CN102846668A - Preparation method for nanometer Periplaneta americana - Google Patents
Preparation method for nanometer Periplaneta americana Download PDFInfo
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Abstract
The invention discloses a preparation method for nanometer Periplaneta americana. The method comprises the following steps: soaking, degreasing, heating, washing, three times of extraction, primary filtration, concentration, secondary filtration and supersonic jet drying. A nanometer Periplaneta americana particle prepared by using the method provided by the invention is fine and uniform and has good dispersity and a particle size of 0 to 100 nm; the solubility and bioavailability of pharmaceutical components of Periplaneta americana can be improved or increased; the pharmaceutical components of Periplaneta americana can be delivered to a specified target area so as to realize targeted drug delivery; the nanometer Periplaneta americana has safety and can reduce some irritation to the stomach; and special biological activity of Periplaneta Americana, such as alanine and the like, is utmostly protected.
Description
Technical field
The invention belongs to the biological medicine technology field, be specifically related to the preparation method of a kind of nanometer periplaneta americana.
Background technology
In the production and preparation process of Chinese medicine preparation, how the medicinal ingredient with (particularly animal drug) in the medical material fully and to greatest extent extracts, and Chinese medicine is extracted, and is refining, is a constantly problem of research to the trace future development.Ubiquity is inadequate to the degree of grinding of raw medicinal material, affects result of use.Often in order to enhance product performance, dosage uses all bigger than normal, causes use cost higher.The dissolving release of medical material miniaturization and solid drugs, medicine in vivo absorption and bioavailability between substantial connection is arranged.Therefore superfine communication technique is the new technique that a raising medical material utilizes effect.
When the granule of material little during to 1 ~ 100nm because its quantum effect, the locality of material, huge Surface and interface effect can make a lot of performance generation qualitative changes of material.
Medicine some new pharmacodynamic profiles occurred after nanorize is processed.Have great importance for adopting new and high technology to promote the Chinese medicine preparation that the quality of Chinese medicine and level and development have new drug effect.
It is documented that periplaneta americana is the insecticide of volume maximum in the Blattidae, originates in South America, all there is distribution China various places, and are especially more common with the south China area.Periplaneta americana is traditional Chinese crude drug, is used as medicine with dry and bright adult, and its salty in the mouth cold in nature has acid, and the effects such as dissipating blood stasis, removing food stagnancy, detoxifcation, diuretic, detumescence are arranged; Curing mainly infantile malnutrition, tonsillitis, health enclosed mass, carbuncle skin ulcer swells and ache and Scolopendra, venom etc.
Along with science and technology constantly develops, after years of research and found that in recent years the periplaneta americana epidermis contains the elements such as sclerotin and chitin, bromine, zinc, nickel, violent, potassium, calcium, titanium, chlorine, sulfur, silicon, aluminum, magnesium.Muscle is hydrolyzed 13 seed amino acids.In addition, health is preserved the plain B1 of little life, vitamin B2, nicotinic acid and ascorbic acid etc., and lymph contains trehalose, trehalase, glycoprotein, inositol, protocatechuic acid Fructus Vitis viniferae glycoside etc.All contain ergothioneine, 1-methyl-2-pyridinium carboxylate, trigonelline, glycine, betanin, anus alkali, trimethylamine, adenine etc.The pharmacological action of periplaneta americana is mainly manifested in antitumor action, improves immunization, hepatoprotective effect, the effect of promotion tissue repair, antiinflammatory and analgesic activity etc.
At present, the preparation method of American-cockroach-extract has a variety of, really rarely has report and can reach nanometer scale, in conjunction with top described, preparing nano level periplaneta americana and have far reaching significance, also will be one of important directions that periplaneta americana is furtherd investigate.
Summary of the invention
The object of the invention is to for above-mentioned the deficiencies in the prior art, a kind of preparation method for preparing the nanometer periplaneta americana of nanometer particle size 0 ~ 100nm is provided.
The technical scheme that the present invention takes is: the preparation method of a kind of nanometer periplaneta americana is provided, may further comprise the steps:
A, immersion: the dry polypide of periplaneta americana is placed multi-function extractor, add the water of 3 ~ 8 times of the dry body weights of periplaneta americana, under 70 ~ 78 ℃ temperature conditions, soaked 0.5 ~ 3 hour;
B, defat: the alkali liquor that adds soak weight 1/200 ~ 1/1000 in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat;
C, heating: airtight multi-function extractor, boil 30 ~ 60min;
D, flushing: when the pressure in the multi-function extractor rose to 0.08 ~ 0.18Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4 ~ 8;
E, extraction: the solution in the multi-function extractor that step D is obtained carries out 2 ~ 4 times and extracts, and each extraction time is 3 ~ 9 hours;
F, for the first time filtration: the extracting solution that extracts in the step e is merged mixing, then filter and make one-level filtrate;
G, concentrated: relative density was 1.00 ~ 1.25 concentrated solution when one-level filtrate was concentrated into 70 ℃ ~ 90 ℃;
H, the second time filter: after concentrated solution was discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate;
I, supersonic jet drying: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 30 ~ 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 330 ~ 990m/s.
The preparation method of above-mentioned nanometer periplaneta americana in preferred embodiment, may further comprise the steps:
A, immersion: the dry polypide of periplaneta americana is placed multi-function extractor, add the water of 3 ~ 6 times of the dry body weights of periplaneta americana, under 70 ~ 78 ℃ temperature conditions, soaked 0.5 ~ 2 hour;
B, defat: the NaOH that adds soak weight 1/300 ~ 1/1000 in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat;
C, heating: airtight multi-function extractor, open jacket steam and straight gas and jointly heat, boil 30 ~ 60min;
D, flushing: when the pressure in the multi-function extractor rose to 0.11 ~ 0.12Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4 ~ 8;
E, three times extract: the solution in the multi-function extractor that step D is obtained carries out extraction first time, and extraction time is 7 ~ 9 hours; Then carry out the second time behind the water of 2 ~ 4 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 5 ~ 7 hours; Extract for the third time behind the water of 2 ~ 4 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 3 ~ 5 hours;
F, for the first time filtration: the extracting solution that three times are extracted in the step e is merged mixing, then filter and make one-level filtrate;
G, concentrated: relative density was 1.05 ~ 1.25 concentrated solution when one-level filtrate was concentrated into 70 ℃ ~ 90 ℃;
H, the second time filter: after concentrated solution was discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate;
I, supersonic jet drying: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 30 ~ 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 330 ~ 990m/s.
Preferred, the dry polypide of the periplaneta americana of adopting in the steps A and water weight ratio are 1:6.
Preferred, in the steps A, the time of soaking the dry polypide of periplaneta americana in water is 2 hours.
Preferred, among the step B, the NaOH that adds soak weight 1/300 in the soak of the dry polypide of periplaneta americana and water carries out defat.
Preferred, among the step C, airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 60 minutes.
Preferred, among the step D purging method for when the pressure in the multi-function extractor rises to 0.11 ~ 0.12Mpa, repeatedly add the water flushing extremely in the multi-functional extraction pot pH value of solution be 8.
Preferred, three extracting method in the step e extract for the solution in the multi-function extractor being carried out the first time, and extraction time is 9 hours; Then carry out the second time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 7 hours; Extract for the third time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 5 hours.
Preferred, relative density is 1.05 concentrated solution when among the step G one-level filtrate being concentrated into 70 ℃ ~ 90 ℃.
Preferred, the supersonic jet drying means among the step I is: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 990m/s.
The purity of the NaOH that the present invention adopts is analytical pure; The water that the present invention adopts is pure water.
The nanometer periplaneta americana that obtains by preparation method provided by the invention adds pharmaceutically acceptable adjuvant or complementary composition is made the dosage form that is more suitable for clinical practice, such as pill, powder, tablet, suppository, granule, membrane, capsule, microcapsule, drop pill, aerosol, injection, unguentum or oral solution; The pharmaceutical composition of above-mentioned dosage form is mainly used in promoting blood circulation to remove blood stasis, sharp infantile malnutrition, inducing diuresis to remove edema detoxify; Use in WEIJIA and gather, infantile malnutrition, beriberi edema, furuncle, toxic swelling and snake bite and insect sting, wound repair, primary hepatocarcinoma etc.
The nanometer periplaneta americana that obtains by preparation method provided by the invention has following beneficial effect:
1, granule is tiny, even, and good dispersion, particle diameter are 0 ~ 100nm;
2, can improve or improve dissolubility and the biological effectiveness of periplaneta americana medicinal component;
3, be convenient to make slow releasing agent or controlled release preparation;
4, be convenient to target administration, different according to the physiology enzyme of different parts in the body and antibacterial distribution, cell distribution, network structure, lymph distribution etc., adopt different macromolecular materials to carry out finishing, make the periplaneta americana nano-particle that needs, the periplaneta americana medicinal component can be transported to the target area of appointment, reach the purpose of target administration;
5, have safety, reduce some to the stimulation of gastrointestinal;
6, protect to greatest extent the special biological activity of periplaneta americana, such as alanine etc.
The specific embodiment
Below in conjunction with embodiment the present invention is described in detail, but they are not to further restriction of the present invention.
Embodiment 1: the dry polypide of 100Kg periplaneta americana is placed multi-function extractor, add the water of 300Kg, soaked 0.5 hour under 70 ~ 78 ℃ temperature conditions; The NaOH that adds 0.5Kg in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat; Airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 30min; When the pressure in the multi-function extractor rose to 0.08 ~ 0.18Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4; Extract twice, extracted 7 hours for the first time; Then carry out the second time behind the water of 2 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 5 hours; The extracting solution of extracted twice is merged mixing, then filter and make one-level filtrate; Relative density was 1.25 concentrated solution when one-level filtrate was concentrated into 70 ℃; After concentrated solution discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate; Secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 30 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 330m/s.
The nanometer periplaneta americana particle diameter that present embodiment obtains is at 0 ~ 100nm, and body surface area is large, and the atom number ratio of grain boundaries is up to 15 ~ 50%; After testing, contain total amino acids with alanine (C in the dry product of this periplaneta americana nanometer extract
3H
7NO
2) count the 12.0%(mass percent).
Embodiment 2: the dry polypide of 100Kg periplaneta americana is placed multi-function extractor, add the water of 400Kg, soaked 1.5 hours under 70 ~ 78 ℃ temperature conditions; The NaOH that adds 2.5Kg in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat; Airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 40min; When the pressure in the multi-function extractor rose to 0.08 ~ 0.18Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 8; Extract four times, extracted 3 hours for the first time; Then carry out the second time behind the water of 3 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 6 hours; Extract for the third time behind the water of 3 times of amounts of liquid more than adding in the remaining liquid after extracting to the second time again, extraction time is 5 hours; Extract for the third time behind the water of 3 times of amounts of liquid more than adding in the remaining liquid after the most backward for the third time extraction, extraction time is 4 hours; The extracting solution of four extractions is merged mixing, then filter and make one-level filtrate; Relative density was 1.00 concentrated solution when one-level filtrate was concentrated into 80 ℃; After concentrated solution discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate; Secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 45 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 550m/s.
The nanometer periplaneta americana particle diameter that present embodiment obtains is at 0 ~ 100nm, and body surface area is large, and the atom number ratio of grain boundaries is up to 15 ~ 50%; After testing, contain total amino acids with alanine (C in the dry product of this periplaneta americana nanometer extract
3H
7NO
2) count the 13.0%(mass percent).
Embodiment 3: the dry polypide of 100Kg periplaneta americana is placed multi-function extractor, add the water of 800Kg, soaked 3 hours under 70 ~ 78 ℃ temperature conditions; The NaOH that adds 0.9Kg in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat; Airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 50min; When the pressure in the multi-function extractor rose to 0.11 ~ 0.12Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4; Extract three times, extracted 8 hours for the first time; Then carry out the second time behind the water of 3 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 6 hours; Extract for the third time behind the water of 3 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 4 hours; The extracting solution of three extractions is merged mixing, then filter and make one-level filtrate; Relative density was 1.15 concentrated solution when one-level filtrate was concentrated into 80 ℃; After concentrated solution discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate; Secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 55 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 770m/s.
The nanometer periplaneta americana particle diameter that present embodiment obtains is at 0 ~ 100nm, and body surface area is large, and the atom number ratio of grain boundaries is up to 15 ~ 50%; After testing, contain total amino acids with alanine (C in the dry product of this periplaneta americana nanometer extract
3H
7NO
2) count the 14.5%(mass percent).
Embodiment 4: the dry polypide of 100Kg periplaneta americana is placed multi-function extractor, add the water of 600Kg, soaked 2 hours under 70 ~ 78 ℃ temperature conditions; The NaOH that adds 2.33Kg in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat; Airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 60min; When the pressure in the multi-function extractor rose to 0.11 ~ 0.12Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 8; Extract three times, extracted 9 hours for the first time; Then carry out the second time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 7 hours; Extract for the third time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 5 hours; The extracting solution of three extractions is merged mixing, then filter and make one-level filtrate; Relative density was 1.05 concentrated solution when one-level filtrate was concentrated into 90 ℃; After concentrated solution discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate; Secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 990m/s.
The nanometer periplaneta americana particle diameter that present embodiment obtains is at 0 ~ 100nm, and body surface area is large, and the atom number ratio of grain boundaries is up to 15 ~ 50%; After testing, contain total amino acids with alanine (C in the dry product of this periplaneta americana nanometer extract
3H
7NO
2) count the 15.0%(mass percent).
Reference embodiment 1
The preparation of American-cockroach-extract preparation:
A, coarse crushing: the periplaneta americana of drying is pulverized, make the periplaneta americana coarse powder, for subsequent use;
B, immersion: add the water of 3 ~ 5 times of amounts according to the coarse powder of every 100kg, under 70 ~ 78 ℃ temperature conditions, soak and made the coarse powder mixed liquor in 0.5 ~ 2 hour, for subsequent use;
C, three extractions: the coarse powder mixed liquor adopts the method that decocts to carry out three times and extracts, and when the coarse powder mixed liquor was carried out extracting the first time, extraction time was 7 ~ 9 hours; Then carry out extraction second time after adding the water of remaining 2 ~ 4 times of amounts of liquid in the remaining liquid after extracting for the first time, extraction time is 5 ~ 7 hours; Extract for the third time behind the water of 2 ~ 4 times of amounts of liquid more than adding in the most backward remaining liquid after extracting for the second time, extraction time is 3 ~ 5 hours, makes respectively three times extracting solution, and is for subsequent use;
D, for the first time filtration: three times extracting solution are merged mixing, then filter and make one-level filtrate, for subsequent use;
E, concentrated for the first time: relative density was 1.05 ~ 1.25 one-level concentrated solution when one-level filtrate was concentrated into 70 ~ 90 ℃, and is for subsequent use;
F, alcoholization are processed: add gradually the ethanol that concentration is 93 ~ 97%w/w in the one-level concentrated solution, and fully stir, make it contain the alcohol amount and reach till 45 ~ 55%, under 70 ~ 90 ℃ temperature conditions, be incubated 20 ~ 40 minutes, then left standstill 10 ~ 14 hours, and made solution of alcoholized, for subsequent use;
G, for the second time filtration: solution of alcoholized is discarded the upper strata oils and fats, and lower floor's medicinal liquid filters and makes secondary filtrate, and is for subsequent use;
H, the second time concentrate: after secondary filtrate was carried out the ethanol recycling, relative density is 1.15 ~ 1.30 secondary concentrated solution when being concentrated into 70 ~ 90 ℃, and was for subsequent use;
The preparation of i, unguentum: the secondary concentrated solution is concentrated into the unguentum of moisture≤25 ~ 35% under condition of normal pressure, namely gets American-cockroach-extract-containing, for subsequent use;
Patent medicine: according to effective ingredient mixture (American-cockroach-extract): the weight ratio of purified water: glycerol=1000g:800 ~ 1200ml:4 ~ 6ml adds purified water and glycerol in the effective ingredient mixture, stir, through plate-and-frame filtration, after filtrate is boiled 30 minutes, be distributed into 100ml/ bottle or 50ml/ bottle, through the autoclave sterilization sterilization, be chilled to room temperature again, namely get patent medicine.
Test example:
Take the nanometer periplaneta americana of preparation method provided by the invention preparation as active component, add pharmaceutically acceptable adjuvant or complementary composition is made the pharmaceutical composition that is used for the treatment of the dissipating blood stasis for subsidence of swelling disease, can make the various ways such as powder, unguentum, tablet, capsule, to satisfy different patients' medication custom
Take the nanometer periplaneta americana of embodiment 1 ~ 4 preparation as powder.
Above-mentioned powder is used for the treatment of the clinical testing data of dissipating blood stasis for subsidence of swelling disease:
One, patient's classified data:
Detumescence hemostasis patient (comprising that recurrence behind the Surgical Resection of Hepatic Carcinoma or transfer and underwent operative treatment need the patient of wound repair) 150 examples meet diagnostic criteria.Be divided into immediately treatment group and matched group, treatment group 100 examples, male's 55 examples, women's 45 examples, 16 ~ 40 years old age; Matched group 50 examples, male's 26 examples, women's 24 examples, 16 ~ 40 years old age.Two groups of patient ages, sex and courses of disease are learned processing by statistics, and no significant difference has comparability.
Two, Therapeutic Method:
Treatment group 1 ~ 4: get the nanometer periplaneta americana powder that makes according to preparation method among the embodiment 1,2,3,4, as treatment group 1,2,3,4.Oral, a 2-5g; 3 times on the one; Took continuously 1 month;
Matched group 1: YUNNAN BAIYAO DING, Yunnan Paiyao Group Corp., Ltd produces, and is oral, a 3 ~ 5ml, 3 times on the one; Took continuously 1 month.
Matched group 2: the American-cockroach-extract preparation, oral according to the method preparation of reference embodiment 1, a 10ml, 3 times on the one; Took continuously 1 month.
Three, curative effect comparative result:
Table 1 is depicted as six groups in the curative effects comparison of passing through after taking 1 month, treats 4 groups, contrasts 2 groups, and table 2 is depicted as six groups 15 days and curative effect comparison (n number of delegates in table 1 and the table 2) in 1 month.
Judging quota:
Cure: the postoperative wound surface peripheral edema alleviates at the appointed time or disappears, and wound surface is checked through antibacterial culturing, without infecting avirulence, anaphylaxis and other untoward reaction, pain relief or disappearance.
Effectively: the pain that reduces dressing change frequency and cause; Shorten wound surface complete repair time, wound pain alleviates, and edema alleviates.
Invalid: postoperative pain increases the weight of or is unchanged, and wound surface fails to stop blooding, and develops complications.
Total effective rate: refer to cure rate and effective percentage sum.
Table 1:
Table 2:
| Group | n | 15 days total effective rates (%) | 1 month total effective rate (%) |
| Treatment group 1 | 25 | 32.0 | 88.0 |
| Treatment group 2 | 25 | 34.0 | 88.0 |
| Treatment group 3 | 25 | 36.0 | 92.0 |
| Treatment group 4 | 25 | 40.0 | 96.0 |
| Matched group 1 | 25 | 28.0 | 84.0 |
| Matched group 2 | 25 | 30.0 | 84.0 |
Four, conclusion (of pressure testing):
Table 1 is depicted as six groups of curative effects relatively, treatment group 100 examples wherein, and total effective rate is respectively 88.0%, 88.0%, 92.0%, 96.0%, matched group 100 examples, total effective rate is respectively 84.0%, 84.0%; Treatment group all is better than matched group.15 days total effective rates are respectively 32.0%, 34.0%, 36.0%, 40.0%, 28.0%, 30.0% shown in the table 2, and the treatment group curative effect all obviously is better than matched group.This shows that the nanometer periplaneta americana is that the pharmaceutical composition of active component and traditional handicraft and conventional medicament method are compared, and can bring into play to a greater extent curative effect of medication, obtains desirable therapeutic effect.
Pharmaceutical composition take the nanometer periplaneta americana as active component provided by the invention, it is little to have improved cell wall breaking rate, specific surface area, molecular weight, can directly act on focus, significantly improve dissolution rate and body internal absorption factor and the bioavailability of its active component, after desmopyknosis the wound repair time, alleviate alleviating pain, detumescence is played positive therapeutic effect aspect the hemostasis.Reduce simultaneously dosage, reduce the Autoscreen II untoward reaction, the clinic recommendation.
Claims (10)
1. the preparation method of a nanometer periplaneta americana is characterized in that may further comprise the steps:
A, immersion: the dry polypide of periplaneta americana is placed multi-function extractor, add the water of 3 ~ 8 times of the dry body weights of periplaneta americana, under 70 ~ 78 ℃ temperature conditions, soaked 0.5 ~ 3 hour;
B, defat: the alkali liquor that adds soak weight 1/200 ~ 1/1000 in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat;
C, heating: airtight multi-function extractor, boil 30 ~ 60min;
D, flushing: when the pressure in the multi-function extractor rose to 0.08 ~ 0.18Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4 ~ 8;
E, extraction: the solution in the multi-function extractor that step D is obtained carries out 2 ~ 4 times and extracts, and each extraction time is 3 ~ 9 hours;
F, for the first time filtration: the extracting solution that extracts in the step e is merged mixing, then filter and make one-level filtrate;
G, concentrated: relative density was 1.00 ~ 1.25 concentrated solution when one-level filtrate was concentrated into 70 ℃ ~ 90 ℃;
H, the second time filter: after concentrated solution was discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate;
I, supersonic jet drying: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 30 ~ 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 330 ~ 990m/s.
2. the preparation method of a nanometer periplaneta americana is characterized in that may further comprise the steps:
A, immersion: the dry polypide of periplaneta americana is placed multi-function extractor, add the water of 3 ~ 6 times of the dry body weights of periplaneta americana, under 70 ~ 78 ℃ temperature conditions, soaked 0.5 ~ 2 hour;
B, defat: the NaOH that adds soak weight 1/300 ~ 1/1000 in the soak of the dry polypide of above-mentioned periplaneta americana and water carries out defat;
C, heating: airtight multi-function extractor, boil 30 ~ 60min;
D, flushing: when the pressure in the multi-function extractor rose to 0.11 ~ 0.12Mpa, repeatedly adding the water flushing pH value of solution to the multi-functional extraction pot was 4 ~ 8;
E, three times extract: the solution in the multi-function extractor that step D is obtained carries out extraction first time, and extraction time is 7 ~ 9 hours; Then carry out the second time behind the water of 2 ~ 4 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 5 ~ 7 hours; Extract for the third time behind the water of 2 ~ 4 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 3 ~ 5 hours;
F, for the first time filtration: the extracting solution that three times are extracted in the step e is merged mixing, then filter and make one-level filtrate;
G, concentrated: relative density was 1.05 ~ 1.25 concentrated solution when one-level filtrate was concentrated into 70 ℃ ~ 90 ℃;
H, the second time filter: after concentrated solution was discarded the upper strata oils and fats, lower floor's medicinal liquid filtered to get secondary filtrate;
I, supersonic jet drying: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 30 ~ 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 330 ~ 990m/s.
3. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: the dry polypide of the periplaneta americana of adopting in the steps A and water weight ratio are 1:6.
4. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: in the steps A, the time of soaking the dry polypide of periplaneta americana in water is 2 hours.
5. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: among the step B, the NaOH that adds soak weight 1/300 in the soak of the dry polypide of periplaneta americana and water carries out defat.
6. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: among the step C, airtight multi-function extractor is opened jacket steam and straight gas and is jointly heated, and boils 60 minutes.
7. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: among the step D purging method for when the pressure in the multi-function extractor rises to 0.11 ~ 0.12Mpa, repeatedly add the water flushing extremely in the multi-functional extraction pot pH value of solution be 8.
8. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: three extracting method in the step e are for carrying out extraction first time to the solution in the multi-function extractor, extraction time is 9 hours; Then carry out the second time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extracting to the first time and extract, extraction time is 7 hours; Extract for the third time behind the water of 4 times of amounts of liquid more than adding in the remaining liquid after extract the most backward second time, extraction time is 5 hours.
9. the preparation method of nanometer periplaneta americana according to claim 2 is characterized in that: relative density is 1.05 concentrated solution when among the step G one-level filtrate being concentrated into 70 ℃ ~ 90 ℃.
10. the preparation method of nanometer periplaneta americana according to claim 2, it is characterized in that: the supersonic jet drying means among the step I is: secondary filtrate is placed spray drying tower, adopt the Supersonic fluidics at 70 ℃, be drying to obtain the nanometer periplaneta americana under pressure 0 ~ 0.05Mpa; Supersonic jet speed is 990m/s.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103222988A (en) * | 2013-01-15 | 2013-07-31 | 四川好医生攀西药业有限责任公司 | Periplaneta americana extract and its preparation method and use |
| CN107367557A (en) * | 2017-07-05 | 2017-11-21 | 四川好医生攀西药业有限责任公司 | A kind of UPLC assay methods of blattaria protocatechuic acid content |
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| CN1723991A (en) * | 2005-07-15 | 2006-01-25 | 余内逊 | Method for preparing strengthening Yang and eliminating fatigue oral liquor contg. nanometer pilose antler and micron powder of semen juglandis, pine pollen and ants etc. |
| CN101837018A (en) * | 2010-05-25 | 2010-09-22 | 耿福能 | American cockroach medicinal composition for curing ulcers or ulcerative inflammation and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1723991A (en) * | 2005-07-15 | 2006-01-25 | 余内逊 | Method for preparing strengthening Yang and eliminating fatigue oral liquor contg. nanometer pilose antler and micron powder of semen juglandis, pine pollen and ants etc. |
| CN101837018A (en) * | 2010-05-25 | 2010-09-22 | 耿福能 | American cockroach medicinal composition for curing ulcers or ulcerative inflammation and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103222988A (en) * | 2013-01-15 | 2013-07-31 | 四川好医生攀西药业有限责任公司 | Periplaneta americana extract and its preparation method and use |
| CN103222988B (en) * | 2013-01-15 | 2015-10-28 | 四川好医生攀西药业有限责任公司 | A kind of American-cockroach-extract and its preparation method and application |
| CN107367557A (en) * | 2017-07-05 | 2017-11-21 | 四川好医生攀西药业有限责任公司 | A kind of UPLC assay methods of blattaria protocatechuic acid content |
| CN107367557B (en) * | 2017-07-05 | 2020-04-21 | 四川好医生攀西药业有限责任公司 | UPLC (ultra Performance liquid chromatography) determination method for protocatechuic acid content in cockroach |
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