of the medicinal materials, soaking for 120 minutes, and distilling for 4 hours; sixthly, adding water which is 90 times of the amount of the medicinal materials, soaking for 30 minutes, and distilling for 8 hours; the water adding amount is 90 times of the amount of the medicinal materials, the soaking time is 30 minutes, and the distillation time is 12 hours. The yield of the volatile oil of fructus Amomi and lignum Santali albi under the above conditions is shown in Table 1.
TABLE 1 yield of bornyl acetate in capsule form of Jingzhu Weitai under different distillation conditions
| Cooking conditions | Yield of fructus Amomi volatile oil | Sandalwood volatile oil yield |
| Adding water 30 times, soaking for 30 min, and distilling for 4 hr | 1.095％ | 2.419％ |
| ② adding 60 times of water, soaking for 30 min, distilling for 4 h | 1.762％ | 2.633％ |
| ③ adding 90 times of water, soaking for 30 minutes, distilling for 4 hours | 2.353％ | 2.548％ |
| Adding water in an amount which is 90 times that of the raw materials, soaking for 60 minutes, and distilling for 4 hours | 2.583％ | 2.564％ |
| Adding 90 times of water, soaking for 120 min, and distilling for 4 hr | 2.842％ | 3.436％ |
| Sixthly, adding water 90 times, soaking for 30 minutes, distilling for 8 hours | 3.465％ | 4.691％ |
| Seventhly, adding 90 times of water, soaking for 30 minutes, and distilling for 12 hours | 3.061％ | 4.834％ |
As can be seen from Table 1, under the condition of (c), the yield of the fructus amomi volatile oil reaches the highest. Although this condition is not the highest yield for sandalwood volatile oil, it is more feasible to produce 8 hours of distillation and with lower energy consumption than 12 hours, so the optimal distillation conditions for volatile oil are finally determined as follows: the water addition amount is 90 times of the amount of the medicinal materials, the soaking time is 30 minutes, and the distillation time is 8 hours.
Example 2 examination of the Effect of different spray drying conditions on active ingredients
The formulation is the same as in example 1.
The preparation method comprises the following steps:
1) the Chinese medicinal materials are treated as follows: grinding Mirabilitum crystallina, lignum Santali albi, and Oletum Trogopterori into fine powder; respectively pulverizing the myrobalan and the fructus amomi into coarse powder for later use; cutting the salvia miltiorrhiza, the prepared rhizoma cyperi and the galangal into decoction pieces for later use;
2) extracting the salvia miltiorrhiza, the prepared rhizoma cyperi, the trogopterus dung and the galangal which are treated in the step 1) for 3 times by using ethanol water solution with the volume fraction of 70% (adding 6 times of ethanol for extracting for 4 hours for the first time, adding 4 times of ethanol for extracting for 3 hours for the second time and adding 4 times of ethanol for extracting for 2 hours for the third time), combining the extracting solutions, concentrating the extracting solutions to thick paste with the relative density of 1.30-1.35 (50 ℃), and performing spray drying to obtain medicinal powder 1;
3) extracting volatile oil from the fructus amomi and the sandalwood processed in the step 1) by adopting a distillation method (the water adding amount is 90 times of the total mass of the fructus amomi and the sandalwood, adding water, soaking for 30 minutes, distilling for 8 hours), collecting the volatile oil and dregs, and collecting the aqueous solution in another container;
4) decocting the medicine residues and the myrobalan and the gypsum rubrum processed in the step 1) with water for three times (the water adding amount is 7 times, 6 times and 5 times of the mass of the medicinal materials in sequence, and the time for the three times of decoction is 3 hours, 2 hours and 2 hours in sequence), combining decoction and the aqueous solution obtained in the step 3), filtering, concentrating the filtrate into thick paste with the relative density of 1.30-1.35 (50 ℃), and performing spray drying to obtain medicine powder 2;
5) primarily mixing the medicinal powder 1 and the medicinal powder 2, spraying the volatile oil obtained in the step 3), uniformly mixing, preparing granules, and filling into capsules.
The spray drying investigation conditions in step 2) and step 4) are as follows: the relative density of the thick paste is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.0 kPa; ② the relative density of the thick paste is 1.40, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.0 kPa; thirdly, the relative density of the thick paste is 1.50, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.0 kPa; fourthly, the relative density of the thick paste is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 75 ℃, and the air inlet pressure is 16.0 kPa; fifthly, the relative density of the thick paste is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 80 ℃, and the air inlet pressure is 16.0 kPa; sixthly, the relative density of the thick paste is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the pressure of an air inlet is 16.5 kPa; the relative density of the thick paste is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 17.0 kPa. The tanshinone IIA content corresponding to the above conditions is shown in Table 2, wherein the tanshinone IIA content refers to the tanshinone IIA content measured by high performance liquid chromatography when the alcohol extract soft extract in the step 2) is condensed to a relative density of 1.30-1.35 (50 ℃).
TABLE 2 Tanshinone IIA content of the soft extract of JINGZHUWEITAI Capsule under different spray drying conditions
Tanshinone IIA is a heat-sensitive substance and is relatively easy to decompose at high temperature, so that the spray drying process condition needs to be optimized. As shown in Table 2, when the relative density of the alcohol extract soft extract is 1.30, the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃ and the air inlet pressure is 16.5kPa, the tanshinone IIA content is higher than that of other process conditions.
Example 3 comparison of the effects of spray drying and microwave vacuum drying on the content of active ingredients in an alcohol extract of Jingzhu Weitai Capsule
The contents of tanshinone IIA and galangin in the soft extract of JINGZHUWEITAI capsule dried by the above method are shown in Table 3. The results show that the spray drying method is superior to the microwave vacuum drying method. Wherein the relative density of the ethanol extract soft extract is 1.30(50 deg.C). Other process conditions of the spray drying method are as follows: the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃ and the air inlet pressure is 16.5 kPa; other process conditions of the microwave vacuum drying method are as follows: the medium-low fire power is intermittently heated (the heating is stopped for 1 minute after 1 minute) in the first 15 minutes, and then the heating is continuously carried out, the temperature is controlled to be 24-39 ℃, and the vacuum degree is-0.084 MPa.
TABLE 3 content of effective components of ethanol extract of JINGZHUWEITAI Capsule by different drying methods
| Active ingredient | Spray drying method (mg/g) | Vacuum drying method of microblog (mg/g) |
| Tanshinone IIA | 1.785±0.158 | 1.291±0.047 |
| Galangin | 2.117±0.131 | 1.436±0.187 |
In this experiment, different drying methods were not used for the aqueous extract thick paste. In comparison, the salvia miltiorrhiza has the efficacies of activating blood and removing stasis, and stimulating the menstrual flow and relieving pain; rhizoma galangae has the effects of warming stomach, dispelling cold, promoting qi circulation and relieving pain, and has a key effect on relieving epigastric cold pain, so the two medicinal materials are selected to compare the change of index component contents.
Example 4 preparation of Jingzhu Weitai Capsule under optimal Process conditions
The prescription composition is as follows:
300.0g of salvia miltiorrhiza, 300.0g of galangal, 180.0g of myrobalan, 200.0g of calcite, 200.0g of amomum villosum,
200.0g of prepared rhizoma cyperi, 120.0g of sandalwood and 100.0g of trogopterus dung.
The preparation method comprises the following steps:
1) the Chinese medicinal materials are treated as follows: grinding Mirabilitum crystallina, lignum Santali albi, and Oletum Trogopterori into fine powder; respectively pulverizing the myrobalan and the fructus amomi into coarse powder for later use; cutting the salvia miltiorrhiza, the prepared rhizoma cyperi and the galangal into decoction pieces for later use;
2) extracting the salvia miltiorrhiza, the prepared rhizoma cyperi, the trogopterus dung and the galangal which are treated in the step 1) with 70 percent ethanol water solution for 3 times (adding 6 times of ethanol with volume for extracting for 4 hours for the first time, adding 4 times of ethanol with volume for extracting for 3 hours for the second time and adding 4 times of ethanol with volume for extracting for 2 hours for the third time), combining the extracting solutions, concentrating the extracting solutions to thick paste with the relative density of 1.30(50 ℃), and performing spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5kPa) to obtain medicinal powder 1;
3) extracting volatile oil from the fructus amomi and the sandalwood processed in the step 1) by adopting a distillation method (the water adding amount is 90 times of the total mass of the fructus amomi and the sandalwood, adding water, soaking for 30 minutes, distilling for 8 hours), collecting the volatile oil and dregs, and collecting the aqueous solution in another container;
4) decocting the medicine residues and the myrobalan and the gypsum rubrum treated in the step 1) with water for three times (the water adding amount is 7 times, 6 times and 5 times of the mass of the medicinal materials in sequence, and the time for the three times of decoction is 3 hours, 2 hours and 2 hours in sequence), combining decoction and the aqueous solution obtained in the step 3), filtering, concentrating the filtrate into thick paste with the relative density of 1.30-1.35 (50 ℃), and performing spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5kPa) to obtain medicine powder 2;
5) primarily mixing the medicinal powder 1 and the medicinal powder 2, spraying the volatile oil obtained in the step 3), uniformly mixing, preparing granules, and filling into capsules.
Comparative example (c),
The formulation is the same as in example 1.
Taking eight traditional Chinese medicinal materials in the prescription, grinding calcite, sandalwood and trogopterus dung into fine powder; pulverizing fructus Chebulae and fructus Amomi into coarse powder; the salvia miltiorrhiza, the prepared rhizoma cyperi and the galangal are cut into decoction pieces. Extracting Saviae Miltiorrhizae radix, rhizoma Cyperi preparata, and Oletum Trogopterori with 70% ethanol for three times (6 times of ethanol for 4 hr, 4 times of ethanol for 3 hr, and 4 times of ethanol for 2 hr), mixing extractive solutions, concentrating into paste, oven drying, and pulverizing. Decocting Mirabilitum crystallina, fructus Chebulae, lignum Santali albi, and fructus Amomi with water for three times (the amount of water is 7 times, 6 times, and 5 times of the medicinal materials in sequence, and the time for decocting for 3 hr, 2 hr, and 2 hr), mixing decoctions, concentrating into paste, oven drying, and pulverizing. Mixing the ethanol extract powder, water extract powder and adjuvants, and making into 250 capsules.
Example 5 test of drug efficacy
The difference between the content of the active ingredient and the clinical efficacy of 5 batches of the capsule prepared by the method of example 3 of the present invention and the method of comparative example was evaluated.
1. Comparison of active ingredient contents tanshinone IIA in Salvia miltiorrhiza, galangin in Alpinia officinarum, and bornyl acetate in fructus Amomi volatile oil were used as evaluation indexes, and elution amounts of the active ingredients were measured by high performance liquid chromatography, and the results are shown in Table 4.
TABLE 4 comparison of active ingredients of Jingzhu Weitai Capsule by different preparation methods
As can be seen from table 4, the dissolution amounts of the active ingredients tanshinone ia, galangin and bornyl acetate in the Jingzhuweitai capsule using the preparation method of the present invention are higher than those of the original preparation method, and the differences have statistical significance.
2. Clinical effects
Chronic atrophic gastritis is a common digestive system disease in clinic, and has high incidence rate, long course of disease, low cure rate and high possibility of canceration. Omeprazole, ranitidine and other medicaments are commonly used for clinical treatment, but the effect is not as expected. Chronic atrophic gastritis belongs to the category of epigastric pain in traditional Chinese medicine, and is seen in many cases in the clinical syndrome differentiation of weakness of the spleen and stomach and congealing cold and qi stagnation. The Jingzhuchangweitai capsule is used in Beijing Gaizhu Chinese medicine hospital for long term to treat chronic atrophic gastritis with spleen and stomach weakness and cold congealing and qi stagnation. The observation compares the curative effect difference of the Jingzhu Weitai capsule prepared by the preparation method of the invention and the Jingzhu Weitai capsule prepared by the original preparation method on the chronic atrophic gastritis with spleen and stomach weakness and cold congealing and qi stagnation.
Therefore, 96 patients with chronic atrophic gastritis who accord with syndrome differentiation are included in the group, and the patients are randomly divided into 48 patients in the A group and the B group, wherein the A group of patients receive the Jingzhuchetai capsule prepared by the method for treating the chronic atrophic gastritis, and the B group of patients receive the Jingzhuchetai capsule prepared by the original method for treating the chronic atrophic gastritis. The two groups are orally administered 3 granules at a time, 3 times a day, with a minimum dosage of 1 month and a maximum dosage of 3 months.
The therapeutic effect criteria are classified into significant effect (disappearance of symptoms such as stomachache after treatment, and normal gastroscopy), significant effect (reduction and alleviation of stomachache frequency after treatment, improvement of other symptoms, and improvement of gastroscopy) and ineffective effect (no improvement or aggravation of clinical symptoms after treatment). The score of symptoms was divided into 0 (no symptoms), 1 (mild symptoms), 2 (moderate symptoms), 3 (severe symptoms) and 4 (severe symptoms).
The clinical efficacy of the two groups is shown in Table 5, and the score of symptoms after treatment is shown in Table 6.
TABLE 5A, B comparison of clinical efficacy of two groups of patients
As shown in Table 5, the total effective rate of the capsule for treating chronic atrophic gastritis with spleen and stomach weakness and cold-coagulation qi stagnation is 87.5%, which is significantly higher than that of the capsule prepared by the original method (77.1%, P < 0.05%).
TABLE 6A, B comparison of symptom scores of two groups of patients after treatment
As shown in Table 6, the weight percentages of dysplasia, gland atrophy and chronic inflammation of patients with chronic atrophic gastritis, weakness of spleen and stomach and cold-coagulation and qi-stagnation syndrome by using the Jingzhu Weitai capsule prepared by the method of the invention are all lower than that of the Jingzhu Weitai capsule prepared by the original method (P is less than 0.05).
In conclusion, the Jingzhu Weitai capsule prepared by the method has obvious clinical curative effect on treating the chronic atrophic gastritis with spleen and stomach weakness and cold congealing and qi stagnation, and can effectively improve the clinical symptoms of patients.
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and the embodiments are within the scope of the present invention.
Claims (10)
1. A method for extracting fructus amomi-sandalwood volatile oil is characterized by comprising the following steps:
grinding lignum Santali albi into fine powder; pulverizing fructus Amomi into coarse powder;
extracting volatile oil from lignum Santali albi fine powder and lignum Santali albi coarse powder by distillation, and collecting volatile oil, aqueous solution and residue respectively;
the conditions for extracting the volatile oil by the distillation method are as follows: adding water in an amount of 90-100 times of the total mass of fructus Amomi and lignum Santali albi, soaking for 20-40 min, and distilling for 8-10 hr;
the mass part of the fructus amomi is 150-250 parts; the mass portion of the sandalwood is 100-140 portions.
2. The extraction method according to claim 1, wherein the conditions for extracting the volatile oil by the distillation method are as follows: adding water in an amount which is 90 times of the total mass of the fructus amomi and the sandalwood, soaking for 30 minutes after adding water, and distilling for 8 hours.
3. A preparation method of a capsule for treating gastritis comprises the following steps:
1) the Chinese medicinal materials are treated as follows: grinding Mirabilitum crystallina and Oletum Trogopterori into fine powder; pulverizing fructus Chebulae into coarse powder; cutting Saviae Miltiorrhizae radix, rhizoma Cyperi preparata, and rhizoma Alpiniae Officinarum into pieces;
2) extracting the salvia miltiorrhiza, the prepared rhizoma cyperi, the trogopterus dung and the galangal which are treated in the step 1) with 70 percent ethanol water solution for 3 times, combining the extracting solutions, concentrating into paste, and performing spray drying to obtain medicinal powder 1;
3) processing lignum Santali albi and fructus Amomi by the extraction method of claim 1 or 2, and collecting volatile oil, aqueous solution and residue respectively;
4) decocting the dregs obtained in the step 3) and the myrobalan and the calcite treated in the step 1) with water for three times, combining decoction and the aqueous solution obtained in the step 3), filtering, concentrating the filtrate into thick paste, and performing spray drying to obtain medicinal powder 2;
5) primarily mixing the medicinal powder 1 and the medicinal powder 2, spraying the volatile oil obtained in the step 3), uniformly mixing, preparing granules, and encapsulating to obtain the capsule for treating gastritis;
the traditional Chinese medicine comprises the following raw materials in parts by mass: 400 portions of salvia miltiorrhiza bunge, 400 portions of galangal 200 bunge, 250 portions of myrobalan 150 bunge, 250 portions of gypsum rubrum 150 bunge, 250 portions of amomum villosum 150 bunge, 250 portions of prepared nutgrass galingale rhizome 150 bunge, 140 portions of sandalwood 100 bunge and 50-150 portions of trogopterus dung.
4. The production method according to claim 3, characterized in that: in the step 2), the extraction conditions are as follows: the mass of the ethanol water solution added in the first extraction is 6 times of the mass of the medicinal materials, and the extraction is carried out for 4 hours; the mass of the ethanol water solution added in the second extraction is 4 times of the mass of the medicinal materials, and the extraction is carried out for 3 hours; the mass of the ethanol water solution added in the third extraction is 4 times of the mass of the medicinal materials, and the extraction lasts 2 hours.
5. The production method according to claim 3, characterized in that: in the step 2), the concentration to obtain the paste is to specifically concentrate the extracting solution to obtain the thick paste with the relative density of 1.30-1.35.
6. The production method according to any one of claims 3 to 5, characterized in that: in the step 4), the water decocting conditions are as follows: the water adding amount of the three times of decoction is 7 times, 6 times and 5 times of the mass of the medicine residues, the myrobalan and the gypsum rubrum in sequence; the time for three times of decoction is 3 hours, 2 hours and 2 hours in sequence.
7. The production method according to any one of claims 3 to 5, characterized in that: in the step 4), the thick paste is thick paste with the relative density of 1.30-1.35.
8. The production method according to claim 3, characterized in that: in the step 2) and the step 4), the spray drying conditions are as follows: the air inlet temperature is 130 ℃, the air outlet temperature is 70 ℃, and the air inlet pressure is 16.5 KPa.
9. The production method according to claim 3, characterized in that: the traditional Chinese medicine comprises the following raw materials in parts by mass: 300 parts of salvia miltiorrhiza, 300 parts of galangal, 180 parts of myrobalan, 200 parts of calcite, 200 parts of fructus amomi, 200 parts of prepared rhizoma cyperi, 120 parts of sandalwood and 100 parts of trogopterus dung.
10. A capsule for treating gastritis prepared by the preparation method of any one of claims 2 to 9.
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| CN115336509B (en) * | 2022-10-19 | 2023-01-31 | 云南省农业科学院园艺作物研究所 | Cultivation method for improving fructus amomi volatile oil at medium-low altitude |
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| CN1323609A (en) * | 2001-01-11 | 2001-11-28 | 李方瑞 | Weitai capsule for treating stomach disease |
| CN101766780A (en) * | 2008-12-31 | 2010-07-07 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Sandalwood-containing traditional Chinese medicine for treating gastrointestinal diseases and preparation method thereof |
| CN107019775A (en) * | 2016-01-31 | 2017-08-08 | 广州中医药大学 | A kind of Chinese medicine composition for treating coronary heart disease |
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| JP2003048844A (en) * | 2001-08-03 | 2003-02-21 | Yakult Honsha Co Ltd | Urease activity inhibitor |
| CN106692853A (en) * | 2015-11-18 | 2017-05-24 | 泸州医学院附属中医医院 | Preparation method of salvia miltiorrhiza extract |
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| CN1323609A (en) * | 2001-01-11 | 2001-11-28 | 李方瑞 | Weitai capsule for treating stomach disease |
| CN101766780A (en) * | 2008-12-31 | 2010-07-07 | 天津中新药业集团股份有限公司乐仁堂制药厂 | Sandalwood-containing traditional Chinese medicine for treating gastrointestinal diseases and preparation method thereof |
| CN107019775A (en) * | 2016-01-31 | 2017-08-08 | 广州中医药大学 | A kind of Chinese medicine composition for treating coronary heart disease |
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