CN111228427A - Granular preparation for treating chronic pelvic inflammatory disease and application thereof - Google Patents

Granular preparation for treating chronic pelvic inflammatory disease and application thereof Download PDF

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Publication number
CN111228427A
CN111228427A CN201911385636.1A CN201911385636A CN111228427A CN 111228427 A CN111228427 A CN 111228427A CN 201911385636 A CN201911385636 A CN 201911385636A CN 111228427 A CN111228427 A CN 111228427A
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ethanol
extracting
dandelion
selfheal
rhizoma
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林凡儒
徐步玺
胡百忠
周龙霞
田凤峰
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Xiangyu Pharmaceutical Co ltd
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Xiangyu Pharmaceutical Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/90Smilacaceae (Catbrier family), e.g. greenbrier or sarsaparilla
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/23Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/236Ligusticum (licorice-root)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
    • A61K36/288Taraxacum (dandelion)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/46Eucommiaceae (Eucommia family), e.g. hardy rubber tree
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/536Prunella or Brunella (selfheal)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A61K36/537Salvia (sage)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/68Plantaginaceae (Plantain Family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/894Dioscoreaceae (Yam family)
    • A61K36/8945Dioscorea, e.g. yam, Chinese yam or water yam
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1605Excipients; Inactive ingredients
    • A61K9/1617Organic compounds, e.g. phospholipids, fats
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P15/00Drugs for genital or sexual disorders; Contraceptives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction 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, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying

Abstract

The invention belongs to the technical field of medicine preparation, and relates to a granular preparation for treating chronic pelvic inflammatory disease, which comprises the following raw material medicines: rhizoma smilacis glabrae, salvia miltiorrhiza, selfheal, dandelion, plantain seed, rhizoma dioscoreae hypoglaucae, eucommia ulmoides and ligusticum wallichii. Compared with the prior art, the invention reduces the cost.

Description

Granular preparation for treating chronic pelvic inflammatory disease and application thereof
Technical Field
The invention belongs to the technical field of medicine preparation, and particularly relates to a granular preparation for treating chronic pelvic inflammatory disease and application thereof.
Background
Pelvic inflammation refers to inflammation of female pelvic reproductive organs, connective tissue around uterus, and pelvic peritoneum. The main causes are infection after delivery or abortion, infection after operation in uterine cavity, bad hygiene in menstrual period, direct spread of inflammation of adjacent organs, acute attack of chronic pelvic inflammatory disease, etc. It is divided into hydrosalpinx, ovarian cyst of fallopian tube, salpingitis and chronic pelvic connective tissue inflammation. The clinical manifestations of pelvic inflammation include acute and chronic, the symptoms of acute pelvic inflammation are lower abdominal pain, fever, vaginal secretion increase, abdominal pain is persistent, the disease becomes worse after activity or sexual intercourse, severe cases can include chill, high fever, headache and inappetence, further development of acute pelvic inflammation can cause diffuse peritonitis, septicemia and septic shock, and severe cases can endanger life. The symptoms of chronic pelvic inflammation are lower abdomen tenesmus and swelling, pain and lumbosacral aching pain, which are aggravated after fatigue, copulation and before and after menstruation, and neurasthenia symptoms such as lassitude, discomfort of the whole body, insomnia and the like can appear during the course of disease.
The bailing pelvic inflammation rehabilitation granules are independently researched and developed by an applicant, have pharmaceutical preparations with batch numbers, and have achieved huge achievements from the market, so the applicant also applies patent technologies about the bailing pelvic inflammation rehabilitation granules, for example, "2006101525479, a medicine for treating chronic pelvic inflammation and a preparation method thereof" protects the bailing pelvic inflammation rehabilitation granules sold on the market, and the prescription comprises 1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae septemlobae, 333.4g of eucommia bark, 133.4g of pseudo-ginseng and 200g of szechuan lovage rhizome; the later patent '2015103361326', a medicinal preparation for treating pelvic inflammatory disease and its detection method 'are improved on the basis of known granules, including 40 parts of dandelion, 35 parts of glabrous greenbrier rhizome, 35 parts of perfoliate knotweed herb, 35 parts of kudzuvine root, 30 parts of lily, 30 parts of nutgrass galingale rhizome, 30 parts of red paeony root, 25 parts of dahurian patrinia herb, 25 parts of amur corktree bark, 25 parts of dragon's blood, 25 parts of cassia bark, 20 parts of common burreed rhizome, 20 parts of cattail pollen, 20 parts of bitter orange, 17 parts of myrrh, 17 parts of platycodon grandiflorum, 15 parts of dahurian angelica root, 10 parts of madder, 10 parts of poria cocos, 10 parts of weeping forsythia, 10 parts of sessile stemona root and 5 parts of honeysuckle flower, and the effects are; on the basis of the research results, the applicant improves the process of the known formula, and submits the invention patent application of 'preparation process of the Pu ling pelvic inflammation rehabilitation granules', which carries out different treatments aiming at different medicines, so that the medicine effect is greatly improved, and the waste of raw materials is avoided.
Disclosure of Invention
On the basis of the prior art, the invention deletes part of raw materials in the prescription, and provides a granular preparation for treating chronic pelvic inflammatory disease and application thereof.
The invention is realized by the following technical scheme:
a granular preparation for treating chronic pelvic inflammatory disease is prepared from the following raw materials:
rhizoma smilacis glabrae, salvia miltiorrhiza, selfheal, dandelion, plantain seed, rhizoma dioscoreae hypoglaucae, eucommia ulmoides and ligusticum wallichii.
Specifically, the compound is prepared from the following raw materials:
1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark and 200g of szechuan lovage rhizome.
Further, the preparation method comprises the following steps:
step 1) weighing raw materials, step 2) percolating with ethanol to extract salvia miltiorrhiza, step 3) extracting ligusticum wallichii, eucommia ulmoides and semen chebulae with ethanol, step 4) extracting rhizoma smilacis glabrae and dandelion with microwave ethanol, step 5) extracting rhizoma dioscoreae hypoglaucae and selfheal with ethanol by ultrasound, and step 6) extracting with water, concentrating, drying and preparing into capsules.
Further, the step 1) of weighing the raw material medicines comprises the following steps: 1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark and 200g of szechuan lovage rhizome.
Further, the step 2) of ethanol percolation extraction of salvia miltiorrhiza comprises the following steps: pulverizing Saviae Miltiorrhizae radix into 200 mesh powder, soaking in 1.5 times of 90% (v/v) ethanol for 24 hr, percolating with 90% (v/v) ethanol solution at a percolating speed of 1-3ml/min, collecting percolate, recovering ethanol from percolate to obtain medicinal liquid, and collecting medicinal residue.
Further, the step 3) of extracting the ligusticum wallichii, the eucommia ulmoides and the semen chebulae by alcohol comprises the following steps: mixing rhizoma Ligustici Chuanxiong, Eucommiae cortex and semen plantaginis, pulverizing into 200 mesh powder, adding 70% (v/v) ethanol 5 times the weight of the crude drug each time, soaking for 24 hr, soaking at room temperature for 3 times, mixing the soaking solutions, recovering ethanol, and collecting the medicinal liquid and residue.
Further, the microwave alcohol extraction of the glabrous greenbrier rhizome and the dandelion in the step 4) comprises the following steps: pulverizing rhizoma Smilacis Glabrae and herba Taraxaci, sieving with 200 mesh sieve, placing in a container, adding 85% (v/v) ethanol twice the weight of the powder, stirring and extracting at 300rpm, controlling microwave power at 500W during extraction process, and extracting for 120 min; then placing at 4 ℃ for 12h, filtering and collecting filtrate, and filtering residues for later use.
Further, the step 5) of ultrasonically extracting the yam rhizome and the selfheal, which comprises the following steps: pulverizing rhizoma Dioscoreae Septemlobae and Prunellae Spica, sieving with 200 mesh sieve, placing into ultrasonic extraction tank, adding 75% (v/v) ethanol with weight of three times of the powder, extracting at 50 deg.C and frequency of 50KHz for 30min, filtering, and collecting filtrate.
Further, step 6) water extraction, concentration, drying and capsule preparation, comprising the following steps: mixing the residues obtained in the step 2), the step 3) and the step 4), adding 10 times of water by weight, decocting for 3 times, each time for 1 hour, mixing the decoctions, filtering, adding the liquid medicine obtained in the step 2), the liquid medicine obtained in the step 3), the filtrate obtained in the step 4) and the filtrate obtained in the step 5), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with the density of 1.20g/ml, spray-drying to obtain a dry extract, crushing, adding silicon dioxide according to the mass ratio of 20:1, granulating with ethanol, drying, and encapsulating to obtain the capsule.
The invention also claims the application of the granular preparation in treating chronic pelvic inflammatory disease.
The identification and the source of the medicinal materials of the invention are as follows:
(1) rhizoma Smilacis Glabrae was purchased from Maifanitum, Pingyi county, Ryankang, Guangdong, province. Is identified as dried rhizome of Smilax glabra Roxb. of Liliaceae by Shandong Xiangyu health pharmaceutical Co. Removing impurities from the medicinal materials.
(2) The Saviae Miltiorrhizae radix is obtained from Maitake, Shandong, of Pingyi county, Ryangkang decoction pieces, Ltd. It is identified as dried root and rhizome of Salvia Miltiorrhiza Bge of Labiatae by Shandong Xiangyu health pharmaceutical Co. Removing impurities from the medicinal materials.
(3) Prunella vulgaris was purchased from Bozhou Fengyan pharmaceutical industry, Inc., Henan of origin. The dried cluster is identified as the dried cluster of Prunella vulgaris L. of Labiatae by Shandong Xiangyu health pharmaceutical Co. Removing impurities from the medicinal materials, and cutting into segments.
(4) The herba Taraxaci is obtained from Maitake of Pingyi county, Shandong, China. Is identified as dry whole herb of Taraxacum mongolicum hand-Mazz of Compositae by Shandong Xiangyu health pharmacy Co. Removing impurities from the medicinal materials, and cutting into segments.
(5) Semen plantaginis is purchased from Maitake-Kung-Shen-Yi-county, Shangjiang province. Is identified as dry mature seed of plantago asiatica L. by Shandong Xiangyu health pharmaceutical Co. Removing impurities from the medicinal materials.
(6) Rhizoma Dioscoreae Septemlobae is purchased from Zhejiang province of Yi county Ruikang Chinese medicinal decoction piece Limited. Is identified as the dried rhizome of Dioscorea hyosogtauca Palibin of Dioscoreaceae by Shandong Xiangyu health pharmaceutical Co. Cutting the medicinal materials into slices.
(7) Eucommia ulmoides is purchased from Mai-kang Chinese herbal pieces Limited, Pingyi county, produced in Sichuan. Is identified as dry bark of Eucommia ulmoides Oliv. of Eucommiaceae by Shandong Xiangyu health pharmaceuticals Ltd. Removing impurities from the medicinal materials.
(8) Rhizoma Ligustici Chuanxiong is obtained from Mai kang Chinese medicinal decoction piece GmbH, Pingyi county, produced by Sichuan province. Is identified as dried rhizome of Ligusticum chuanxiong Hort. belonging to the family Umbelliferae by Shandong Xiangyu health pharmaceutical Co. Removing impurities from the medicinal materials.
Compared with the prior art, the starting point and the beneficial effects of the invention mainly comprise the following aspects:
on the basis of the existing research results, the invention researches the components; the price of the pseudo-ginseng is high, the raw material components from different sources have large differences and are often in a state of insufficient supply, the main components of the pseudo-ginseng are saponin and also sanchinin and the like, and the effects mainly comprise the bidirectional regulation effects of promoting blood circulation and stopping bleeding; by combining the two main factors, the research deletes the adjuvant pseudo-ginseng in the formula to form a new formula, accords with the principle of the formula of monarch, minister, adjuvant and guide, reduces the cost of raw materials, has no obvious difference in drug effect, and still needs further research by subsequent tests.
The currently known product of the Puling pelvic inflammation rehabilitation granule is prepared by simply extracting rhizoma smilacis glabrae, dandelion, rhizoma dioscoreae hypoglaucae and selfheal with water, so that water-insoluble flavonoid and saponin substances are lost; flavonoid substances in the dandelion are generally insoluble in water, have broad-spectrum antibacterial, heat-clearing and detoxifying, and disperse stasis and detumescence, while polysaccharide substances are soluble in water and have the functions of antibiosis, antioxidation, antifatigue, immunoregulation and the like; rhizoma smilacis glabrae and dandelion flavone, triterpenes mainly including ursolic acid and oleanolic acid in selfheal, and the dioscorea tokay steroid compound have good antibacterial and anti-inflammatory functions, and the effective components are difficult to obtain by a water extraction method; the preparation process is simple and feasible aiming at the defects of the existing product, different traditional Chinese medicine components are treated by different technologies, the effective components of the raw materials are improved, the drug effect is increased, and the waste of the raw materials is reduced; the raw materials are firstly crushed to prepare powder with the particle size of 200 meshes, the particle size is small, and the cell wall breakage and the leaching of effective components are facilitated; when the glabrous greenbrier rhizome and the dandelion are extracted, phenolic acid and ketone substances are easily decomposed by adopting a decoction mode, and the flavonoid compound cannot be dissolved in water and cannot be effectively extracted; rhizoma Dioscoreae Septemlobae and Prunellae Spica are extracted with ethanol in ultrasonic tank to obtain alcohol-soluble effective components.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the present invention will be described more clearly and completely below with reference to specific embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The granular preparation for treating chronic pelvic inflammatory disease is prepared by the following process:
step 1), weighing raw material medicines: 1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark and 200g of szechuan lovage rhizome.
Step 2) ethanol percolation extraction of salvia miltiorrhiza: pulverizing Saviae Miltiorrhizae radix into 200 mesh powder, soaking in 1.5 times of 90% (v/v) ethanol for 24 hr, percolating with 90% (v/v) ethanol solution at a percolating speed of 1-3ml/min, collecting percolate, recovering ethanol from percolate to obtain medicinal liquid, and collecting medicinal residue;
step 3), alcohol extraction of ligusticum wallichii, eucommia ulmoides and semen chebulae: mixing rhizoma Ligustici Chuanxiong, Eucommiae cortex and semen plantaginis, pulverizing into 200 mesh powder, adding 70% (v/v) ethanol 5 times the weight of the crude drug each time, soaking for 24 hr, soaking at room temperature for 3 times, mixing the soaking solutions, recovering ethanol, and keeping the medicinal liquid and residue;
step 4), microwave alcohol extraction of rhizoma smilacis glabrae and dandelion: pulverizing rhizoma Smilacis Glabrae and herba Taraxaci, sieving with 200 mesh sieve, placing in a container, adding 85% (v/v) ethanol twice the weight of the powder, stirring and extracting at 300rpm, controlling microwave power at 500W during extraction process, and extracting for 120 min; then placing at 4 ℃ for 12h, filtering and collecting filtrate, and keeping filter residues for later use;
step 5), ultrasonically extracting rhizoma dioscoreae hypoglaucae and selfheal to obtain the extract: pulverizing rhizoma Dioscoreae Septemlobae and Prunellae Spica, sieving with 200 mesh sieve, placing into ultrasonic extraction tank, adding 75% (v/v) ethanol with weight of three times of the powder, extracting at 50 deg.C and frequency of 50KHz for 30min, filtering, and collecting filtrate;
step 6), water extraction, concentration, drying and capsule preparation: mixing the residues obtained in the step 2), the step 3) and the step 4), adding 10 times of water by weight, decocting for 3 times, each time for 1 hour, mixing the decoctions, filtering, adding the liquid medicine obtained in the step 2), the liquid medicine obtained in the step 3), the filtrate obtained in the step 4) and the filtrate obtained in the step 5), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with the density of 1.20g/ml at 50 ℃, spray drying to obtain a dry extract, crushing, adding silicon dioxide (20 parts of the dry extract and 1 part of silicon dioxide), granulating with ethanol, drying, and encapsulating to obtain 1000 granules. The filling amount of each grain is 0.45 g.
Comparative example 1
The granular preparation for treating chronic pelvic inflammatory disease is prepared by the following process: :
step 1) weighing raw materials: 1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark, 133.4g of pseudo-ginseng and 200g of szechuan lovage rhizome.
Step 2) ethanol percolation extraction of salvia miltiorrhiza: pulverizing Saviae Miltiorrhizae radix into 200 mesh powder, soaking in 1.5 times of 90% (v/v) ethanol for 24 hr, percolating with 90% (v/v) ethanol solution at a percolating speed of 1-3ml/min, collecting percolate, recovering ethanol from percolate to obtain medicinal liquid, and collecting medicinal residue;
step 3), alcohol extraction of ligusticum wallichii, eucommia ulmoides, pseudo-ginseng and semen chebulae: mixing rhizoma Ligustici Chuanxiong, Eucommiae cortex, Notoginseng radix and semen plantaginis, pulverizing into 200 mesh powder, adding 70% (v/v) ethanol 5 times of the crude drug weight for soaking for 24 hr, soaking at room temperature for 3 times, mixing soaking solutions, recovering ethanol, and keeping the medicinal liquid and residue;
step 4), microwave alcohol extraction of rhizoma smilacis glabrae and dandelion: pulverizing rhizoma Smilacis Glabrae and herba Taraxaci, sieving with 200 mesh sieve, placing in a container, adding 85% (v/v) ethanol twice the weight of the powder, stirring and extracting at 300rpm, controlling microwave power at 500W during extraction process, and extracting for 120 min; then placing at 4 ℃ for 12h, filtering and collecting filtrate, and keeping filter residues for later use;
step 5), ultrasonically extracting rhizoma dioscoreae hypoglaucae and selfheal to obtain the extract: pulverizing rhizoma Dioscoreae Septemlobae and Prunellae Spica, sieving with 200 mesh sieve, placing into ultrasonic extraction tank, adding 75% (v/v) ethanol with weight of three times of the powder, extracting at 50 deg.C and frequency of 50KHz for 30min, filtering, and collecting filtrate;
step 6), water extraction, concentration, drying and capsule preparation: mixing the residues obtained in the step 2), the step 3) and the step 4), adding 10 times of water by weight, decocting for 3 times, each time for 1 hour, mixing the decoctions, filtering, adding the liquid medicine obtained in the step 2), the liquid medicine obtained in the step 3), the filtrate obtained in the step 4) and the filtrate obtained in the step 5), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with the density of 1.20g/ml at 50 ℃, spray drying to obtain a dry extract, crushing, adding silicon dioxide (20 parts of the dry extract and 1 part of silicon dioxide), granulating with ethanol, drying, and encapsulating to obtain 1000 granules. The filling amount of each grain is 0.45 g.
Comparative example 2
The dandelion and poria cocos pelvic inflammation rehabilitation granules comprise the following raw material medicines by weight:
1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark, 133.4g of pseudo-ginseng and 200g of szechuan lovage rhizome.
The preparation method comprises the following steps:
taking the raw materials;
pulverizing Saviae Miltiorrhizae radix into 80 mesh coarse powder, soaking in 90% (v/v) ethanol 1.5 times by weight for 24 hr, percolating with 90% (v/v) ethanol solution at a percolating speed of 1-3ml/min, collecting percolate 5 times of the crude drug weight, primary percolate 1 times of the crude drug weight, recovering ethanol from the rest percolate, and collecting medicinal liquid and residue;
soaking rhizoma Ligustici Chuanxiong, Eucommiae cortex, Notoginseng radix and semen plantaginis in 70% (v/v) ethanol 5 times the weight of the crude drug for 24 hr, soaking at room temperature for 3 times, mixing soaking solutions, recovering ethanol, and collecting medicinal liquid and residue;
decocting rhizoma Dioscoreae Septemlobae, Saviae Miltiorrhizae radix residue, rhizoma Ligustici Chuanxiong and other residues with 10 times of water for 3 times (1 hr each time), mixing decoctions, filtering, concentrating, adding the above Saviae Miltiorrhizae radix liquid and rhizoma Ligustici Chuanxiong liquid, concentrating under reduced pressure to obtain fluid extract with density of 1.20 at 50 deg.C, drying under reduced pressure to obtain dry extract,
adding auxiliary materials according to the weight ratio of 4: 1 of the crude drug, wherein the auxiliary materials are sugar powder and dextrin in a weight ratio of 3: 1, then crushing, sieving by a 80-mesh sieve, and uniformly mixing to obtain dry extract powder; granulating with Saviae Miltiorrhizae radix primary percolate and 80% (v/v) ethanol, drying, grading, and making into capsule, 1000 granules. The filling amount of each grain is 0.45 g.
Example 2
Experiments in zoology
Establishing a pelvic inflammatory disease mouse animal model: a healthy Kunming strain mouse is selected to construct a mouse pelvic inflammation model. Injecting 4% chloral hydrate into abdominal cavity according to 1% of mouse weight, general anaesthetizing, placing the mouse on a fixed table after several minutes, subtracting abdominal hair, disinfecting skin with 75% ethanol, taking sterilized scissors forceps, cutting off the skin and muscle layer of the lower abdomen of the mouse, cutting an incision of about 1cm, exposing uterus, taking a sterile needle to stab the middle position of uterine horn on one side of the uterus for about 5-6 needles, closing abdomen layer by layer after finishing, and disinfecting the abdominal operation area.
The experimental process comprises the following steps: selecting the mice molded above, and randomly dividing the mice into a blank control group (without any treatment), a model group, an example 1 group (20mg/d), a comparative example 2 group (20mg/d) after 7d, wherein each group contains 10 mice; except for the blank control and the model group, corresponding test samples were administered with an equal volume of pure water, and the gavage was continued for 21 d. Stopping taking the medicine the next day, weighing the mice, taking serum and killing the mice, taking the uterus after dissection, fixing the uterus with 4% neutral formaldehyde fixing solution, embedding the uterus with paraffin, and conventionally slicing the uterus; HE staining, and observing the pathological morphological change of the uterus under a light microscope. The results of the measurement of mouse serum indices cytokines are shown in Table 1.
TABLE 1
Group of Interleukin 2 (pg/ml) Interleukin 6 (pg/ml) Tumor necrosis factor α (pg/ml)
Blank control group 511.4 42.7 209.8
Model set 478.6 45.5 251.7
EXAMPLE 1 group 601.9 36.8 186.1
Comparative example 1 group 598.2 35.5 184.5
Comparative example 2 group 553.4 37.9 203.1
Conclusion, it can be seen from Table 1 above that the serum IL-2 content of the model group is reduced compared to the blank control group, while IL-6 and TNF α are significantly increased, indicating successful molding, the results of example 1 and comparative example 1
The content of interleukin 2 is higher than that of the group of the comparative example 2, the content of interleukin 6 and the content of tumor necrosis factor α are lower than that of the group of the comparative example 1, and the three indexes of interleukin 2, interleukin 6 and tumor necrosis factor α are not obviously different between the group of the example 1 and the group of the comparative example 1, which shows that the two indexes have similar anti-inflammatory effects.
The uterus pathology observation indexes and integral standards are as follows: (1) occlusion or expansion of intrauterine adhesions: "-" no lesion score 0; lesions "+" < 1/3 scored 1; "+ +" 1/3-2/3 lesions scored 2; "+ + + +" 2/3 the lesions above were scored 3 points. (2) And (3) pathological changes of the cavity wall structure: "-" each layer structure is normally marked with 0 point; the + mucosal lamina glandular structure disappearance score 1; the boundary between the muscle layer and the mucosa layer is not marked for 2 minutes; the "+ + + +" hierarchy does not note 3 points. (3) Epithelial cell degeneration and necrosis: "-" monolayer columnar epithelium score 0; "+" epithelial cell flattening or shedding < 1/3 score 1; "+ +" epithelial flattening or shedding 1/3-2/3 lesions scored 2; "+ + + +" Whole layer epithelial cells degenerated bad death for 3 points. (4) Infiltration of chronic inflammatory cells: "-" no chronic inflammatory cell infiltration score 0; the "+" decimal fraction is scattered or focal and only marks 1 point in the inherent layer of the mucosa; "+ +" scattered or focal but deep into the muscle layer scored 2 points; the majority of +++, is dispersed or layered and covers 3 points of the whole layer. (5) Intimal congestion and edema: "-" No intimal congestion edema score 0; "+" mild hyperemia and edema of lamina propria score of 1; "+ +" clear hyperemia and edema score 2; the total hyperemia and edema score 3 points +++ "is given. The results of the uterine pathology scoring are shown in table 2:
TABLE 2
Group of Occlusion or dilatation of intrauterine adhesions Pathological changes of cavity wall structure Degeneration and necrosis of epithelial cells Chronic inflammatory cell infiltration Congestion and edema of intima Total score
Blank pairPhoto group 0 0 0 0 0 0
Model set 7 6 5 4 7 29
EXAMPLE 1 group 1 0 2 2 3 8
Comparative example 1 group 2 0 1 2 2 7
Comparative example 2 group 2 1 3 2 5 13
And (4) conclusion: as can be seen from table 2, the example 1 and the comparative examples 1-2 both significantly improved the lesion degree of the uterus compared to the model group, wherein the example 1 and the comparative example 1 are not much different and are superior to the comparative example 2; the above data indicate that the deletion of the component notoginseng does not have a significant effect on the efficacy of the drug, but further tests are required to determine whether other indicators will be affected.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (5)

1. A granular preparation for treating chronic pelvic inflammatory disease comprises the following raw material medicines:
rhizoma smilacis glabrae, salvia miltiorrhiza, selfheal, dandelion, plantain seed, rhizoma dioscoreae hypoglaucae, eucommia ulmoides and ligusticum wallichii.
2. The granular preparation according to claim 1, which is prepared from the following raw material medicines:
1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark and 200g of szechuan lovage rhizome.
3. The granular preparation according to claim 1, which is prepared by the following process:
step 1) weighing raw materials, step 2) percolating with ethanol to extract salvia miltiorrhiza, step 3) extracting ligusticum wallichii, eucommia ulmoides and semen chebulae with ethanol, step 4) extracting rhizoma smilacis glabrae and dandelion with microwave ethanol, step 5) extracting rhizoma dioscoreae hypoglaucae and selfheal with ethanol by ultrasound, and step 6) extracting with water, concentrating, drying and preparing into capsules.
4. The granular preparation according to claim 1, which is prepared by the following process:
step 1), weighing raw material medicines: 1000g of glabrous greenbrier rhizome, 533.4g of salvia miltiorrhiza, 533.4g of selfheal, 666.6g of dandelion, 533.4g of plantain seed, 333.4g of rhizoma dioscoreae hypoglaucae, 333.4g of eucommia bark and 200g of szechuan lovage rhizome;
step 2) ethanol percolation extraction of salvia miltiorrhiza: pulverizing Saviae Miltiorrhizae radix into 200 mesh powder, soaking in 1.5 times of 90% (v/v) ethanol for 24 hr, percolating with 90% (v/v) ethanol solution at a percolating speed of 1-3ml/min, collecting percolate, recovering ethanol from percolate to obtain medicinal liquid, and collecting medicinal residue;
step 3), alcohol extraction of ligusticum wallichii, eucommia ulmoides and semen chebulae: mixing rhizoma Ligustici Chuanxiong, Eucommiae cortex and semen plantaginis, pulverizing into 200 mesh powder, adding 70% (v/v) ethanol 5 times the weight of the crude drug each time, soaking for 24 hr, soaking at room temperature for 3 times, mixing the soaking solutions, recovering ethanol, and keeping the medicinal liquid and residue;
step 4), microwave alcohol extraction of rhizoma smilacis glabrae and dandelion: pulverizing rhizoma Smilacis Glabrae and herba Taraxaci, sieving with 200 mesh sieve, placing in a container, adding 85% (v/v) ethanol twice the weight of the powder, stirring and extracting at 300rpm, controlling microwave power at 500W during extraction process, and extracting for 120 min; then placing at 4 ℃ for 12h, filtering and collecting filtrate, and keeping filter residues for later use;
step 5), ultrasonically extracting rhizoma dioscoreae hypoglaucae and selfheal to obtain the extract: pulverizing rhizoma Dioscoreae Septemlobae and Prunellae Spica, sieving with 200 mesh sieve, placing into ultrasonic extraction tank, adding 75% (v/v) ethanol with weight of three times of the powder, extracting at 50 deg.C and frequency of 50KHz for 30min, filtering, and collecting filtrate;
step 6), water extraction, concentration, drying and capsule preparation: mixing the residues obtained in the step 2), the step 3) and the step 4), adding 10 times of water by weight, decocting for 3 times, each time for 1 hour, mixing the decoctions, filtering, adding the liquid medicine obtained in the step 2), the liquid medicine obtained in the step 3), the filtrate obtained in the step 4) and the filtrate obtained in the step 5), uniformly mixing, concentrating under reduced pressure to obtain a clear paste with the density of 1.20g/ml, spray-drying to obtain a dry extract, crushing, adding silicon dioxide according to the mass ratio of 20:1, granulating with ethanol, drying, and encapsulating to obtain the capsule.
5. The use of a granular formulation according to any one of claims 1 to 4 for the treatment of chronic pelvic inflammatory disease.
CN201911385636.1A 2019-12-29 2019-12-29 Granular preparation for treating chronic pelvic inflammatory disease and application thereof Pending CN111228427A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115192696A (en) * 2022-07-13 2022-10-18 翔宇药业股份有限公司 Active antibacterial gynecological lotion and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101019982A (en) * 2006-09-29 2007-08-22 林凡儒 Medicine for treating chronic pelvic inflammation and its prepn
CN107468865A (en) * 2017-09-06 2017-12-15 翔宇药业股份有限公司 The preparation technology of Pu Ling basin inflammation recovering particles

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101019982A (en) * 2006-09-29 2007-08-22 林凡儒 Medicine for treating chronic pelvic inflammation and its prepn
CN107468865A (en) * 2017-09-06 2017-12-15 翔宇药业股份有限公司 The preparation technology of Pu Ling basin inflammation recovering particles

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115192696A (en) * 2022-07-13 2022-10-18 翔宇药业股份有限公司 Active antibacterial gynecological lotion and preparation method thereof
CN115192696B (en) * 2022-07-13 2023-07-14 翔宇药业股份有限公司 Active antibacterial gynecological lotion and preparation method thereof

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Application publication date: 20200605