CN105079865B - A kind of preparation method of the outer compress material of oxycellulose - Google Patents
A kind of preparation method of the outer compress material of oxycellulose Download PDFInfo
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- CN105079865B CN105079865B CN201510612262.8A CN201510612262A CN105079865B CN 105079865 B CN105079865 B CN 105079865B CN 201510612262 A CN201510612262 A CN 201510612262A CN 105079865 B CN105079865 B CN 105079865B
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- 239000000463 material Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000012141 concentrate Substances 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 8
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 8
- 241000123069 Ocyurus chrysurus Species 0.000 claims abstract description 8
- 241000967218 Selaginella tamariscina Species 0.000 claims abstract description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 125000004494 ethyl ester group Chemical group 0.000 claims description 5
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 1
- 239000001768 carboxy methyl cellulose Substances 0.000 abstract description 6
- 230000000025 haemostatic effect Effects 0.000 abstract description 4
- SJIXRGNQPBQWMK-UHFFFAOYSA-N 2-(diethylamino)ethyl 2-methylprop-2-enoate Chemical compound CCN(CC)CCOC(=O)C(C)=C SJIXRGNQPBQWMK-UHFFFAOYSA-N 0.000 abstract description 3
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 abstract 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 abstract 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 abstract 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 5
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 5
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 241000699666 Mus <mouse, genus> Species 0.000 description 3
- 230000000740 bleeding effect Effects 0.000 description 3
- 230000023597 hemostasis Effects 0.000 description 3
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 238000003032 molecular docking Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 1
- 241000581650 Ivesia Species 0.000 description 1
- 238000012449 Kunming mouse Methods 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 101100203936 Mus musculus Srpra gene Proteins 0.000 description 1
- 206010048629 Wound secretion Diseases 0.000 description 1
- 238000010171 animal model Methods 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 230000002439 hemostatic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a kind of preparation method of compress material outside oxycellulose, first takes 10 20 parts of Selaginella tamariscina in parts by weight, 8 15 parts of madder, adds water to cook, and obtains decoction liquor one and then concentrates decoction liquor one, obtains concentrate one；14 parts of calcium carbonate in parts by weight, 26 parts of HES, 5 10 parts of sodium carboxymethylcellulose are added in concentrate one, 24 parts of disodium ethylene diamine tetraacetate, 50 80 parts of water, under vacuum heating stirring 50 100 minutes, then concentrate, obtain concentrate two；20 30 parts of oxycellulose in parts by weight is added in concentrate two, 14 parts of diethyl aminoethyl methacrylate, is uniformly mixed, is warming up to 40 50 DEG C, stands 150 200 minutes, obtains the outer compress material of oxycellulose.The outer compress material that preparation method provided by the invention obtains has good haemostatic effect, can be preferably applied for medical field.
Description
Technical field
The invention belongs to medical material field, and in particular to a kind of preparation method of the outer compress material of oxycellulose.
Background technology
With the growing interest and attention of global environmental pollution and shortage of resources problem, there is biodegradability, ring
The material of border harmony turns into the focus that countries in the world are competitively developed.Cellulose is renewable natural polymer most abundant on the earth
Inexhaustible, nexhaustible organic resource in son and nature, and cellulosic material itself is nontoxic, water-resistance is strong, meets
Biodegradability, the requirement of Study on Environment Compatible Materials, thus use and cellulose derivative of the cellulose as host material
The focus for being developed into studying outside Now Domestic.Cellulose derivative, such as carboxymethyl cellulose, hydroxypropyl cellulose, because
This kind of high molecular biocompatibility, biodegradability and nontoxicity and make it that its application in the industry is very wide
It is general.Chemical modification is to obtain this kind of high molecular effective ways with property.Oxidation reaction, especially selective oxidation
Reaction, some or certain several hydroxyls that can optionally on the glucose residue of oxycellulose macromolecular basic ring, and in spy
Positioning, which is put, introduces new functional group, and such as carboxyl, aldehyde radical or carbonyl, this kind of cellulose oxidation thing can make fiber because of its unique texture
Element has new purposes.Oxycellulose is widely applied in medical field as styptic at present, can play good hemostasis
Effect, but the outer compress material for being currently based on oxycellulose is actually rare, while also strengthen without preferably preparation method
The haemostatic effect of material.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art and provides a kind of preparation side of compress material outside oxycellulose
Method so that the outer compress material being prepared has excellent hemostatic function.
Technical scheme is as follows：
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1, Selaginella tamariscina 10-20 parts in parts by weight are taken, madder 8-15 parts, adds water to cook, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one；
Step 3, calcium carbonate 1-4 parts in parts by weight, HES 2-6 parts, carboxymethyl are added in concentrate one
Sodium cellulosate 5-10 parts, disodium ethylene diamine tetraacetate 2-4 parts, water 50-80 parts, heating stirring 50-100 points under vacuum
Clock, then concentrate, obtain concentrate two；
Step 4, oxycellulose 20-30 parts in parts by weight, methacrylic acid diethyl are added in concentrate two
Amino ethyl ester 1-4 parts, are uniformly mixed, and are warming up to 40-50 DEG C, stand 150-200 minutes, obtain oxycellulose external application material
Material.
The preparation method of the outer compress material of described oxycellulose, in step 1 plus the parts by weight of water be 100-120 parts, pan-fried
Boil hour time 2-4.
The preparation method of the outer compress material of described oxycellulose, the volume of concentrate one is two before concentration in step 2
/ mono-.
The preparation method of the outer compress material of described oxycellulose, the vacuum of vacuum condition is 0.01- in step 3
0.05MPa。
The preparation method of the outer compress material of described oxycellulose, the temperature heated in step 3 is 50-60 DEG C.
The preparation method of the outer compress material of described oxycellulose, the volume of concentrate two is three before concentration in step 3
/ bis-.
The preparation method of the outer compress material of oxycellulose provided by the invention be prepared by specific preparation technology
With component, the compress material oxycellulose with excellent haemostatic effect outer is prepared, medical neck can be preferably applied for
In domain.
Embodiment
Embodiment 1
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1,10 parts of Selaginella tamariscina in parts by weight is taken, 8 parts of madder, is added water to cook, the parts by weight for adding water are 100 parts, are decocted
Time 2 h is boiled, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one, the volume of concentrate one is the half before concentration；
Step 3,1 part of calcium carbonate in parts by weight, HES 2- parts, carboxymethyl fibre are added in concentrate one
Tie up plain 5 parts of sodium, 2 parts of disodium ethylene diamine tetraacetate, 50 parts of water, in the heated under vacuum that vacuum is 0.01MPa to 50 DEG C,
Stirring 50 minutes, is then concentrated, and obtains concentrate two, the volume of concentrate two is 2/3rds before concentration；
Step 4,20 parts of oxycellulose in parts by weight, methacrylic acid diethyl amino are added in concentrate two
1 part of base ethyl ester, is uniformly mixed, and is warming up to 40 DEG C, stands 150 minutes, obtains the outer compress material of oxycellulose.
Embodiment 2
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1,12 parts of Selaginella tamariscina in parts by weight being taken, 10 parts of madder, is added water to cook, the parts by weight for adding water are 105 parts,
Decocting time 3 hours, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one, the volume of concentrate one is the half before concentration；
Step 3,2 parts of calcium carbonate in parts by weight, 3 parts of HES, carboxymethyl cellulose are added in concentrate one
Plain 6 parts of sodium, 3 parts of disodium ethylene diamine tetraacetate, 60 parts of water, in the heated under vacuum that vacuum is 0.02MPa to 53 DEG C, stir
Mix 70 minutes, then concentrate, obtain concentrate two, the volume of concentrate two is 2/3rds before concentration；
Step 4,25 parts of oxycellulose in parts by weight, methacrylic acid diethyl amino are added in concentrate two
2 parts of base ethyl ester, is uniformly mixed, and is warming up to 45 DEG C, stands 160 minutes, obtains the outer compress material of oxycellulose.
Embodiment 3
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1,17 parts of Selaginella tamariscina in parts by weight being taken, 13 parts of madder, is added water to cook, the parts by weight for adding water are 110 parts,
Decocting time 3 hours, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one, the volume of concentrate one is the half before concentration；
Step 3,3 parts of calcium carbonate in parts by weight, 5 parts of HES, carboxymethyl cellulose are added in concentrate one
Plain 8 parts of sodium, 3 parts of disodium ethylene diamine tetraacetate, 70 parts of water, in the heated under vacuum that vacuum is 0.03MPa to 56 DEG C, stir
Mix 80 minutes, then concentrate, obtain concentrate two, the volume of concentrate two is 2/3rds before concentration；
Step 4,29 parts of oxycellulose in parts by weight, methacrylic acid diethyl amino are added in concentrate two
3 parts of base ethyl ester, is uniformly mixed, and is warming up to 48 DEG C, stands 190 minutes, obtains the outer compress material of oxycellulose.
Embodiment 4
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1,20 parts of Selaginella tamariscina in parts by weight being taken, 15 parts of madder, is added water to cook, the parts by weight for adding water are 120 parts,
Decocting time 4 hours, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one, the volume of concentrate one is the half before concentration；
Step 3,4 parts of calcium carbonate in parts by weight, 6 parts of HES, carboxymethyl cellulose are added in concentrate one
Plain 10 parts of sodium, 4 parts of disodium ethylene diamine tetraacetate, 80 parts of water, in the heated under vacuum that vacuum is 0.05MPa to 60 DEG C,
Stirring 100 minutes, is then concentrated, and obtains concentrate two, the volume of concentrate two is 2/3rds before concentration；
Step 4,30 parts of oxycellulose in parts by weight, methacrylic acid diethyl amino are added in concentrate two
4 parts of base ethyl ester, is uniformly mixed, and is warming up to 50 DEG C, stands 200 minutes, obtains the outer compress material of oxycellulose.
Reference examples
A kind of preparation method of the outer compress material of oxycellulose, comprises the following steps：
Step 1,17 parts of Selaginella tamariscina in parts by weight being taken, 13 parts of madder, is added water to cook, the parts by weight for adding water are 110 parts,
Decocting time 3 hours, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one, the volume of concentrate one is the half before concentration；
Step 3,3 parts of calcium carbonate in parts by weight, 5 parts of HES, carboxymethyl cellulose are added in concentrate one
Plain 8 parts of sodium, 3 parts of disodium ethylene diamine tetraacetate, 70 parts of water, in the heated under vacuum that vacuum is 0.03MPa to 56 DEG C, stir
Mix 80 minutes, then concentrate, obtain concentrate two, the volume of concentrate two is 2/3rds before concentration；
Step 4,29 parts of oxycellulose in parts by weight is added in concentrate two, is uniformly mixed, is warming up to
48 DEG C, 190 minutes are stood, obtains the outer compress material of oxycellulose.
Compress material carries out animal experiment test outside the oxycellulose that above example is prepared, specific as follows：
Kun Ming mice is used as experimental animal, 100, body weight 30-35g.5 groups of experiment point：Blank group, control group,
Experimental group A, experimental group B, experimental group C, mouse are fixed in mouse fixing device by every group 20, and mouse tail is sterilized with alcohol swab
Bar end, cut with sharp scissors and cut at Mouse Tail-tip 1cm, there is blood flow to go out.Each experimental group carries out lower column processing：(1) blank
Group otch exposure；(2) experimental group A, B, C closely sticks the oxidation fibre that 1cm × 1cm above example is prepared at docking
The outer compress material of dimension element；(3) control group closely sticks the oxidized fibre that 1cm × 1cm above reference examples are prepared at docking
The outer compress material of element.Bleeding at mouse docking is observed in experiment, wound oozing of blood is sucked with filter paper per 10s, until bleeding stops
Only, bleeding stopping period is recorded.Experiment condition and result are as shown in the table：
As can be seen from the above results, the outer compress material of oxycellulose that preparation method of the present invention is prepared can be quick
Hemostasis, relative to blank group, the time needed for the hemostasis of outer compress material that preparation method of the present invention obtains is equivalent to blank auto-stopping
/ 10th of blood time, and control group is the experiment carried out using reference examples of the present invention, wherein reference examples are based on the present invention
The improvement carried out on the basis of embodiment 3, wherein no in preparation process four add diethyl aminoethyl methacrylate,
Other are same as Example 3, as a result as can be seen that the haemostatic effect of outer compress material finally obtained has declined, therefore can be with
Illustrate, diethyl aminoethyl methacrylate is in preparation process of the present invention except can be by oxycellulose and other compositions
Solidification is outer well also aids in the anthemorrhagic performance for enhancing material.
Claims (3)
1. the preparation method of the outer compress material of a kind of oxycellulose, it is characterised in that comprise the following steps：
Step 1, Selaginella tamariscina 10-20 parts in parts by weight are taken, madder 8-15 parts, adds water to cook, obtains decoction liquor one；
Step 2, decoction liquor one is concentrated, obtain concentrate one；
Step 3, calcium carbonate 1-4 parts in parts by weight, HES 2-6 parts, carboxymethyl are added in concentrate one
Sodium cellulosate 5-10 parts, disodium ethylene diamine tetraacetate 2-4 parts, water 50-80 parts, under vacuum heating stirring 50-
100 minutes, then concentrate, obtain concentrate two；
Step 4, oxycellulose 20-30 parts in parts by weight, methacrylic acid diethyl amino are added in concentrate two
Base ethyl ester 1-4 parts, are uniformly mixed, and are warming up to 40-50 DEG C, stand 150-200 minutes, obtain outside oxycellulose
Compress material；
Wherein in step 1 plus the parts by weight of water are 100-120 parts, decocting time 2-4 hours；Concentrate one in step 2
Volume for concentration before half；The vacuum of vacuum condition is 0.01-0.05MPa in step 3.
2. the preparation method of compress material outside the oxycellulose according to claim 1, it is characterised in that add in step 3
The temperature of heat is 50-60 DEG C.
3. the preparation method of compress material outside the oxycellulose according to claim 1, it is characterised in that dense in step 3
The volume of contracting liquid two is 2/3rds before concentration.
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| CN201510612262.8A CN105079865B (en) | 2015-09-23 | 2015-09-23 | A kind of preparation method of the outer compress material of oxycellulose |
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| CN105079865B true CN105079865B (en) | 2018-02-16 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109756A (en) * | 1993-12-23 | 1995-10-11 | 庄臣及庄臣医药有限公司 | Calcium modified oxidized cellulose hemostat |
| CN1312726A (en) * | 1998-08-14 | 2001-09-12 | 清水庆彦 | Topically absorbent hemostatic material |
| CN103110786A (en) * | 2013-02-09 | 2013-05-22 | 王维萌 | Preparation method of traditional Chinese medicine for treating traumatic type subconjunctival hemorrhage |
| CN104524624A (en) * | 2014-12-17 | 2015-04-22 | 安徽省健源医疗器械设备有限公司 | Chitosan hemostatic gauze and preparation method thereof |
-
2015
- 2015-09-23 CN CN201510612262.8A patent/CN105079865B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109756A (en) * | 1993-12-23 | 1995-10-11 | 庄臣及庄臣医药有限公司 | Calcium modified oxidized cellulose hemostat |
| CN1312726A (en) * | 1998-08-14 | 2001-09-12 | 清水庆彦 | Topically absorbent hemostatic material |
| CN103110786A (en) * | 2013-02-09 | 2013-05-22 | 王维萌 | Preparation method of traditional Chinese medicine for treating traumatic type subconjunctival hemorrhage |
| CN104524624A (en) * | 2014-12-17 | 2015-04-22 | 安徽省健源医疗器械设备有限公司 | Chitosan hemostatic gauze and preparation method thereof |
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Effective date of registration: 20210809 Address after: 212400 first floor, building A3, Jiangsu Dongheng airport high tech Industrial Park, No. 19, airport new area, Guozhuang Town, Jurong City, Zhenjiang City, Jiangsu Province Patentee after: Zhenjiang Junlin Biotechnology Co.,Ltd. Address before: 212434 building 03, east of Huamao Road, Guozhuang Town, Jurong City, Zhenjiang City, Jiangsu Province Patentee before: JIANGSU LANWAN BIOTECHNOLOGY Co.,Ltd. |