CN104415058B - The supercritical extraction method of American cockroach grease and the preparation of degreasing American cockroach - Google Patents

The supercritical extraction method of American cockroach grease and the preparation of degreasing American cockroach Download PDF

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CN104415058B
CN104415058B CN201410403971.0A CN201410403971A CN104415058B CN 104415058 B CN104415058 B CN 104415058B CN 201410403971 A CN201410403971 A CN 201410403971A CN 104415058 B CN104415058 B CN 104415058B
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american cockroach
degreasing
extraction
preparation
supercritical
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CN104415058A (en
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苏柘僮
熊永爱
邹俊波
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Sichuan Good Doctor Panxi Pharmaceutical Co., Ltd.
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CHENGDU BAICAO HEJI TECHNOLOGY Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/56Materials from animals other than mammals
    • A61K35/63Arthropods
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Insects & Arthropods (AREA)
  • Engineering & Computer Science (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
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Abstract

The present invention provides the preparation method of degreasing American cockroach, it is by American cockroach medicinal material, crushes, is placed in supercritical CO2Extracted in extraction equipment, collect grease and the dregs of a decoction respectively, slag of getting it filled is up to degreasing American cockroach.Present invention research shows that degreasing American cockroach medicinal material prepared by the present invention significantly reduces side effect during gastric ulcer treatment, and new selection is provided for clinical application.Meanwhile the method for the present invention degreasing rate is high, and it is easy to operate, quick, suitable for industrialized production.

Description

The supercritical extraction method of American cockroach grease and the preparation of degreasing American cockroach
Technical field
The present invention relates to the extracting method of American cockroach grease and the preparation of degreasing American cockroach.
Background technology
American cockroach (PeriplanetaAmericana) belongs to Insecta, and Blattaria, Blattidae, " cockroach " is its popular name, Head is seen《A Supplement to the Compendium of Materia Medica》, also referred to as stone ginger, sliding worm survived 3.5 hundred million years on earth, is life in the world Power is most strong, it is most ancient, multiply one of most successful insect assembly so far.The medicinal Zhu Disorder lumps in the abdomen of American cockroach, broken accumulation, tonneau blood Arteries and veins, external application can sore, draw out pus by applying a plaster to the affected part, change rotten, myogenic, modern research shows that it also has good antibacterial action.
Kangfuxin Liquid main component dries the ethanol extract of polypide for American cockroach, and function is promoting blood circulation, nourishing yin and promoting granulation, Modern medicine think Kangfuxin Liquid have promote granulation tissue growth, anti-inflammatory and eliminate inflammatory edema, improve body's immunity, The pharmacological actions such as gastric acid secretion inhibiting, are clinically used for the treatment of duodenal ulcer, gastric ulcer, burn and scald etc..
The pre-treatment to American cockroach medicinal material also rarely has research at present.
The content of the invention
It is an object of the invention to provide the extracting method of American cockroach grease and the preparation of degreasing American cockroach.
The present invention provides the extracting method of American cockroach grease, it includes following operating procedure:
American cockroach medicinal material is taken, crushes, is placed in supercritical CO2Extracted in extraction equipment, collect grease to obtain the final product.
Further, the supercritical CO2The condition of extraction is:20~40MPa of pressure, 30~50 DEG C of temperature, CO2Flow 10~30L/h, when extraction 1~3 is small.
Preferably, the supercritical CO2The condition of extraction is:Pressure 30MPa, 40 DEG C of temperature, CO2Flow 20L/h, extraction 2 Hour.
Wherein, the American cockroach medicinal material be by live body American cockroach after the execution that suffocates or shock by electricity, clean, be dried to obtain Medicinal material.
Present invention also offers the preparation method of degreasing American cockroach medicinal material, American cockroach medicinal material is taken, according to claim 1 After~3 any one the methods extraction grease, the dregs of a decoction are collected, up to degreasing American cockroach.
Present invention also offers degreasing American cockroach prepared by the above method.
Present invention also offers the use of degreasing American cockroach or its extract in the medicine for preparing treatment peptic ulcer On the way.
Further, the extract is water or ethanol extract.
Wherein, the concentration of alcohol is 50~95%v/v.
Further, the concentration of alcohol is 70~80%v/v.
Preferably, the concentration of alcohol is 75~80%v/v.
Present invention research shows that degreasing American cockroach medicinal material prepared by the present invention significantly reduces pair during gastric ulcer treatment Effect, new selection is provided for clinical application.Meanwhile the method for the present invention degreasing rate is high, and it is easy to operate, quick, it is suitable for Industrialized production.
Embodiment
The extraction of 1 American cockroach grease of embodiment
American cockroach pulverizing medicinal materials weigh 250g coarse powder, are placed in supercritical CO into coarse powder2In extraction equipment, in pressure 30MPa, 40 DEG C of temperature, CO2When extraction 2 is small in the state of flow 20L/h, collect American cockroach grease to obtain the final product.
The extraction of 2 American cockroach grease of embodiment
American cockroach pulverizing medicinal materials weigh 250g coarse powder, are placed in supercritical CO into coarse powder2In extraction equipment, in pressure 20MPa, 30 DEG C of temperature, CO2When extraction 1 is small in the state of flow 10L/h, collect American cockroach grease to obtain the final product.
The extraction of 3 American cockroach grease of embodiment
American cockroach pulverizing medicinal materials weigh 250g coarse powder, are placed in supercritical CO into coarse powder2In extraction equipment, in pressure 40MPa, temperature 50 C, CO2When extraction 3 is small in the state of flow 30L/h, collect American cockroach grease to obtain the final product.
Using American cockroach oil yield as evaluation index, to the pressure, temperature, CO of supercritical fluid extraction2Flow and carry The time is taken to be investigated, it is as a result as follows:
According to upper table, the present invention uses supercritical extraction method, can effectively extract American cockroach grease, wherein, It is optimal with the operating condition recovery rate of embodiment 2.
The preparation of 4 degreasing American cockroach of embodiment
American cockroach pulverizing medicinal materials weigh 250g coarse powder, are placed in supercritical CO into coarse powder2In extraction equipment, in pressure 30MPa, 40 DEG C of temperature, CO2When extraction 2 is small in the state of flow 20L/h, collect the dregs of a decoction, to obtain the final product.
The American cockroach medicinal material that the present invention uses, is removal of impurities, drying by live body American cockroach after the execution that suffocates or shock by electricity Obtain.
The preparation of 5 degreasing American cockroach Ultramicro-powder of embodiment
Degreasing American cockroach 100kg is weighed, is placed in sterilizing combination drying all-in-one machine, adds 75% ethanol 20L, 40~ When 60 DEG C of sterilizings 1~2 are small, ethanol is recycled, 40~60 DEG C are dried under vacuum to moisture≤6%, through efficient universal pulverizer 4000 ~5000rpm/min is crushed, and powder is with ultra micro vibromill in amplitude 5mm, 0~10 DEG C of operating temperature, crushing 20min, system Into 10~50 μm of particle.The specific surface area increase of American cockroach Ultramicro-powder, dissolution rate and the stripping quantity increase of active principle, Improve curative effect or reduce the dosage of the product, bioavilability greatly improves, and medical value is greatly enhanced, can conduct Bulk pharmaceutical chemicals are applied to powder, pill, tablet, suppository, granule, film, capsule, microcapsules, pill, aerosol, injection Agent, paste, vina, syrup or oral solution.
The preparation of 6 degreasing American cockroach nano powder of embodiment
Degreasing American cockroach 100kg is weighed, is crushed through efficient universal pulverizer in 4000~5000rpm/min, powder adds 3 ~10 times of water are made into suspension, are ground 1~2 time with colloid mill, then through superhigh-voltage homogenizing machine in 100~180MPa of pressure into horizontal high voltage Homogeneous, 40~80 DEG C of spray drying of homogenizing fluid, is made the degreasing American cockroach nano powder that particle diameter is less than 100nm.American cockroach receives The specific surface area of rice flour substantially increases, and the dissolution rate and stripping quantity of active principle greatly increase, and improve curative effect or reduce The dosage of the product, bioavilability greatly improve, and medical value is greatly enhanced, can be used as bulk pharmaceutical chemicals be applied to powder, Pill, tablet, suppository, granule, film, capsule, microcapsules, pill, aerosol, injection, paste, vina, syrup Agent or oral solution.
The preparation of 7 degreasing American cockroach alcohol extract of embodiment
Degreasing American cockroach 100kg is weighed, coarse powder is ground into, is placed in multi-function extractor, adds 8 times of 80% ethanol, is returned When stream extraction 4.5 is small, filtering, add 10~20 times of water to stir evenly, stand, be cooled to room temperature, filter, be concentrated under reduced pressure into density 1.1 American-cockroach-extract is made in~1.3,40~80 DEG C of spray drying.The invention has the characteristics that method is simple, easy to operate.The production Product active constituent content is high, easily absorbs, long shelf-life, has and improves immunization, hepatoprotective effect, promotes tissue repair effect. Using extract as active ingredient, add pill made of pharmaceutically acceptable auxiliary material or complementary component, powder, tablet, Suppository, granule, film, capsule, microcapsules, pill, aerosol, injection, paste or oral solution.
The preparation of 8 degreasing American cockroach alcohol extract of embodiment
Degreasing American cockroach 100kg is weighed, fine powder is ground into, is placed in ultrasonic extraction tank, adds 8 times of 80% ethanol, is surpassed When sound extraction 1~2 is small, filtering, 40~60 DEG C are concentrated under reduced pressure into density 1.1~1.3, and 40~60 DEG C of spray drying of concentrate are made American-cockroach-extract.15% (quality percentage is calculated as with alanine (C3H7NO2) containing total amino acid in the dry product of the extract Than).The invention has the characteristics that extraction efficiency is high, extraction time is short, Extracting temperature is low, efficient, energy-saving and environmental protection.The product has Effective component content is high, easily absorbs, long shelf-life, has and improves immunization, hepatoprotective effect, promotes tissue repair effect.To carry It is active ingredient to take thing, add pill made of pharmaceutically acceptable auxiliary material or complementary component, powder, tablet, suppository, Granule, film, capsule, microcapsules, pill, aerosol, injection, paste or oral solution.
Illustrate beneficial effects of the present invention below by way of test example.
The front and rear treatment peptic ulcer drug effect contrast of 1 American cockroach medicinal material degreasing of test example
1 experiment material
1.1 experimental animal
Cleaning grade SD rats, 60, male, weight 180-220g, is provided by Chengdu up to large bio tech ltd.It is dynamic The amount of substance quality certification:SCXK (river) 2008-24.
1.2 test medicine
1. American cockroach medicinal powder:Live body American cockroach removes impurity after the execution that suffocates or shock by electricity, and 60 DEG C dry, Crushed again using high speed disintegrator.
2. American cockroach medicinal powder:Live body American cockroach removes impurity after the execution that suffocates or shock by electricity, and 60 DEG C dry, Then supercritical CO is used2Fluids extraction (embodiment 4), then crushed using high speed disintegrator.
3. Periplaneta Americana powder:Sample preparation methods continue to use commercially available American cockroach fine powder preparation process.
1.3 laboratory apparatus and reagent
▲ electronic balance (Beijing Sai Duolisi balances Co., Ltd, model BS-200S-WEI);
▲ centrifuge (flying pigeon board, model:LXJ-ⅡB);
▲ numerical control ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd., model:KQ-500DB);
The weight calculation of ▲ high-precision electronic claims (Foochow Chen Electronics Co., Ltd.s, model:AWH-30KC);
▲ Rotary Evaporators, condenser pipe, iron stand, round-bottomed flask (1000ml, 2000ml)
▲ other:EP pipe (5ml, 10ml), beaker, graduated cylinder, conical flask, pan paper, operation sewing needle, operation suture thread, Glass bar, cotton swab, gastric perfusion needle, syringe, constant temperature water bath apparatus, rat fixed plate, syringe, needle holder, tweezers number handle, size Operating scissors numbers is appropriate etc., rubber band.
▲ chloraldurate (Chengdu Ke Long chemical reagents factory, product batch number:20100920, specification:250g);
▲ formaldehyde (Chengdu Ke Long chemical reagents factory, product batch number:20120320, specification:500ml);
▲ absolute ethyl alcohol (Chengdu Ke Long chemical reagents factory, product batch number:20110820, specification:500ml);
▲ sodium chloride injection (Kuming Nanjiang Pharmacy Co., Ltd, product batch number:D101211A2, specification:500ml: 4.5g);Distilled water etc..
2 experimental methods
2.1 experiment packets and administration
60 SD rats are divided into 5 groups by weight stochastic averagina:1. sham-operation group (JSS groups):Isometric pure water;2. mould Type group (MD groups):Isometric pure water;3. American cockroach medicinal material group (MZDL groups);4. American cockroach medicinal material de-oiling fat group (TYZ Group).5. American cockroach fine powder group (DLJF groups).Every group of 12 rats, since experimental day, each experimental group medicinal powder, greatly Mouse gives relative medicine or pure water by group, dosage gavage, continuous 7 days.
2.2 fasting
After the last administration, each group rat single cage is raised, and fasting for solids but not liquids 24h (is administered) as usual during fasting.
2.3 model copy
After fasting 24h, each experimental group rat is with 10% chloraldurate solution (dosage:0.3ml/100g) intraperitoneal injection of anesthesia Rat, along ventrimeson under xiphoid-process open abdomen about 2-3cm, at left costal margin position, touched with hand, make gastroduodenal intersection Pylorus be exposed to notch, in addition to blank group, by remaining each group rat stomach pylorus ligation, blank group, which only carries out anesthesia, to be opened abdomen and does evil through another person Art, each group animal sends stomach and 12 rectum back to abdominal cavity original place, so through duodenum final injection to relative medicine after ligation It is layered suturing them notch again afterwards, records the modeling time.
2.4 materials
Postoperative each group rat single cage is raised, and after 18h fasting for solids and liquids, rat is put to death, and opens abdominal cavity, and ligation orifice of the stomach takes out complete Stomach, stomach is immersed in 1% formalin, and fixed 5-10min, then cuts off stomach wall along greater curvature by stomach, clean gastric content, will Stomach wall is unfolded, and tiles on blank sheet of paper, with the naked eye or amplifies sem observation stomach lining face, records number of animals, the ulcer of every group of generation ulcer Area lesion situation.
3 observation indexs
3.1 ulcer inhibition rate
With the area of each ulcer of vernier caliper measurement, ulcer diameter>1mm calculates ulcer area, and area is burst less than 1mm's Ulcer point, 10 equivalent to ulcer area 1mm2.Using the square millimeter number of ulcer area summation as ulcer index, ulcer suppression is calculated Percentage processed.
Ulcer suppresses percentage (%)=(control group ulcer area summation-administration group ulcer area summation)/control group and bursts Ulcer area summation × 100%.
3.2 pathology damage indexes
Pathological score is carried out to gastric tissue microexamination situation, appraisal result is in terms of damage index.
Gastric tissue microexamination standards of grading:0 point:Not damaged or inflammation;1 point:Mild hyperaemia, oedema, surface is smooth, Without rotten to the corn or ulcer;2 points:Congestion and edema, cell infiltration, has rotten to the corn or stomach to be adhered;3 points:Height congestion and edema, surface have bad Dead and ulcer is formed, the maximum vertical footpath of ulcer<There are necrosis and inflammation in 1cm, thickened stomach wall or surface;4 points:Height congestion and edema, sticks Film necrosis and ulcer are formed, the maximum vertical footpath of ulcer>1cm, or full wall stomach necrosis.
4 statistical procedures
Statistical analysis is carried out with 17.0 softwares of SPSS.Data with mean ± standard deviation () represent, use Dan Yin between group Plain variance analysis, LSD inspections are carried out between the neat person's group of variance, and heterogeneity of variance person carries out Tamhane ' s T2 and examines.
5 experimental results
5.1 ulcer inhibition rates compare
It the results are shown in Table 1.
Table 1 to rat gastric ulcer inhibiting rate influence (N=10)
Note:Compared with MD groups,**P<0.01,*P<0.05;Compared with MZDL groups,△△P<0.01,P<0.05;With DLJF groups Compare,▲▲P<0.01,P<0.05。
As shown in Table 1, compared with sham-operation group, model group rats gastric ulcer area pole conspicuousness increase (P<0.01), with Model group compares, and DLJF group rat gastric ulcer areas are substantially reduced (P<0.05), TYZ groups pole is substantially reduced (P<0.01);With MZDL groups compare, and DLJF group rat gastric ulcer areas are substantially reduced (P<0.05), TYZ groups pole is substantially reduced (P<0.01);With DLJF groups compare, and TYZ group rat gastric ulcer areas are substantially reduced (P<0.05).
5.2 gastric tissue pathology damage indexes compare
It the results are shown in Table 2.
2 each group rat stomach Histopathological lesions index of tableN=10)
Note:Compared with MD groups,**P<0.01,*P<0.05;Compared with MZDL groups,△△P<0.01,P<0.05;With DLJF groups Compare,▲▲P<0.01,P<0.05。
As shown in Table 1, compared with sham-operation group, model group rats gastric tissue pathology damage index pole conspicuousness increase (P< 0.01), compared with model group, DLJF group rat stomach Histopathological lesions indexes are substantially reduced (P<0.05), TYZ groups extremely significantly subtract Small (P<0.01);Compared with MZDL groups, DLJF group rat stomach Histopathological lesions indexes are substantially reduced (P<0.05), TYZ groups pole It is substantially reduced (P<0.01);Compared with DLJF groups, TYZ group rat stomach Histopathological lesions indexes are substantially reduced (P<0.05).
6 experiment conclusions
Using CO2Supercritical fluid extraction bursts stomach to can obviously reduce it after the progress de-oiling fat processing of American cockroach medicinal material The toxic side effect of ulcer, and the therapeutic effect to gastric ulcer can be improved.

Claims (7)

  1. A kind of 1. preparation method for the degreasing American cockroach for treating peptic ulcer, it is characterised in that:It is by American cockroach medicine Material, crushes, is placed in supercritical CO2Extracted in extraction equipment, collect grease respectively and the dregs of a decoction, slag of getting it filled are big up to degreasing America Lian;
    The supercritical CO2The condition of extraction is:20 ~ 40MPa of pressure, 30 ~ 50 DEG C of temperature, CO210 ~ 30L/h of flow, extraction 1 ~ 3 Hour.
  2. 2. preparation method according to claim 1, it is characterised in that:The supercritical CO2The condition of extraction is:Pressure 30MPa, 40 DEG C of temperature, CO2Flow 20L/h, when extraction 2 is small.
  3. 3. preparation method according to claim 1, it is characterised in that:The American cockroach medicinal material is by live body American cockroach After the execution that suffocates or shock by electricity, the medicinal material that clean, is dried to obtain.
  4. 4. the preparation-obtained degreasing American cockroach of claim 1 ~ 3 any one the method.
  5. 5. the use of degreasing American cockroach or its extract in the medicine for preparing treatment peptic ulcer described in claim 4 On the way.
  6. 6. purposes according to claim 5, it is characterised in that:The extract is water or ethanol extract.
  7. 7. purposes according to claim 6, it is characterised in that:The concentration of alcohol is 50 ~ 95%v/v.
CN201410403971.0A 2013-08-19 2014-08-15 The supercritical extraction method of American cockroach grease and the preparation of degreasing American cockroach Active CN104415058B (en)

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CN109820873B (en) * 2019-04-17 2023-05-02 云南京新生物科技有限公司 Defatted periplaneta americana and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101116471A (en) * 2006-08-01 2008-02-06 西安市轻工业研究所 Edible insect albumen powder and the production process and application thereof
CN101837144A (en) * 2010-05-25 2010-09-22 耿福能 American-cockroach-extract-containing gelatin sponge and preparation method thereof
CN103239482A (en) * 2013-05-29 2013-08-14 四川好医生攀西药业有限责任公司 Intragastric floating tablet for periplaneta americana as well as preparation method and application of intragastric floating tablet

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101116471A (en) * 2006-08-01 2008-02-06 西安市轻工业研究所 Edible insect albumen powder and the production process and application thereof
CN101837144A (en) * 2010-05-25 2010-09-22 耿福能 American-cockroach-extract-containing gelatin sponge and preparation method thereof
CN103239482A (en) * 2013-05-29 2013-08-14 四川好医生攀西药业有限责任公司 Intragastric floating tablet for periplaneta americana as well as preparation method and application of intragastric floating tablet

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