CN104689296A - Zaocys dhumnades oil product and preparation method thereof - Google Patents
Zaocys dhumnades oil product and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a product which is primarily based on zaocys dhumnades oil and a preparation method thereof. The preparation method comprises the following steps: by taking drug level zaocys dhumnades as a raw material, crushing the raw materials, adding acetone, extracting under nitrogen protection and deodorizing and decoloring through active carbon to obtain refined zaocys dhumnades oil; and adding neutral protease and trypsin into acetone extraction residues for enzymolysis, centrifugalizing after high-temperature treatment, adding ether into a supernate to be precipitated, wherein the precipitate is a small peptide dried object, and mixing with the refined zaocys dhumnades oil to obtain the zaocys dhumnades oil product. The method can effectively prevent damage of linoleic acid and is high in oil yield, shallow in luster, high in transparency, free of precipitate and suspended solids and relatively small in viscosity. The content of linoleic acid can be over 16% and the expiration date of the product is long.
Description
Technical field
The invention belongs to animal oil extraction separation technology field, be specifically related to based on product of dark glaucoma Adeps Serpentis and preparation method thereof.
Background technology
Zaocys dhumnades is commonly called as Zaocys, Zaocys, for Colubridae Zaocys belongs to the larger nonpoisonous snake of the bodily form, is distributed widely in China, lives in hilly country, stenophagy Serpentis class, with batrachia (staple food), Eremiatis argi, Fish, muroid etc. for food.Because habitat destruction and the mankind catch and kill in a large number, current field survivorship quantity subtracts greatly, should protect.Zaocys can be used as medicine.Cure mainly: dispel the wind, dredging collateral, relieving convulsion.For rheumatoid arthritis stubborn, numbness contracture, apoplexy facial hemiparalysis, hemiplegia, tic spasm, tetanus, leprosy scabies, scrofula malignant boil.
Adeps Serpentis contains abundant natural active matter and antipathogenic composition, has superpower penetration, directly can permeate human body skin, promotes skin cell metabolism, strengthens skin immunization regulatory function; Be a kind of not only being rich in nutrition but also be beneficial to the material of health care, China's traditional Chinese medical science or happiness Adeps Serpentis disease-treatment and health-care among the people, have endocrine regulation imbalance, loosening bowel to relieve constipation, skin maintenance, prevents skin aging, prevents sclerosis of blood vessels from having good effect.Adeps Serpentis contains 12 kinds of fatty acids, mainly contains the unsaturated fatty acid such as linoleic acid, linolenic acid and glycerol Palmic acid etc.Wherein maximum unsaturated fatty acids---linoleic acid, the excessive temperature of long period can cause it to be oxidized.
Publication number is that the Chinese patent of CN104027669A discloses a kind of Chinese medicinal formulae for the treatment of wind syndrome of head, it is characterized in that being made up of the raw material of Chinese medicine of following weight proportion: Rhizoma Pinelliae 10-20 part, Rhizoma Gastrodiae 10-20 part, Rhizoma Atractylodis Macrocephalae 10-20 part, Poria 10-30 part, Os Draconis 15-45 part, Concha Ostreae 15-45 part, Radix Puerariae 15-45 part, Rhizoma Alismatis 10-30 part, Semen Coicis 15-45 part, Pericarpium Citri Reticulatae 10-30 part, Zaocys 10-30 part, Radix Clematidis 10-30 part, Radix Salviae Miltiorrhizae 20-40 part, Lignum Dalbergiae Odoriferae 10-30 part, Rhizoma Corydalis 10-30 part, Oletum Trogopterori 10-30 part, Semen Persicae 10-30 part, Flos Carthami 10-30 part, Bombyx Batryticatus 10-30 part.The present invention has vital base and primordial QI consolidating for the treatment of the diseases such as wind-induced headache, dizziness, treating both the principal and secondary aspects of a disease, curative effect are obvious, and has no side effect, controls the advantages such as recurrence rate after healing is low.
Publication number is that the Chinese patent of CN104013867A discloses a kind of Chinese medicine for the treatment of eczema, and it is mainly made up of following Chinese crude drug: Radix Sophorae Flavescentis, Cortex Dictamni, Radix Polygoni Multiflori, Indigo Naturalis, Zaocys, Cortex Phellodendri, the Radix Angelicae Dahuricae, Pollen Typhae, Herba Portulacae, Herba Taraxaci, fresh Rhizoma Phragmitis, Herba Houttuyniae, Semen Coicis, Semen Sinapis Albae, Herba Schizonepetae, Radix Saposhnikoviae, Semen Armeniacae Amarum, Radix Glycyrrhizae.The present invention is intended to the defect making up prior art, provide a kind of curative effect obviously, treating both the principal and secondary aspects of a disease, the Chinese medicine for the treatment of eczema that has no side effect.
Publication number is the compound Chinese medicine external preparation that the Chinese patent of CN103385905A discloses a kind for the treatment of dermatitis and eczema class disease, it is characterized in that being prepared from by by the raw material of following weight percents and pharmaceutically acceptable carrier: Adeps Serpentis 3-15 parts, Radix Arnebiae (Radix Lithospermi) 3-12 parts, Ilex purpurea Hassk.[I.chinensis Sims 10-45 parts.Its dosage form is ointment, Emulsion, liniment, liposome or spray.The present invention is applied to the clinical treatment of dermatitis and eczema class disease, has the effects such as antiinflammatory, antiallergic, antibacterial, moisturizing, and Be very effective.
Publication number is that the Chinese patent of CN103027870A discloses a kind of natural whiting hand cream, it comprises the component of following mass percent: 40-50% glycerol, 5-10% carbamide, 10-15% Dormant oils, 3-9% Fructus Luffae elite, 1-3% isopropyl myristate, 2-6% polydimethylsiloxane, 2-4% Flos Osmanthi Fragrantis extract, 2-8% vaseline, 1-3% Tryfac 5573 potassium, 1-3% cetearyl alcohol, 3-7% Aloe extract, 3-9% snake oil essence, surplus is deionized water.Natural whiting hand cream of the present invention has Fructus Luffae elite whitening elite, and natural whiting has no side effect, and snake oil essence and Aloe extract can effectively be releived chapped skin, skin care, and anti-freezing anti-cracking, this hand cream also has natural Flos Osmanthi Fragrantis fragrance simultaneously.
Publication number is that the Chinese patent of CN102895167A discloses a kind of snake oil hand cream, is specifically related to a kind of snake oil hand cream effectively preventing pachylosis drying, bursting by freezing.The present invention by Adeps Serpentis 20%-30%, glycerol 15%-20%, Flos Matricariae chamomillae essence 1%-3%, Jojoba oil 1%-3%, safflower oil 0.5%-1%, Dormant oils 0.2%-0.5%, cetearyl alcohol 0.2%-0.5%, sorbitol 0.2%-0.5%, sheep placental extract elite 0.2%-0.5%, sodium lauryl sulfate 0.5%-2%, ring is siloxanes 0.2%-0.5%, essence 0.2%-0.5%, all the other are medical ventolin.Multiple moist protection nutritional labeling is rich in the present invention, and reducing the adverse circumstances such as dry, cold to skin surface is injury, promotes skin metabolism speed and improves immunity, recovers and keeps both hands elasticity of skin.
Publication number is that the Chinese patent of CN101537124 discloses a kind of ointment for the treatment of burn, and medicine components is: Borneolum Syntheticum 50-70g, Herba Artemisiae Anomalae 80-100g, Endoconcha Sepiae 80-100g, Calamina (calcined and quenched) 140-160g, Borax 90-110g, Flos Carthami 20-30g, Sanguis Draxonis 30-50g, Cinnabaris 40-50g, Nidus Vespae 20-30g, Pseudobulbus Bletillae (Rhizoma Bletillae) 90-110g, Concha Ostreae 13-150g, Adeps Serpentis 150-200g, vaseline 1800-2200g.First get the pure Chinese medicine of front 12 taste respectively single concoct after smash carefully cross 100 mesh sieves, then Homogeneous phase mixing, then by vaseline fusing boil, Adeps Serpentis and mixed powder are added in vaseline stir evenly respectively, cooling after encapsulation.Ointment of the present invention has quick pain relief, controls wound fluid required time short, and anti-inflammatory effects is obvious, treats easy, and wound surface is rear without advantages such as cicatrixes, and by clinical observation, its therapeutic effect is obviously better than existing treatment burn medicine.
Publication number is that the Chinese patent of CN103610869A discloses a kind of burn cream, the ointment that it is made up of following raw materials according: Flos Carthami, Radix Sanguisorbae, Cacumen Platycladi, Radix Notoginseng, Sanguis Draxonis, Flos Chrysanthemi Indici.Above-mentioned each crude drug is cleaned, dries, bake, be ground into end, after sieving, reconcile into paste by after each crude drug powder mix homogeneously with Rrinaceus earopaeus oil and Adeps Serpentis, namely make burn cream of the present invention.A kind of burn cream provided by the invention and preparation method thereof, can solve the shortcoming of existing burn class medicine, effectively can treat heat injury, chemical burn, radiation burn and physical property burn; Manufacturing process is simple, safe and reliable.
Publication number is that the Chinese patent of CN103638307A discloses a kind of Adeps Serpentis moist expose burn ointment, is made up of Adeps Serpentis, Rhizoma Polygoni Cuspidati, Cortex Phellodendri, Endothelium Corneum Gigeriae Galli, Pseudobulbus Bletillae (Rhizoma Bletillae), Radix Sanguisorbae, Camphora, vaseline 8 kinds of raw materials.It integrates Adeps Serpentis, Rhizoma Polygoni Cuspidati, Cortex Phellodendri, Endothelium Corneum Gigeriae Galli, Pseudobulbus Bletillae (Rhizoma Bletillae), Radix Sanguisorbae, Camphora, cures fast to empyrosis wound surface, does not need the crust skin-grafting that disappears, preventing from scar after curing, has heat clearing away, removing toxic substances, reducing swelling and alleviating pain, convergence granulation promoting, easy to use, manufacture simple, the feature that medical expense is low.The medication times solving existing treatment burn is long, costly, easily leaves the problem of cicatrix more.For skin frostbite, festering also has special curative effect.
Publication number is that the Chinese patent of CN103735846A discloses a kind of kibe ointment and preparation method thereof, this kibe ointment is formed according to weight proportion configuration by following composition: 25-45 part Radix Angelicae Sinensis, 15-25 part Flos Carthami, 20-30 part Radix Angelicae Dahuricae, 25-35 part Cortex cinnamomi japonici (Ramulus Cinnamomi), 10-20 part Pseudobulbus Bletillae (Rhizoma Bletillae), 20-30 part Aloe gel juice, 5-10 part Cera Flava Oleum Camelliae, 20-30 part Adeps Serpentis, 10-20 part vitamin B3,15-30 part allantoin.Beneficial effect: poisonous side effect of medicine of the present invention is little, wound healing is fast, and antipruritic effect is good, and therapeutic effect is excellent, cheap.
Publication number is that the Chinese patent of CN103393844A discloses a kind of pharmaceutical formulation for the treatment of gastropathy, relate to the pharmaceutical formulation of the treatment gastropathy in medical formulation field, especially a kind for the treatment of time is short, the pharmaceutical formulation of the treatment gastropathy that with low cost and therapeutic effect is good.It is fatty by Naja, Agkistrodon is fatty, Zaocys is fatty and Margarita Oleum Camelliae mixes according to certain refinement mode and certain ratio.This pharmaceutical formulation treatment gastropathy time is very short, can cure about two weeks, and this formula is simple, and cost is very cheap, can save unnecessary expenses to patient; And zest can not be produced to the intestines and stomach on therapeutic effect, do not have other any side effect yet.
Publication number is that the Chinese patent of CN102885875A discloses a kind of pharmaceutical formulation for the treatment of empyrosis, relate to the pharmaceutical formulation of the treatment empyrosis in medical formulation field, especially a kind for the treatment of time is short, the pharmaceutical formulation of the treatment empyrosis that with low cost and therapeutic effect is good.It is fatty by Naja, Agkistrodon is fatty, Zaocys is fatty and Margarita Oleum Camelliae mixes according to certain refinement mode and certain ratio.This pharmaceutical formulation treatment empyrosis time is very short, and wound generally healed in one week, and this formula is simple, and cost is very cheap, can save unnecessary expenses to patient; And can not scar on therapeutic effect, do not have other any side effect yet.
" Zaocys typeⅡ Collagen Isolation and purification and to AA rat intervention effect " documents and materials show, collagen protein be mammal in-vivo content at most, the widest functional protein of distribution, account for 25% ~ 30% of total protein; And experiment shows that Zaocys typeⅡ Collagen is by oral PP cytosis afterwards and in body, produces inhibition inflammatory factor, thus reaches the effect of the inflammation-inhibiting factor.
" Primary Study of collagen oligomeric peptide moisture-keeping crease-shedding efficacy assessments and mechanism thereof " documents and materials show, collagen oligopeptide significantly can increase the water content of keratodermatitis in a short time, improves wrinkle near the eyes, and has the effect of bright color; At cellular level, significantly fibroblast proliferation can be promoted.
Above-mentioned documents and materials show, domestic more to the application of Adeps Serpentis research on utilization, but it is little to the preparation method research of various Adeps Serpentis, traditional method is simply the fat peeled off in Serpentis body, temper in pot and form, temper and unsaturated fatty acid in Adeps Serpentis can be made easily to be oxidized, functional component is destroyed, and drug effect is reduced.Also someone adopts and extracts under ultrasound wave, adopts the method recycling design of distillation, and logical nitrogen, obtain this refining Adeps Serpentis.Although done certain improvement in traditional method, shorten and boiled the time, product quality is had a certain upgrade, shortened the time of Adeps Serpentis high temperature refining, but still do not departed from high temperature and boil this link.In addition, Serpentis collagen protein direct mixing with Adeps Serpentis applies skin, and be difficult to directly to enter skin and absorb, the Adeps Serpentis preparation method tool therefore developing a kind of available protecting Adeps Serpentis functional component is of great significance.
Summary of the invention
Serpentis itself is containing a large amount of unsaturated fatty acid, and energy long-term existence, mainly contain a large amount of antioxidative collagenic protein or little peptide in Serpentis body, fat and protein are all directly first peeled off by existing method, in leaching process, adopt isolation oxygen to slow down unsaturated fatty acids acid oxidase, but main task slows down unsaturated fatty acids acid oxidase in product use procedure, open source literature data cannot reach this purpose at present, in order to overcome above-mentioned deficiency of the prior art, it is high that order of the present invention is just to provide a kind of extraction efficiency, improve the dark glaucoma Adeps Serpentis preparation method of functional component in Adeps Serpentis.
The present invention adopts following technical scheme: with pharmaceutical grade zaocys dhumnades for raw material, shatter, add acetone, nitrogen protection lixiviate, through activated carbon deodorization decolouring, obtain refining dark glaucoma Adeps Serpentis.Acetone extraction residue adds neutral protease respectively and trypsin carries out enzymolysis, and centrifugal after high-temperature process, supernatant adds ether sedimentation, and precipitation is the dry thing of little peptide, is mixed to get zaocys dhumnades oil product with refining dark glaucoma Adeps Serpentis.
Zaocys dhumnades oil product is directly mixed by refining dark glaucoma Adeps Serpentis and the dry thing of little peptide, get the water dissolution of the weight such as the dry thing of a certain amount of little peptide adds again, dissolve after refining dark glaucoma Adeps Serpentis heating 35 ~ 45 DEG C again, little peptide aqueous solution is joined in the Adeps Serpentis after dissolving in proportion, stirs made by final vacuum lyophilization.
In one embodiment, zaocys dhumnades oil product is made up of with following weight portion each raw material composition: the dry thing 0.01 ~ 8 part of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
In a specific embodiment, wherein each material composition forms with following weight portion: the dry thing 0.05 ~ 5 part of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
In a specific embodiment, wherein each material composition forms with following weight portion: the dry thing 0.5 ~ 3 part of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
In a specific embodiment, wherein each material composition forms with following weight portion: make after the dry thing 1 part mixing of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
The preparation method of described refining dark glaucoma Adeps Serpentis and the dry thing of little peptide, its concrete steps are as follows:
(1) shatter: pharmaceutical grade zaocys dhumnades is carried out shattering to 10-20 order, obtains snake powder;
(2) acetone extraction: add acetone to above-mentioned snake powder, in nitrogen protection stirring at room temperature lixiviate twice, each lixiviate 60-90min, obtains lixiviating solution through ceramic membrane filter, merges twice lixiviating solution and obtains acetone filtrate and Serpentis residue;
(3) decoloration and deodorization: add appropriate neutral active carbon granule to acetone filtrate; room temperature decolouring 20-30 minute under nitrogen protection; ceramic membrane filter once; 40 DEG C of concentrating under reduced pressure remove acetone; obtain grease; carry out extracting once with the ethanol of two volumes, obtain ethanolic extract, 40 DEG C of concentrating under reduced pressure are removed ethanol and must be refined dark glaucoma Adeps Serpentis.
(4) enzymolysis: acetone extraction residue adds the water of double weight, adds neutral protease, reaches 5-10U/L to final concentration, constantly stirs, enzymolysis 1h at 30 DEG C, then add trypsin, reach 15-20U/L to final concentration, carry out enzymolysis, constantly stir, enzymolysis 2-4h at 37 DEG C;
(5) little peptide separation and Extraction: after 90-100 DEG C of high-temperature process enzymolysis solution 10-30min, the centrifugal 5min of 6000rpm, supernatant adds two volumes ether and leaves standstill the centrifugal 5min of 5 ~ 20min, 6000rpm, precipitates the dry thing of dry little peptide.
In one embodiment, the consumption of acetone described in step (2), the ratio of its volume L/ snake powder weight kg is 3 ~ 6:1.
In one embodiment, the consumption of neutral active carbon granule described in step (3), the ratio of its weight kg/ snake powder acetone filtrate volume L is 3 ~ 6:50, neutral active carbon granule diameter 0.2-5mm.
In one embodiment, neutral protease described in step (4) and trypsin can commercially, and general neutral protease activity is 500U/kg, and tryptic activity is 300U/kg, and " U " refers to international unit of enzyme activity.
Technique effect
(1) what this method adopted is the pharmaceutical grade zaocys dhumnades be relatively easy to get is raw material, raw material relative abundance.
(2) the protein restriction endonuclease polypeptide chain to Denatured protein is adopted to carry out large fragment enzymolysis, a large amount of small peptide materials can be obtained, for the antioxidant of dark glaucoma Adeps Serpentis and the additive of Adeps Serpentis skin care item, small peptide material is made an addition to the stability that greatly can improve its utilization rate and peptide matters in Adeps Serpentis.
(3) adopt acetone cold-maceration to carry out extraction Adeps Serpentis, effectively avoid linoleic destruction, the snake egg white matter meeting partial denaturation after acetone extraction, is more conducive to the enzymolysis process in later stage, also can prevents direct hydrolysis from becoming single amino acids.
(4) the product oil yield that obtains of the present invention is high, lighter color, and transparency is high, and without precipitation and float, stickiness is less, and linoleic acid content is up to more than 16%, and shelf life of products is long.
Detailed description of the invention
Further illustrate essentiality content of the present invention with embodiment of the present invention below, but do not limit the present invention with this.
Embodiment 1
Pharmaceutical grade zaocys dhumnades 100kg is carried out shattering to 10-20 order, obtains snake powder.The acetone of 200L is added to snake powder; at nitrogen protection stirring at room temperature lixiviate 90min; via hole diameter is that the ceramic membrane filter of 0.22 μm obtains lixiviating solution; the acetone of 200L is added again to the snake powder of extracted; at nitrogen protection stirring at room temperature lixiviate 60min; via hole diameter is that the ceramic membrane filter of 0.22 μm obtains lixiviating solution, merges twice lixiviating solution and obtains acetone filtrate and Serpentis residue.0.5mm neutral active carbon granule 12kg is added to acetone filtrate; room temperature decolouring 20-30 minute under nitrogen protection; ceramic membrane filter once; 40 DEG C of concentrating under reduced pressure remove acetone; obtain grease; carry out extracting once with the ethanol of two volumes, obtain ethanolic extract, 40 DEG C of concentrating under reduced pressure are removed ethanol and must be refined dark glaucoma Adeps Serpentis 12.08kg.
Acetone extraction residue 85kg is added the water of 170kg, add the neutral protease of 5kg, reach 5-10U/L to final concentration, constantly stir, enzymolysis 1h at 30 DEG C, then add 12kg trypsin, reach 15-20U/L to final concentration, carry out enzymolysis, constantly stir, enzymolysis 3h at 37 DEG C.At 100 DEG C after high-temperature process enzymolysis solution 15min, the centrifugal 5min of 6000rpm, supernatant adds two volumes ether and leaves standstill 15min, the centrifugal 5min of 6000rpm, precipitates the dry thing 30kg of dry little peptide.To refine dark glaucoma Adeps Serpentis 50kg to heat after 35 ~ 45 DEG C, stir after adding the dry thing 1kg of little peptide zaocys dhumnades oil product obtained by final vacuum lyophilization, and detecting made Adeps Serpentis product Linoleic acid through gas chromatograph, to obtain content be 16.39%.
Comparative examples 1
Grade of getting it filled zaocys dhumnades 100kg, is crushed to by 10 mesh sieves, obtains snake powder; Above-mentioned snake powder is added 400kg acetone, lixiviate 150min, reclaim acetone and must obtain the neutral active charcoal that thick Adeps Serpentis adds 3%, be heated to 50 DEG C of decolourings 20 minutes, 500 orders filter removes active carbon, obtains refining dark glaucoma Adeps Serpentis.Detecting made Adeps Serpentis product Linoleic acid through gas chromatograph, to obtain content be 17.2%.
Comparative examples 2
By the method that CN103468390A provides, described concrete steps are as follows: the fatty tissue extracting Serpentis, repeatedly clean, and remove the impurity such as Periostracum Serpentis, fiber be mixed into; The fat of extraction is carried out heating refining, after 10min, stop heating, must produce liquid, use filtered through gauze while hot 1 time in 1min, until the invisible impurity of filtrate, obtain filtrate and filtering residue, gained filtrate is the main liquid of Adeps Serpentis; Above-mentioned filtering residue is carried out squeezing 5min, till oozing out without oil, obtains pressed liquor; Above-mentioned pressed liquor is carried out filtration 1 time, gained filtrate is contained Adeps Serpentis in filtering residue; Merged and crossed above-mentioned gained filtrate and obtained the thick product of Adeps Serpentis; By thick for Adeps Serpentis product organic solvent extraction 3 times, organic solvent quality is 1 times of the thick product quality of Adeps Serpentis, is to extract 5min under the ultrasound wave of 30KHZ in frequency, merges organic solvent layer liquid, reclaims organic solvent by the way of distillation, and logical nitrogen; Fetch the Adeps Serpentis product after receiving organic solvent again, add organic solvent extraction 3 times, organic solvent quality is 1 times of the thick product quality of Adeps Serpentis, be extract 5min under the ultrasound wave of 30KHZ in frequency, merge organic solvent layer liquid, the way of distillation reclaims organic solvent, and logical nitrogen, eliminate organic solvent and namely obtain this refining Adeps Serpentis.The fatty tissue of described Serpentis is the fat that abdominal part extracts.Described heating refining temperature is 30 DEG C.Described squeeze pressure is 1000Psi.The described way of distillation reclaims organic solvent, and temperature controls at 40 DEG C.Gained Adeps Serpentis is faint yellow or yellow oily liquid, and Serpentis fishy smell is heavier.The content detecting gained Adeps Serpentis Linoleic acid through gas chromatograph is 15.60%.
Embodiment 2
Pharmaceutical grade zaocys dhumnades 200kg is carried out shattering to 10-20 order, obtains snake powder.The acetone of 400L is added to snake powder; at nitrogen protection stirring at room temperature lixiviate 90min; via hole diameter is that the ceramic membrane filter of 0.22 μm obtains lixiviating solution; the acetone of 400L is added again to the snake powder of extracted; at nitrogen protection stirring at room temperature lixiviate 60min; via hole diameter is that the ceramic membrane filter of 0.22 μm obtains lixiviating solution, merges twice lixiviating solution and obtains acetone filtrate and Serpentis residue.0.5mm neutral active carbon granule 25kg is added to acetone filtrate; room temperature decolouring 20-30 minute under nitrogen protection; ceramic membrane filter once; 40 DEG C of concentrating under reduced pressure remove acetone; obtain grease; carry out extracting once with the ethanol of two volumes, obtain ethanolic extract, 40 DEG C of concentrating under reduced pressure are removed ethanol and must be refined dark glaucoma Adeps Serpentis 26.65kg.
Acetone extraction residue 170kg is added the water of 340kg, add the neutral protease of 10kg, reach 5-10U/L to final concentration, constantly stir, enzymolysis 1h at 30 DEG C, then add 25kg trypsin, reach 10-20U/L to final concentration, carry out enzymolysis, constantly stir, enzymolysis 4h at 30 DEG C.At 100 DEG C after high-temperature process enzymolysis solution 20min, the centrifugal 5min of 6000rpm, supernatant adds two volumes ether and leaves standstill 20min, the centrifugal 5min of 6000rpm, precipitates the dry thing 75kg of dry little peptide.To refine dark glaucoma Adeps Serpentis 50kg to heat after 35 ~ 45 DEG C, stir after adding the dry thing 1.5kg of little peptide zaocys dhumnades oil product obtained by final vacuum lyophilization, and detecting made Adeps Serpentis product Linoleic acid through gas chromatograph, to obtain content be 16.23%.
Linoleic acid content situation after table 1. product placement different time
Claims (7)
1. zaocys dhumnades oil product mixes obtained by the dry thing of refining dark glaucoma Adeps Serpentis and little peptide, wherein each raw material composition forms with following weight portion: after refining dark glaucoma Adeps Serpentis 50 parts heating 35 ~ 45 DEG C, stirs made by final vacuum lyophilization after adding the dry thing 0.01 ~ 8 part of little peptide.
2. method according to claim 1, wherein each material composition forms with following weight portion: make after dry thing 0.05 ~ 5 part mixing of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
3. method according to claim 1, wherein each material composition forms with following weight portion: make after dry thing 0.5 ~ 3 part mixing of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
4. method according to claim 1, wherein each material composition forms with following weight portion: make after the dry thing 1 part mixing of refining dark glaucoma Adeps Serpentis 50 parts, little peptide.
5. according to the method for claim 1 or 2 or 3 or 4, the preparation method of wherein said refining dark glaucoma Adeps Serpentis and the dry thing of little peptide, its concrete steps are as follows:
(1) shatter: pharmaceutical grade zaocys dhumnades is carried out shattering to 10-20 order, obtains snake powder;
(2) acetone extraction: add acetone to above-mentioned snake powder, in nitrogen protection stirring at room temperature lixiviate twice, each lixiviate 60-90min, obtains lixiviating solution through ceramic membrane filter, merges twice lixiviating solution and obtains acetone filtrate and Serpentis residue;
(3) decoloration and deodorization: add appropriate neutral active carbon granule to acetone filtrate, room temperature decolouring 20-30 minute under nitrogen protection, ceramic membrane filter once, 40 DEG C of concentrating under reduced pressure remove acetone, obtain grease, carry out extracting once with the ethanol of two volumes, obtain ethanolic extract, 40 DEG C of concentrating under reduced pressure are removed ethanol and must be refined dark glaucoma Adeps Serpentis;
(4) enzymolysis: acetone extraction residue adds the water of double weight, adds neutral protease, reaches 5-10U/L to final concentration, constantly stirs, enzymolysis 1h at 30 DEG C, then add trypsin, reach 15-20U/L to final concentration, carry out enzymolysis, constantly stir, enzymolysis 2-4h at 37 DEG C;
(5) little peptide separation and Extraction: after 90-100 DEG C of high-temperature process enzymolysis solution 10-30min, the centrifugal 5min of 6000rpm, supernatant adds two volumes ether and leaves standstill the centrifugal 5min of 5 ~ 20min, 6000rpm, precipitates the dry thing of dry little peptide.
6. method according to claim 5, the wherein consumption of acetone described in step (2), the ratio of its volume L/ snake powder weight kg is 3 ~ 6:1.
7. method according to claim 5, the wherein consumption of neutral active carbon granule described in step (3), the ratio of its weight kg/ snake powder acetone filtrate volume L is 3 ~ 6:50, neutral active carbon granule diameter 0.2-5mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754716A (en) * | 2016-02-25 | 2016-07-13 | 湖南科技学院 | Low-temperature extracted snake oil and method for deodorizing and de-coloring snake oil |
| CN109385331A (en) * | 2018-10-25 | 2019-02-26 | 南京润力生物科技有限公司 | A kind of extraction preparation method of multiple-effect snake oil |
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| CN105754716A (en) * | 2016-02-25 | 2016-07-13 | 湖南科技学院 | Low-temperature extracted snake oil and method for deodorizing and de-coloring snake oil |
| CN105754716B (en) * | 2016-02-25 | 2020-02-07 | 湖南科技学院 | Method for extracting snake oil at low temperature and removing fishy smell and decoloring of snake oil |
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