CN109394793A - The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis - Google Patents
The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis Download PDFInfo
- Publication number
- CN109394793A CN109394793A CN201811639076.3A CN201811639076A CN109394793A CN 109394793 A CN109394793 A CN 109394793A CN 201811639076 A CN201811639076 A CN 201811639076A CN 109394793 A CN109394793 A CN 109394793A
- Authority
- CN
- China
- Prior art keywords
- extraction
- formica fusca
- heat type
- damp
- vulvitis
- 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
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K35/00—Medicinal preparations containing materials or reaction products thereof with undetermined constitution
- A61K35/56—Materials from animals other than mammals
- A61K35/63—Arthropods
- A61K35/64—Insects, e.g. bees, wasps or fleas
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
- A61P15/02—Drugs for genital or sexual disorders; Contraceptives for disorders of the vagina
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Insects & Arthropods (AREA)
- Chemical & Material Sciences (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Veterinary Medicine (AREA)
- Animal Behavior & Ethology (AREA)
- Gynecology & Obstetrics (AREA)
- Animal Husbandry (AREA)
- Epidemiology (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Endocrinology (AREA)
- Reproductive Health (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses the preparation methods of the Formica fusca extract for the treatment of damp-heat type vulvitis, include the following steps: feedstock processing；High pressure microjet ultramicro crushing treatment；Separation: aqueous two-phase extraction is carried out to paste serous material is obtained, it obtains the upper phase of extraction and extracts lower phase, double-aqueous phase system used in aqueous two-phase extraction is made of polyethylene glycol, sodium chloride and water, mass percent of the polyethylene glycol in double-aqueous phase system is 10-25%, mass percent of the sodium chloride in double-aqueous phase system is 10-20%, surplus is water, and the weight average molecular weight of the polyethylene glycol is 1000-8000；Desalting processing；Column chromatography；It is dry: upper step eluent is dried to obtain Formica fusca extract.
Description
Technical field
The present invention relates to the active constituent of field of biotechnology and its extracting methods, specifically treat damp-heat type vulvitis
Formica fusca extract and preparation method thereof.
Background technique
The skins such as pruitus, eczema, body stock addiction, pruritus vulvue, vulvitis, nonspecific vaginitis and allergic dermatitis
Disease is common disease.In the ratio of human diseases, skin disease patient occupies sizable specific gravity, shows according to relevant information
There is 60% or more people to suffer from skin disease to varying degrees.
Silky ant (Polyrhachis vicina Roger), is called Polyhachis vicina Roger, polyrhachis vicina Roger, bidentate thorniness
Ant belongs to Arthropoda, Insecta, film wing day, Formicidae, Formicinae, Polyrhachis, for the social insect being gregariousness." herbal guiding principle
Mesh " in, to the habit of ant, toxicity, it is edible and it is medicinal all made detailed record, ant has " strengthening vital QI to eliminate pathogenic factors " and " different disease
With controlling " unique effects.The pharmacological evaluation of nineteen eighty-three Zhao's first-class prompts, and silky ant has anti-inflammatory, protect liver, calmness, relievings asthma, spasmolysis
The effects of, while carried out toxicity and subacute measurement prompt its is nontoxic.Formica fusca extract includes melanin
(Melanin), the nitrogenous high polymer of the complexity of one kind as made of indoles substance or polyphenols oxidation polymerization, it is extensively
It is present in plant, animal and microorganism.Melanin is to be insoluble in water, acid and organic molten generally in black, brown or brown
A kind of large biological molecule of agent.Melanin, which has, the health cares work such as adjusts physiological function, improves immunity, anti-aging, keeps fit and healthy
With.In addition, melanin also has protection large biological molecule, has significant inhibiting effect to AIDS virus in vitro.Currently, black
Natural black pigment contained in sesame, black rice, semen sojae atricolor, blank corn, black-bone chicken etc. has caused the great interest of people, finds it
Have effects that nourishing, health, anti-oxidant and anti-aging etc., but the research of silky ant melanin is rarely reported.
Silky ant is known as " microfauna high-grade nutrient treasure-house ", and 1993, health ministry determined it as the nontoxic nothing of dual-purpose of drug and food
Harmful excellent ant kind.
In existing research, extraction for Formica fusca extract or ant melanin is general to use: silky ant crushes-
Precipitating-vacuum drying-is collected in the heavy operation of the heavy-centrifugation-precipitating-repetition alkali soluble acid of sour water solution-centrifugation-melanin crude product-alkali soluble acid
The technique of melanin product, such operation, one is complex process, and the time used in entire technique is long.The country is to silky ant
Chemical component, pharmacological action and clinical application carried out more research.Result of study shows that silky ant has enhancing immune
Function, anti-aging effects, it is antitumor, adjust blood glucose the effects of, for Formica fusca extract be applied to treatment skin disease, gynaecological disease
It has not been reported.
The domestic externally applied drug for using pure Chinese herbal medicine preparation for treating skin disease, gynaecological disease, effect are preferably few in number at present.
There are many patients in clinic, influences the physical and mental health of patient due to cannot get efficient drug therapy and cause suffering, very
To causing unnecessary economic loss.Therefore, research and development have significant curative effect skin disease, gynecology externally used pharmaceutical has very much must
It wants, in particular with the local animal and plant resource abundant in Guangxi, development, for the disease for releasing skin disease and gynaecology patient
Hardship protects the health of the people, provides effective pure Chinese medicinal preparation, it is contemplated that can produce good social benefit and significant warp
Ji benefit.
Summary of the invention
The object of the present invention is to provide the preparation method of the Formica fusca extract for the treatment of damp-heat type vulvitis, obtained extraction
Ant melanin rich in object, can effectively treat damp-heat type vulvitis.
The invention is realized by the following technical scheme:
The preparation method for treating the Formica fusca extract of damp-heat type vulvitis, includes the following steps:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained, the pure water of the weight such as addition add phase
When handling 10-20min, revolving speed 8000- with high-speed shearing emulsion machine in the petroleum sodium sulfonate of powder weight 0.3-0.5%
Then 12000r/min is handled with high pressure microjet Ultra-Micro Grinding Equipment in 25 DEG C, processing pressure 80-120MPa, place
Managing number is 2-3 times, obtains paste serous material；
3) separation: carrying out aqueous two-phase extraction to paste serous material is obtained, and obtains the upper phase of extraction and extracts lower phase, aqueous two-phase extraction
Used double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality of the polyethylene glycol in double-aqueous phase system
Percentage is 10-25%, and mass percent of the sodium chloride in double-aqueous phase system is 10-20%, and surplus is water, described poly-
The weight average molecular weight of ethylene glycol is 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merging the liquid obtained after desalination, filters, concentration is chromatographed by column, with D101 type macroporous absorption tree
Rouge is adsorbed, and cleaning resin to trickle with deionized water is colourless, then the ethanol solution for being 20-30% with volumetric concentration
Eluent is collected in elution；
6) dry: upper step eluent is dried to obtain Formica fusca extract.
Sieving described in step 1) of the present invention is to sieve with 100 mesh sieve.
Desalination described in step 4) is using ultrafiltration or dialysis, and ultrafiltration uses molecular cut off for 1000-
100000 ultrafiltration membrane desalination, dialysis use molecular cut off for the bag filter desalination of 1000-100000.
Drying described in step 6), using spray drying or freeze-drying.
Compared with prior art, advantages of the present invention:
1, super using high pressure microjet by the present invention in that handling silky ant raw material with high pressure microjet superfine communication technique
Micro-crushing equipment generate extruding force, shearing force, impact force, by liquid-liquid, it is liquid-solid between high-speed impact, high shear, hole
Effect etc., makes the molecular structure of material change.High pressure microjet Ultra-Micro Grinding Equipment can accomplish nano-dispersed, refinement effect
For fruit up to 0.lum even hereinafter, pressure is up to 80-120MPa, obtained solution particles particle diameter distribution is uniform, has operation letter
It is single, pollution-free, can online cleaning-sterilizing, can high efficiency many advantages, such as carrying out breaking-wall cell.
2, Formica fusca extract, main component is ant melanin, is to be insoluble in generally in black, brown or brown
A kind of large biological molecule of water, acid and organic solvent.Existing extracting method is all that directly silky ant raw material is smashed or crushed
Afterwards by sour water solution, alkali soluble acid sinks and extracts repeatedly, or mentioned by water/modes such as alcohol extracting, enzymatic hydrolysis or Microwave Extraction are straight
Connect extraction, the above processing, the grease in silky ant cell can be isolated simultaneously, and the ingredients such as group and melanin containing greasy are mixed
Together, to influence the separation of subsequent effective component, the processing difficulty of process is increased.The present invention first uses high pressure microjet
Superfine communication technique processing joined mahogany acid when using high pressure microjet superfine communication technique processing silky ant raw material
Sodium has the sulfonic group of a strongly hydrophilic to be linked with alkyl in molecular structure, and surface-active is strong, so that in ant melanin
2 kinds of incompatible polar groups: hydrophilic group and lipophilic group separately adsorb, using non-oil component to oil and water affinity it is poor
Different and grease specific gravity is different and separates oil with non-oil component, conducive to the aqueous two-phase extraction of lower step, passes through different extraction items
Part, so that melanin and other compositions are kept completely separate.
3, the separation of ant melanin is more complete in the Formica fusca extract by means of the present invention, obtained, makes to develop the color
The ant melanin of High color values, color value E are obtained after reaction214> 345, the Formica fusca extract obtained by the experimental verification present invention
Application in treatment damp-heat type vulvitis drug.
Detailed description of the invention
Fig. 1 is the UV-visible spectrum for the Formica fusca extract that the embodiment of the present invention 3 obtains.
Fig. 2 is the infrared spectrum spectrogram for the Formica fusca extract that the embodiment of the present invention 3 obtains.
Specific embodiment
With embodiment, the invention will be further described below, but the invention is not limited to these embodiments.
Embodiment 1:
The preparation method for treating the Formica fusca extract of damp-heat type vulvitis, includes the following steps:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained, the pure water of the weight such as addition add phase
When handling 20min, revolving speed 8000r/min with high-speed shearing emulsion machine, then in the petroleum sodium sulfonate of powder weight 0.3%
It is handled with high pressure microjet Ultra-Micro Grinding Equipment in 25 DEG C, processing pressure 120MPa, number of processes is 2 times, obtains cream
Shape slurries；
3) separation: carrying out aqueous two-phase extraction to paste serous material is obtained, and obtains the upper phase of extraction and extracts lower phase, aqueous two-phase extraction
Used double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality of the polyethylene glycol in double-aqueous phase system
Percentage is 10%, and mass percent of the sodium chloride in double-aqueous phase system is 10%, and surplus is water, the polyethylene glycol
Weight average molecular weight be 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merging the liquid obtained after desalination, filters, concentration is chromatographed by column, with D101 type macroporous absorption tree
Rouge is adsorbed, and cleaning resin to trickle with deionized water is colourless, then the ethanol solution for being 20-30% with volumetric concentration
Gradient elution collects eluent；
6) dry: to be freeze-dried upper step eluent to obtain Formica fusca extract powder.
Embodiment 2:
The preparation method for treating the Formica fusca extract of damp-heat type vulvitis, includes the following steps:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained, the pure water of the weight such as addition add phase
When handling 10min, revolving speed 12000r/min with high-speed shearing emulsion machine, then in the petroleum sodium sulfonate of powder weight 0.4%
It is handled with high pressure microjet Ultra-Micro Grinding Equipment in 25 DEG C, processing pressure 80MPa, number of processes is 3 times, obtains paste
Slurries；
3) separation: carrying out aqueous two-phase extraction to paste serous material is obtained, and obtains the upper phase of extraction and extracts lower phase, aqueous two-phase extraction
Used double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality of the polyethylene glycol in double-aqueous phase system
Percentage is 15%, and mass percent of the sodium chloride in double-aqueous phase system is 20%, and surplus is water, the polyethylene glycol
Weight average molecular weight be 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merging the liquid obtained after desalination, filters, concentration is chromatographed by column, with D101 type macroporous absorption tree
Rouge is adsorbed, and cleaning resin to trickle with deionized water is colourless, then the ethanol solution for being 20-30% with volumetric concentration
Gradient elution collects eluent；
6) dry: to be spray-dried upper step eluent to obtain Formica fusca extract powder.
Embodiment 3:
The preparation method for treating the Formica fusca extract of damp-heat type vulvitis, includes the following steps:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained, the pure water of the weight such as addition add phase
When handling 15min, revolving speed 10000r/min with high-speed shearing emulsion machine, then in the petroleum sodium sulfonate of powder weight 0.5%
It is handled with high pressure microjet Ultra-Micro Grinding Equipment in 25 DEG C, processing pressure 100MPa, number of processes is 3 times, obtains cream
Shape slurries；
3) separation: carrying out aqueous two-phase extraction to paste serous material is obtained, and obtains the upper phase of extraction and extracts lower phase, aqueous two-phase extraction
Used double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality of the polyethylene glycol in double-aqueous phase system
Percentage is 25%, and mass percent of the sodium chloride in double-aqueous phase system is 15%, and surplus is water, the polyethylene glycol
Weight average molecular weight be 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merging the liquid obtained after desalination, filters, concentration is chromatographed by column, with D101 type macroporous absorption tree
Rouge is adsorbed, and cleaning resin to trickle with deionized water is colourless, then the ethanol solution for being 20-30% with volumetric concentration
Gradient elution collects eluent；
6) dry: to be freeze-dried upper step eluent to obtain Formica fusca extract powder.
Comparative example 1:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained the pure water of weight such as is added, with cutting at a high speed
Mulser processing 15min, revolving speed 10000r/min are cut, then with high pressure microjet Ultra-Micro Grinding Equipment at 25 DEG C
Reason, processing pressure 100MPa, number of processes are 3 times, obtain paste serous material；
3) separation: carrying out aqueous two-phase extraction to paste serous material is obtained, and obtains the upper phase of extraction and extracts lower phase, aqueous two-phase extraction
Used double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality of the polyethylene glycol in double-aqueous phase system
Percentage is 25%, and mass percent of the sodium chloride in double-aqueous phase system is 15%, and surplus is water, the polyethylene glycol
Weight average molecular weight be 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merging the liquid obtained after desalination, filters, concentration is chromatographed by column, with D101 type macroporous absorption tree
Rouge is adsorbed, and cleaning resin to trickle with deionized water is colourless, then the ethanol solution for being 20-30% with volumetric concentration
Gradient elution collects eluent；
6) dry: to be freeze-dried upper step eluent to obtain Formica fusca extract powder.
Comparative example 2:
The heavy operation of the heavy-centrifugation-precipitating-repetition alkali soluble acid of silky ant crushing-sour water solution-centrifugation-melanin crude product-alkali soluble acid
Collect precipitating-vacuum drying-melanin product.
Experimental example 1: the UV-visible spectrum for the Formica fusca extract that embodiment 3 obtains
Melanin polymer generates spectral absorption characteristics because of the conjugation of its height, silky ant melanin it is ultraviolet-
Visible spectrum, a length of 214nm of its maximum absorption wave as shown in Figure 1:, without characteristic absorption peak, absorption value in visible region
It is reduced with the increase of wavelength.This with it is existing studies have reported that separate sources melanin maximum absorption wavelength in 210nm or so
It is consistent.
Experimental example 2: the infrared spectrum spectrogram for the Formica fusca extract that embodiment 3 obtains
Existing research shows that indoles type melanin leaded wastewater is 6-9%, 3 silky ant of embodiment is measured using Kjeldahl's method
Extract (silky ant melanin) nitrogen content is 6.35%.
As shown in Figure 2: existing research is it is also shown that Formica fusca extract (silky ant melanin) is that complicated biology is big
Molecule, infrared spectroscopy is a series of width and strong absorption peak, each broad peak are all to be vibrated to be formed by a variety of functional groups.From figure
In 2, it can deduce:
(1) in 1450-1650cm-1Nearby there is stronger absorption peak caused by phenyl ring skeletal vibration, in 602cm-1Place absorbs
Peak is weaker, illustrates that phenyl ring is substituted, forms π-conjugated systems；
(2) in 1646cm-1Neighbouring strong absworption peak is caused by completing the C=0 stretching vibration of base, with 3421cm-1Place
Strong absworption peak together, the presence of instruction-C00H structure, the in addition absorption frequency red shift of carbonyl, illustrate the carboxyl in molecule be with
Aromatic carboxylic acids structure exists；
(3) in 2853cm-1、2925cm-1Neighbouring weak absorbing band, be on phenyl ring-stretching vibration of c h bond formed；
(4) in 3421cm-1Nearby there is the resonance absorbing peak of Qiang Erkuan, illustrates presence -0H and indoles-NH structure, absorption peak
It is wide and be by force the as caused by the hydrogen bond connection between -0H and-NH
Indoles type can be tentatively classified as according to the similarity of infrared spectroscopy.Meanwhile it is existing research shows that silky ant black
Element has the structure feature of indoles type, and the viewpoint that indoles type more is belonged to animal sources melanin is consistent.
Experimental example 3: the measurement of silky ant melanin color value
0.1000g sample is accurately weighed, 0.0002g is accurate to, is dissolved in the phosphate buffer solution that pH is 8.0,40 DEG C
Water-bath 1h is settled in 100mL volumetric flask after dissolving melanin.A certain amount of weak solution dilution is drawn, accurately again with absorbance
It is advisable in 0.3-0.7.At melanin maximum absorbance 214nm, make reference liquid with phosphate buffer, surveys its absorbance.
The color value of melanin solution is calculated according to the following formula: (in formula: A is actual measurement light absorption value to E=Axf/m；F is dilution times
Number；M is sample mass)
Experimental example 4: the embodiment of the present invention 3 and comparative example 2 treat damp-heat type vulvitis clinical observation on the therapeutic effect:
Place: affiliated hospital, Medical Colleges Of Guilin
Time: in May, -2018 in April, 2016
1. general information (is shown in Table)
1.1 wind-heat blood-heat type pruritus due to wind pathogen
Table 1 (A is treatment group, and B, C are control group, similarly hereinafter)
1.2 damp-heat type leukorrhagia
Table 2
2. case selection
It is all to meet tcm diagnosis standard, dialectical category wind-heat blood-heat type pruritus due to wind pathogen and damp-heat type leukorrhagia patient and be included in observation
Object.
3. diagnostic criteria
3.1 tcm diagnosis standard
3.1.1 wind-heat blood-heat type pruritus due to wind pathogen
Generally be with year less serious case it is more, disease belongs to new and rises, can cause to break out or aggravate itch as bedding is too warm, moss thin yellow,
Slippery or sliding number.
3.1.2 damp-heat type leukorrhagia
Woman's leukorrhagia amount increased significantly, and color, matter are abnormal, or have foul smell, with whole body or local symptom person.
3.2 Western medicine diagnostic criteria
3.2.1 wind-heat blood-heat type pruritus due to wind pathogen
3.2.1.1 there was only itch when onset, can be systemic and limitation without any primary fash.
3.2.1.2 paroxysmal itch often influences to sleep often based on night because of itch, often excited.Temperature
Change, drink or eat maror induction and Cheng Jiachong.
There is the secondary skin lesion such as scratch, scab, pigmentation, eczematization, lichenification when 3.2.1.3.
3.2.2 damp-heat type leukorrhagia
3.2.2.1 vulvitis
Skin of vulva itch, pain.Local redness is shown in inspection, and swelling often has scratch, and secretion increases, and is sometimes in purulence.
Nymphae can stain be rotten due to being impregnated by secretion, and is covered with opposite side adhesion or even urethral orifice and the labia of introitus adhesion,
Cause dysuria.By checking, trichomonad, mould, senile vahinitis and leukoplakia vulvae, diabetes, Behcet's disease institute are excluded
Caused itching of vulva pain.
3.2.2.2 nonspecific vaginitis
3.2.2.2.1 symptom: pruritus vulvue, cusalgia or with the urethral stimulants symptom such as frequent micturition, urgent urination, urodynia, or with
Local stimulation symptom.
3.2.2.2.2 gynecologial examination: vaginal fluid is in purulence or serosity, and still bed or curdy, vagina mucosa fill
Blood has erosion pain.
3.2.2.2.3 laboratory checks: can have white thin full or pyocyte in vaginal fluid under microscope.
4. exclusion criteria (packet hangs inadaptation or rejects standard)
4.1 wind-heat blood-heat type pruritus due to wind pathogen
4.1.1 belong to scabies, grain itch, lice disease, local neurodermatitis, diabetes, yellow subcutaneous ulcer, endocrine battle array hinder, ephritis,
Itch caused by enterozoon etc..
4.1.2 the age is in under-18s or over-65s, pregnant or breast feeding women, those who are allergic to this drug.
4.1.3 the severe primaries diseases, mental patient such as cardiovascular, liver kidney and hemopoietic system are associated with.
4.1.4 the standard of being included in is not met, not by regulation medication, can not judge that curative effect or data be not congruent and affect the treatment or pacify
Full property judgement person.
4.2 damp-heat type leukorrhagia
4.2.1 it confirms on inspection by gynecological tumor and venereal disease causer.
4.2.2 the age is in under-18s or over-65s person, gestation or breast feeding women and to research drug allergy person.
4.2.3 be associated with the severe primaries such as angiocarpy, liver, kidney and hemopoietic system disease, mental patient "
4.2.4 the standard of being included in is not met, not by regulation medication, can not judge that curative effect or data be not congruent and affect the treatment or pacify
Full property judgement person.
5. observation method
5.1 wind-heat blood-heat type pruritus due to wind pathogen
90 are observed altogether, are randomly divided into 3 groups, wherein treatment group 30, are used 3 liniment of embodiment；Control group 1 30, make
With " clean that yin " washing lotion (production of Chengdu EnXue Shiheng pharmaceutical Co. Ltd)；Control group 2 30, use 2 liniment of comparative example.
Treatment group: the processing of 3 product of embodiment, it is 1.05- that the column chromatographic eluate of embodiment 3, which is concentrated into relative density,
1.08 (65-70 DEG C), let cool, and ethyl alcohol, which is added, makes alcohol content up to 32%, stir evenly, stand overnight, take supernatant, add water to
1000ml mixes to get liniment.
Control group 1: " clean that yin " washing lotion (production of Chengdu EnXue Shiheng pharmaceutical Co. Ltd) is used.
Control group 2: the heavy operation of alkali soluble acid is repeated in comparative example 2 and collects precipitating, being concentrated into relative density is 1.05-1.08
(65-70 DEG C), lets cool, and ethyl alcohol, which is added, makes alcohol content up to 32%, stirs evenly, stands overnight, take supernatant, adds water to 1000ml, mixes
It is even to get liniment.
Usage: directly medical fluid painting is put on the skin in affected part, day applies 3 times, is used in conjunction 7 days.
It is conventional before test that detailed physical examination made to subject, it is all to meet case selection standard person and be included in observation pair
As.3rd, 7 day each follow-up 1 time after test records the state of an illness and side effect.Therapeutic effect is evaluated with integration method.Symptom and sign degree
Classification and scoring criteria are detailed in " observation table ".Curative effect judgement is directly made by observer.Do not have to other medicines during observation:
5.2 damp-heat type leukorrhagia
80 are observed altogether, are randomly divided into 3 groups.Wherein treatment group 30 control group 1 20, are made using 3 liniment of embodiment
With " clean that yin " washing lotion (production of Chengdu EnXue Shiheng pharmaceutical Co. Ltd)；Control group 2 30, use 2 liniment of comparative example.
Usage: directly medicine liquid spray is used in conjunction 7 days, non-specific vagina 3 times a day in clean affected part by vulvitis person
Scorching person is used in conjunction 7 days after medical fluid is then diluted 5 times with warm water with vaginal douche washing vagina one time a day.
It is conventional before test that gynecologial examination is made to subject, it takes vaginal fluid to make microexamination, meets case selection mark
Quasi- person can be included in observation object.Ji Zuo gynaecology and the check of vaginal fluid microscope after the course for the treatment of.It is controlled with integration method evaluation
Therapeutic effect.Symptom and sign grading and scoring criteria are detailed in " observation table ".Curative effect judgement is directly made by observer.Observation period
Between deactivate other medicines.
6. result
The conspicuousness that 6.1 wind-heat blood-heat type pruritus due to wind pathogen witness integral difference before and after treatment compares (t examines Check)
Table 3
A, B has significant difference (P<0.01), and there was no significant difference by C (P>0.05)
The conspicuousness that 6.2 damp-heat type leukorrhagia witness integral difference before and after treatment compares (t inspection)
Table 4
A, B has significant difference (P<0.01), and there was no significant difference by C (P>0.05)
6.3 damp-heat type leukorrhagia drugs be in harmony treat after vaginal fluid leucocyte negative conversion rate comparison (X2It examines)
Table 5
A, there was no significant difference (P > 0.05) by B.
Comparison (the X of vaginal fluid pyocyte negative conversion rate after 6.4 damp-heat type leukorrhagia drug therapies2It examines)
Table 6
A, there was no significant difference (P > 0.05) by B
7. the comparison (Ridit analysis) of curative effect of medication
Table 7
A, there was no significant difference (P > 0.05) for curative effect of the two groups of drugs of B to two kinds of diseases
8. adverse reaction and toxic side effect
There is adverse reaction and toxic side effect without an example during 170 verifyings.
9. discussing
Without conspicuousness on the sex structure of two groups of cases of 9.1 wind-heat blood-heat type pruritus due to wind pathogen and damp-heat type leukorrhagia and age distribution
Difference (is shown in Table 1,2).
Two groups of drugs of 9.2A, B its card integral pretherapy and post-treatment to wind-heat blood-heat type pruritus due to wind pathogen and damp-heat type leukorrhagia and sign are equal
There is significant difference (P < 0.01), that is to say, that two kinds of drugs are significantly improved effect to the sings and symptoms of two kinds of diseases
(being shown in Table 3,4)；C group drug its card integral pretherapy and post-treatment to wind-heat blood-heat type pruritus due to wind pathogen and damp-heat type leukorrhagia and sign are without significantly
Sex differernce (P > 0.05), that is to say, that drug is to the sings and symptoms of two kinds of diseases without significant improvement result (being shown in Table 3,4).
Two kinds of drugs of 9.3A, B to the cell and pyocyte of damp-heat type leukorrhagia vaginal secretion have it is higher kill suppression rate, but between group
There was no significant difference.(P > 0.05 is shown in Table 5,6)；C group drug kills suppression rate to the cell of damp-heat type leukorrhagia vaginal secretion and pyocyte
There were significant differences for lower and A, B group.
Two groups of drugs of 9.4A, B have higher curative effect to two kinds of diseases, but there was no significant difference between group (P > 0.05).
10. conclusion
10.1 verification results show that 3 liniment of embodiment has the effect of dispelling wind and arresting itching, removing damp-heat really, to wind-heat blood
The clinical symptoms of heat type pruritus due to wind pathogen and damp-heat type leukorrhagia are significantly improved effect.
10.2 embodiment, 3 liniment has higher curative effect to wind-heat blood-heat type pruritus due to wind pathogen and damp-heat type leukorrhagia, total effective
Rate is respectively 93.33% and 93.33%, is suitable for the treatment medication of two kinds of diseases, and curative effect is affirmative.
The effect of 10.3 embodiments 3 and the difference on effect of comparative example 2 are significant, illustrate the black ant that different preparation processes obtains
Ant extract activity has difference.
There is adverse reaction and toxic side effect without an example during verifying, illustrates that 3 liniment clinical application of embodiment is that safety can
It leans on, dosage form is also reasonable.
There is adverse reaction and toxic side effect without an example during 10.4 verifyings, illustrates that 3 liniment clinical application of embodiment is peace
Complete reliable, dosage form is also reasonable.
Claims (5)
1. the preparation method for treating the Formica fusca extract of damp-heat type vulvitis, which comprises the steps of:
1) feedstock processing: the silky ant of drying is crushed, sieving；
2) high pressure microjet ultramicro crushing treatment: the powder that upper step is obtained, the pure water of the weight such as addition are added and are equivalent to
The petroleum sodium sulfonate of powder weight 0.3-0.5% handles 10-20min, revolving speed 8000-12000r/ with high-speed shearing emulsion machine
Min, is then handled with high pressure microjet Ultra-Micro Grinding Equipment in 25 DEG C, processing pressure 80-120MPa, and number of processes is
2-3 times, obtain paste serous material；
3) it separates: carrying out aqueous two-phase extraction to paste serous material is obtained, acquisition extraction is upper mutually to be made with the lower phase of extraction, aqueous two-phase extraction
Double-aqueous phase system is made of polyethylene glycol, sodium chloride and water, quality percentage of the polyethylene glycol in double-aqueous phase system
Than for 10-25%, mass percent of the sodium chloride in double-aqueous phase system is 10-20%, and surplus is water, the poly- second two
The weight average molecular weight of alcohol is 1000-8000；
4) desalting processing: phase in the extraction that step 3) is obtained, desalination, phase under the extraction that step 3) is obtained, desalination；
5) column chromatographs: merge obtained liquid after desalination, filter, concentration is chromatographed by column, with D101 type macroporous absorbent resin into
Row absorption, it is colourless for cleaning resin to trickle with deionized water, then is washed with the ethanol solution that volumetric concentration is 20-30%
It is de-, collect eluent；
6) dry: upper step eluent is dried to obtain Formica fusca extract.
2. the preparation method of the Formica fusca extract for the treatment of damp-heat type vulvitis according to claim 1, it is characterised in that:
Sieving described in step 1) is to sieve with 100 mesh sieve.
3. the preparation method of the Formica fusca extract for the treatment of damp-heat type vulvitis according to claim 1, it is characterised in that:
Desalination described in step 4) is using ultrafiltration or dialysis, and ultrafiltration uses molecular cut off for the ultrafiltration of 1000-100000
Film desalination, dialysis use molecular cut off for the bag filter desalination of 1000-100000.
4. the preparation method of the Formica fusca extract for the treatment of damp-heat type vulvitis according to claim 1, it is characterised in that:
Drying described in step 6), using spray drying or freeze-drying.
5. the Formica fusca extract that any preparation method of claim 1-5 obtains is in the drug for the treatment of damp-heat type vulvitis
In application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811639076.3A CN109394793A (en) | 2018-12-29 | 2018-12-29 | The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811639076.3A CN109394793A (en) | 2018-12-29 | 2018-12-29 | The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109394793A true CN109394793A (en) | 2019-03-01 |
Family
ID=65462729
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811639076.3A Pending CN109394793A (en) | 2018-12-29 | 2018-12-29 | The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109394793A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067377A (en) * | 1992-07-21 | 1992-12-30 | 温元凯 | Formica fusca extract and preparation thereof |
| GB0017046D0 (en) * | 2000-07-11 | 2000-08-30 | Pharmaceutical Ind Tech & Dev | Anti-ulcer pharmaceutical composition and the preparation thereof |
| CN103497535A (en) * | 2013-10-10 | 2014-01-08 | 西南科技大学 | Animal melanin extraction method and application of extraction product thereof |
| CN104672345A (en) * | 2015-03-31 | 2015-06-03 | 广西还珠海洋生物科技有限公司 | Method for preparing crude polysaccharide from steindachner soft-shelled turtle carapace |
| CN106344616A (en) * | 2016-10-25 | 2017-01-25 | 桂林淮安天然保健品开发有限公司 | Black ant extract and preparation technique thereof |
| CN107365284A (en) * | 2017-08-16 | 2017-11-21 | 桂林茗兴生物科技有限公司 | A kind of method that taxol is extracted from Chinese yew |
-
2018
- 2018-12-29 CN CN201811639076.3A patent/CN109394793A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067377A (en) * | 1992-07-21 | 1992-12-30 | 温元凯 | Formica fusca extract and preparation thereof |
| GB0017046D0 (en) * | 2000-07-11 | 2000-08-30 | Pharmaceutical Ind Tech & Dev | Anti-ulcer pharmaceutical composition and the preparation thereof |
| CN103497535A (en) * | 2013-10-10 | 2014-01-08 | 西南科技大学 | Animal melanin extraction method and application of extraction product thereof |
| CN104672345A (en) * | 2015-03-31 | 2015-06-03 | 广西还珠海洋生物科技有限公司 | Method for preparing crude polysaccharide from steindachner soft-shelled turtle carapace |
| CN106344616A (en) * | 2016-10-25 | 2017-01-25 | 桂林淮安天然保健品开发有限公司 | Black ant extract and preparation technique thereof |
| CN107365284A (en) * | 2017-08-16 | 2017-11-21 | 桂林茗兴生物科技有限公司 | A kind of method that taxol is extracted from Chinese yew |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101095751B (en) | Medicinal composition having functions of removing chloasma and improving nutritional anemia and method for preparing the same | |
| CN106692692A (en) | Dendrobium officinale extract and preparation method thereof | |
| CN101002858A (en) | Medicine composition for enhancing immunity, and its preparing method and use | |
| CN104622740B (en) | Purposes of the Horse chest Nut P.E in cosmeceutical is prepared | |
| CN106729136A (en) | A kind of functional food for adjusting immunity | |
| CN102304189B (en) | Method for extracting anti-oxidant mung bean polysaccharide | |
| CN108157575A (en) | A kind of pressed candy for alleviating visual fatigue and preparation method and application | |
| CN107320565A (en) | A kind of Chinese medicine composition with antiallergic sense effect and its preparation method and application | |
| CN104288201A (en) | Safflower soft capsule and preparation method thereof | |
| CN103584091B (en) | A kind of guarantor with raising immunity, hypolipemic function builds food and preparation method thereof | |
| CN107912771A (en) | A kind of stem of noble dendrobium composition with enhancing immune function and preparation method thereof | |
| CN105056128B (en) | A kind of Chinese medicine composition and preparation method and application for treating atrophic gastritis and intestines | |
| CN102885307B (en) | Composition for damp-heat constitutions, preparation method and applications thereof | |
| CN104012982A (en) | Health care product composition with immunity increasing function, soft capsule and preparation method thereof | |
| CN109394793A (en) | The Formica fusca extract and preparation method thereof for treating damp-heat type vulvitis | |
| CN101972334A (en) | Traditional Chinese medicine preparation for preventing and treating infantile eczema and preparation method thereof | |
| AU2004318154B2 (en) | Pharmaceutics of traditional chinese medicine of treating aids and preparation method thereof | |
| CN108186920A (en) | A kind of pharmaceutical composition with auxiliary lipid-lowering efficacy and preparation method thereof | |
| CN106749732A (en) | Artemisia rupestris extraction method of polysaccharides | |
| CN102764338A (en) | Medicine composition for treating renal diseases | |
| CN100428951C (en) | Yuanhe tablet and process for preparing the same | |
| CN109370254A (en) | A method of preparing High color values ant melanin from silky ant | |
| CN101785815A (en) | Health care product with auxiliary functions on blood fat reduction and chemical liver injury protection | |
| CN105998191A (en) | Application of general anesthetic to preparation of drugs for treating gout | |
| CN104587300A (en) | Traditional Chinese medicine composition for treating acute leukemia and preparation method of traditional Chinese medicine composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190301 |
|
| RJ01 | Rejection of invention patent application after publication |