CN109106972A - A kind of preparation method of hydrophily polylactic acid operation suture thread - Google Patents

A kind of preparation method of hydrophily polylactic acid operation suture thread Download PDF

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CN109106972A
CN109106972A CN201810911852.4A CN201810911852A CN109106972A CN 109106972 A CN109106972 A CN 109106972A CN 201810911852 A CN201810911852 A CN 201810911852A CN 109106972 A CN109106972 A CN 109106972A
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polylactic acid
filament yarn
chitosan
drying
lipase
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刘淑强
吴改红
刘明芳
余娟娟
张瑶
王鹏
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
    • A61L17/06—At least partially resorbable materials
    • A61L17/10—At least partially resorbable materials containing macromolecular materials
    • A61L17/12—Homopolymers or copolymers of glycolic acid or lactic acid
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
    • A61L17/14—Post-treatment to improve physical properties
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment

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  • Engineering & Computer Science (AREA)
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  • Surgery (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Veterinary Medicine (AREA)
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Abstract

本发明涉及一种亲水性聚乳酸手术缝合线的制备方法，是针对聚乳酸手术缝合线亲水性较差的情况，对聚乳酸长丝纱线的表面进行亲水改性，用磷酸盐缓冲液中的脂肪酶来处理聚乳酸长丝纱线，增加纱线表面的羟基数量；用壳聚糖的醋酸溶液来处理经脂肪酶处理后的纱线，将亲水性物质壳聚糖接枝到聚乳酸长丝纱线的表面，从而有效提高聚乳酸长丝纱线的亲水性；处理后的聚乳酸长丝纱线的吸湿率为0.6206％，比处理前提高了26.27％。

The invention relates to a preparation method of a hydrophilic polylactic acid surgical suture. In view of the poor hydrophilicity of the polylactic acid surgical suture, the surface of the polylactic acid filament yarn is hydrophilically modified, and phosphate The lipase in the buffer is used to treat the polylactic acid filament yarn to increase the number of hydroxyl groups on the surface of the yarn; the acetic acid solution of chitosan is used to treat the lipase-treated yarn, and the hydrophilic substance chitosan is bonded to the yarn. Branches to the surface of the polylactic acid filament yarn, thereby effectively improving the hydrophilicity of the polylactic acid filament yarn; the moisture absorption rate of the treated polylactic acid filament yarn is 0.6206%, which is 26.27% higher than that before treatment.

Description

A kind of preparation method of hydrophily polylactic acid operation suture thread
Technical field:
The present invention relates to a kind of preparation methods of hydrophily polylactic acid operation suture thread, belong to the skill of medical and health preparation Art field.
Background technique:
Currently, the surgical sewing thread of domestic clinical use is broadly divided into nonabsorable suture and absorbable suture Two kinds, nonabsorable suture needed because that cannot be absorbed by the body it is secondary take out stitches, the secondary pain of injury is caused to sufferer；Absorbable hand Art suture degrades and is absorbed by the body automatically after wound healing, takes out stitches without second operation, is particularly suitable for inside of human body group The wound healing knitted.Polylactic acid operation suture thread have it is nontoxic, nonirritant, have good biocompatibility, can biology point Solve absorbability and the high feature of mechanical strength；Polylactic acid operation suture thread degrades and is absorbed by the body automatically after wound healing, It takes out stitches without second operation, is particularly suitable for the wound healing of human body deep tissue.
But the molecule of polylactic acid operation suture thread is macro molecules, contained by a large amount of ester bonds make suture surface have There is extremely strong hydrophobicity, so that suture has poor biocompatibility, cellular affinity, will cause suture redness knot Block, serious to may also result in infective inflammation, these symptoms are all unfavorable for the healing of wound；Therefore, it is necessary to improve polylactic acid The hydrophily of operation suture thread, this technology is also in scientific research.
Summary of the invention:
Goal of the invention
The purpose of the present invention is being directed to the deficiency and applied defect of background technique, the surface of polylactic acid filament yarn is carried out Hydrophilic modifying handles polylactic acid filament yarn with the lipase being dissolved in phosphate buffer, increases the hydroxyl of yam surface Quantity；The yarn after lipase treatment is handled with the acetum of chitosan, by hydroaropic substance chitosan graft to poly- The surface of lactic acid filament yarn, so that the hydrophily of polylactic acid filament yarn is effectively improved, to expand its application range.
Technical solution
The chemical substance material that the present invention uses are as follows: polylactic acid filament yarn, chitosan, lipase, potassium dihydrogen phosphate, phosphorus It is as follows to prepare dosage for sour disodium hydrogen, phosphoric acid, glacial acetic acid, dehydrated alcohol, deionized water, nitrogen, alcohol: with gram, milliliter, it is vertical Square centimetre, millimeter are measurement unit
The preparation method is as follows:
(1) selected chemical substance material
The chemical substance material that uses of preparation to be carried out selected, and carry out quality purity, concentration, content control:
Polylactic acid filament yarn: solid state, fibrous filament, 99.5%
Chitosan: solid powder, 99%
Lipase: solid powder, mixture, 99%
Potassium dihydrogen phosphate: solid state, 99.5%
Disodium hydrogen phosphate: solid state, 99.5%
Phosphoric acid: liquid liquid, 99.5%
Glacial acetic acid: liquid liquid, 99.5%
Nitrogen: gaseous atmospheres, 99.9%
Dehydrated alcohol: liquid liquid, 99.9%
Deionized water: liquid liquid, 99.9%
Alcohol: liquid liquid, concentration 75%
(2) it is cleaned by ultrasonic
1. polylactic acid filament yarn is placed in conical flask, and dehydrated alcohol 100mL is added；
2. conical flask is placed in ultrasonic cleaner, it is cleaned by ultrasonic, ultrasonic frequency 60KHz, ultrasonic cleaning Time is 60min；
3. deionized water is cleaned, the polylactic acid filament yarn after ultrasonic cleaning is added in another beaker, deionization is added Water 100mL, is cleaned, and cleaning repeats three times；
4. being dried in vacuo, the polylactic acid filament yarn after cleaning is placed in quartz container, vacuum oven is subsequently placed in Middle drying, 40 DEG C of drying temperature, vacuum degree 2Pa, drying time 30min；
(3) surface etch polylactic acid filament yarn
1. matching liquid, weigh potassium dihydrogen phosphate 0.5874g ± 0.01g, disodium hydrogen phosphate 3.2338g ± 0.01g, measurement go from Sub- water 337mL ± 0.01mL is added in beaker, stirring and dissolving, at mixed liquor；
Then phosphoric acid 8mL ± 0.01mL is added, adjusts pH value at 7.4；
2. weighing lipase 0.8425g ± 0.01g, it is added in mixed solution, lipase solution, concentration 2.5g/ is made L；
The beaker for filling lipase solution is put into ultrasonic disperser, progress ultrasonic disperse, supersonic frequency 60KHz, Jitter time 120min；
3. polylactic acid filament yarn is put into lipase solution, and seal, be subsequently placed in water bath chader, 45 6h is vibrated in DEG C water；
4. deionized water is cleaned, polylactic acid filament yarn is placed in another beaker, deionized water 200mL, stirring is added Cleaning；
5. being dried in vacuo, after cleaning, polylactic acid filament yarn is placed in quartz container, is subsequently placed in vacuum oven It is dry, vacuum degree 2Pa, 20 DEG C of drying temperature, drying time 10h；
(4) chitosan grafted polylactic acid filament yarn
1. drying, the polylactic acid filament yarn of lipase treatment is placed in a vacuum drying oven, vacuum degree 2Pa, dry temperature 50 DEG C of degree, drying time 10min；
2. preparing acetum, glacial acetic acid 10mL ± 0.01mL, deionized water 327mL ± 0.01mL are added in beaker, Stir into acetum；
3. weighing chitosan 1g ± 0.01g, it is added in acetum, at chitosan-acetic acid solution；
4. the polylactic acid filament yarn of pretreated drying is put into chitosan-acetic acid solution, it is placed in conical flask, It is passed through nitrogen, is sealed；
Then conical flask is placed in water-bath constant temperature oscillator and vibrates 4h, 45 DEG C of bath temperature；
5. eluting, polylactic acid filament yarn is sling, is sprayed and is cleaned with dehydrated alcohol, time 3min；
6. drying, polylactic acid filament yarn is placed in vacuum drying oven drying, vacuum degree 2Pa, drying temperature 45 after elution DEG C, dry 30min obtains chitosan grafted polylactic acid filament yarn after dry；
(5) it sterilizes
Chitosan grafted polylactic acid filament yarn is placed in a beaker, alcohol 200mL is then added, impregnates 120min；
(6) it is dried in vacuo, after disinfection, chitosan grafted polylactic acid filament yarn is placed in quartz container, is subsequently placed in In vacuum oven, 45 DEG C of drying temperature, vacuum degree 2Pa, drying time 30min；
Obtain hydrophily polylactic acid operation suture thread；
(7) test, analysis and characterization
The surface topography, physical and chemical performance, mechanical property of the hydrophily polylactic acid operation suture thread of preparation are examined It surveys, analysis, characterization；
Hydrophily test is carried out under standard atmosphere environment, i.e., temperature is 20 DEG C ± 1 DEG C, relative humidity 65%, Test fiber hygroscopicity；
The configuration of surface of hydrophilic polylactic acid operation suture thread is observed with JSM-6510LA type scanning electron microscope；
Conclusion: the hydroscopicity of hydrophily polylactic acid operation suture thread is 0.6206%, is improved compared to hydroscopicity before modified 26.27%.
Beneficial effect
It for raw material, chitosan is modified material that the present invention, which uses acid fiber by polylactic, and polylactic acid suture is through lipase surface It is modified, with chitosan graft, hydrophilic polylactic acid suture is made；The chitosan for being grafted to suture surface has well Biocompatibility, microbial resistance, antiviral property, wound healing can be promoted, the aminoglucose discharged in degradation process The alkaline smalls substance such as sugar can neutralize the acid products such as the lactic acid released when polylactic acid degradation, can inhibit polylactic acid and cause Delayed onset foreign matter inflammatory reaction；Chitosan also has good hydrophily, water diffusion can be accelerated to penetrate into polylactic acid Rate in operation suture thread improves the hydrophily of polylactic acid operation suture thread；The hydroscopicity of modified polylactic acid suture is 0.6206%, increase by 26.27% compared to hydroscopicity before modified, the hydrophily of polylactic acid operation suture thread is improved, Biocompatibility and cellular affinity are greatly improved.
Detailed description of the invention
Fig. 1 is chitosan concentration to the hygroscopic influence diagram of polylactic acid suture
Fig. 2 is polylactic acid operation suture thread electron microscope: it is (a) untreated, (b) after chitosan graft
Specific embodiment
Below in conjunction with attached drawing, the invention will be further described:
The magnitude for preparing the chemical substance used is determined by pre-set range, with gram, millimeter, milliliter, cube Centimetre be measurement unit.
It is chitosan concentration to the hygroscopic influence diagram of polylactic acid suture, with the increasing of chitosan concentration shown in Fig. 1 Add, hygroscopicity increases considerably first, and then basic variation is little；It is hydrophilic that this explanation is grafted to having for suture surface Chitosan is more, and the hygroscopicity of suture is bigger, when the chitosan quantity of suture surface grafting saturation, suture hygroscopicity It is held essentially constant.
It is polylactic acid operation suture thread electron microscope shown in Fig. 2, the polylactic acid hand without any processing it can be seen from figure a Art suture surface is smooth and gloss is preferable；It can be seen from figure b through the attachment of chitosan graft treated suture surface compared with The chitosan of bulky grain, rough surface, this illustrates that chitosan has been grafted to suture surface really.

Claims (1)

1.一种亲水性聚乳酸手术缝合线的制备方法，其特征在于：使用的化学物质材料为：聚乳酸长丝纱线、壳聚糖、脂肪酶、磷酸二氢钾、磷酸氢二钠、磷酸、冰醋酸、无水乙醇、去离子水、氮气、酒精，其准备用量如下：以克、毫升、立方厘米、毫米为计量单位1. a preparation method of a hydrophilic polylactic acid surgical suture is characterized in that: the chemical material used is: polylactic acid filament yarn, chitosan, lipase, potassium dihydrogen phosphate, disodium hydrogen phosphate , phosphoric acid, glacial acetic acid, anhydrous ethanol, deionized water, nitrogen gas, alcohol, the preparation dosage is as follows: in grams, milliliters, cubic centimeters, millimeters as the unit of measurement 聚乳酸长丝纱线：HO[OCCH(CH3)]nOH,n＝4500 0.5mm×100000mmPolylactic acid filament yarn: HO[OCCH(CH 3 )] n OH, n=4500 0.5mm×100000mm 制备方法如下：The preparation method is as follows: (1)精选化学物质材料(1) Selected chemical materials 对制备使用的化学物质材料要进行精选，并进行质量纯度、浓度、含量控制：The chemical materials used in the preparation should be selected, and the quality, purity, concentration and content should be controlled: 聚乳酸长丝纱线：固态固体，纤维状长丝，99.5％Polylactic acid filament yarn: solid solid, fibrous filament, 99.5% 壳聚糖：固体粉末，99％Chitosan: solid powder, 99% 脂肪酶：固体粉末，混合物，99％Lipase: solid powder, mixture, 99% 磷酸二氢钾：固态固体，99.5％Potassium dihydrogen phosphate: solid solid, 99.5% 磷酸氢二钠：固态固体，99.5％Disodium hydrogen phosphate: solid solid, 99.5% 磷酸：液态液体，99.5％Phosphoric Acid: Liquid Liquid, 99.5% 冰醋酸：液态液体，99.5％Glacial Acetic Acid: Liquid Liquid, 99.5% 氮气：气态气体，99.9％Nitrogen: gaseous gas, 99.9% 无水乙醇：液态液体，99.9％Anhydrous ethanol: liquid liquid, 99.9% 去离子水：液态液体，99.9％Deionized water: liquid liquid, 99.9% 酒精：液态液体，浓度75％Alcohol: liquid liquid, concentration 75% (2)超声清洗(2) Ultrasonic cleaning ①将聚乳酸长丝纱线置于锥形瓶中，并加入无水乙醇100mL；①Place the polylactic acid filament yarn in a conical flask, and add 100 mL of absolute ethanol; ②将锥形瓶置于超声波清洗器中，进行超声清洗，超声波频率60KHz，超声波清洗时间为60min；②Place the conical flask in an ultrasonic cleaner for ultrasonic cleaning, the ultrasonic frequency is 60KHz, and the ultrasonic cleaning time is 60min; ③去离子水清洗，将超声清洗后的聚乳酸长丝纱线加入另一烧杯中，加入去离子水100mL，进行清洗，清洗重复进行三次；③Cleaning with deionized water, adding the ultrasonically cleaned polylactic acid filament yarn into another beaker, adding 100 mL of deionized water, cleaning, and repeating the cleaning three times; ④真空干燥，将清洗后的聚乳酸长丝纱线置于石英容器中，然后置于真空干燥箱中干燥，干燥温度40℃，真空度2Pa，干燥时间30min；④Vacuum drying, the cleaned polylactic acid filament yarn is placed in a quartz container, and then placed in a vacuum drying oven to dry, the drying temperature is 40°C, the vacuum degree is 2Pa, and the drying time is 30min; (3)表面刻蚀聚乳酸长丝纱线(3) Surface etching polylactic acid filament yarn ①配液，称取磷酸二氢钾0.5874g±0.01g、磷酸氢二钠3.2338g±0.01g，量取去离子水337mL±0.01mL，加入烧杯中，搅拌溶解，成混合液；① To prepare the solution, weigh 0.5874g±0.01g of potassium dihydrogen phosphate and 3.2338g±0.01g of disodium hydrogen phosphate, measure 337mL±0.01mL of deionized water, add it to a beaker, stir and dissolve to form a mixed solution; 然后加入磷酸8mL±0.01mL，调节pH值成7.4；Then add phosphoric acid 8mL±0.01mL, adjust the pH value to 7.4; ②称取脂肪酶0.8425g±0.01g，加入混合溶液中，制成脂肪酶溶液，浓度为2.5g/L；②Weigh 0.8425g ± 0.01g of lipase, add it to the mixed solution, and make a lipase solution with a concentration of 2.5g/L; 将盛有脂肪酶溶液的烧杯放入超声波分散器中，进行超声分散，超声频率60KHz，分散时间120min；Put the beaker containing the lipase solution into the ultrasonic disperser, carry out ultrasonic dispersion, ultrasonic frequency 60KHz, dispersion time 120min; ③将聚乳酸长丝纱线，放入脂肪酶溶液中，并密封，然后置于水浴振荡器中，在45℃水中振荡6h；③Put the polylactic acid filament yarn into the lipase solution, seal it, and then place it in a water bath shaker and shake it in water at 45°C for 6 hours; ④去离子水清洗，将聚乳酸长丝纱线置于另一烧杯中，加入去离子水200mL，搅拌清洗；④Clean with deionized water, place the polylactic acid filament yarn in another beaker, add 200 mL of deionized water, stir and clean; ⑤真空干燥，清洗后，将聚乳酸长丝纱线置于石英容器中，然后置于真空干燥箱中干燥，真空度2Pa，干燥温度20℃，干燥时间10h；⑤Vacuum drying, after cleaning, put the polylactic acid filament yarn in a quartz container, and then put it in a vacuum drying oven to dry, the vacuum degree is 2Pa, the drying temperature is 20℃, and the drying time is 10h; (4)壳聚糖接枝聚乳酸长丝纱线(4) Chitosan grafted polylactic acid filament yarn ①干燥，将脂肪酶处理的聚乳酸长丝纱线置于真空干燥箱中，真空度2Pa，干燥温度50℃，干燥时间10min；①Drying, place the polylactic acid filament yarn treated with lipase in a vacuum drying oven, the vacuum degree is 2Pa, the drying temperature is 50℃, and the drying time is 10min; ②制备醋酸溶液，将冰醋酸10mL±0.01mL、去离子水327mL±0.01mL加入烧杯中，搅拌成醋酸溶液；② To prepare acetic acid solution, add 10 mL ± 0.01 mL of glacial acetic acid and 327 mL ± 0.01 mL of deionized water into a beaker, and stir to form an acetic acid solution; ③称取壳聚糖1g±0.01g，加入醋酸溶液中，成壳聚糖醋酸溶液；③ Weigh 1g ± 0.01g of chitosan, add it to acetic acid solution, and form chitosan acetic acid solution; ④将预处理的干燥的聚乳酸长丝纱线放入壳聚糖醋酸溶液中，并置于锥形瓶中，通入氮气，密封；④Put the pretreated dry polylactic acid filament yarn into the chitosan acetic acid solution, put it in a conical flask, pass nitrogen gas, and seal; 然后将锥形瓶置于水浴恒温振荡器中振荡4h，水浴温度45℃；Then the conical flask was placed in a water bath thermostatic oscillator for 4 hours, and the water bath temperature was 45°C; ⑤淋洗，将聚乳酸长丝纱线吊起，用无水乙醇喷淋清洗，时间3min；⑤ Rinse, hoist the polylactic acid filament yarn, and spray and clean it with absolute ethanol for 3 minutes; ⑥干燥，淋洗后将聚乳酸长丝纱线置于真空烘箱中干燥，真空度2Pa，干燥温度45℃，干燥30min，干燥后得壳聚糖接枝聚乳酸长丝纱线；⑥Drying, after rinsing, the polylactic acid filament yarn is dried in a vacuum oven, the vacuum degree is 2Pa, the drying temperature is 45 ℃, and the drying is 30 minutes, and after drying, the chitosan-grafted polylactic acid filament yarn is obtained; (5)消毒(5) Disinfection 将壳聚糖接枝聚乳酸长丝纱线置于烧杯中，然后加入酒精200mL，浸泡120min；Put the chitosan grafted polylactic acid filament yarn in a beaker, then add 200 mL of alcohol, and soak for 120 min; (6)真空干燥，消毒后，将壳聚糖接枝聚乳酸长丝纱线置于石英容器中，然后置于真空干燥箱中，干燥温度45℃，真空度2Pa，干燥时间30min；(6) vacuum drying, after sterilization, the chitosan grafted polylactic acid filament yarn is placed in a quartz container, and then placed in a vacuum drying oven, drying temperature is 45°C, vacuum degree is 2Pa, and drying time is 30min; 得亲水性聚乳酸手术缝合线；Hydrophilic polylactic acid surgical sutures were obtained; (7)检测、分析、表征(7) Detection, analysis and characterization 对制备的亲水性聚乳酸手术缝合线的表面形貌、物理化学性能、力学性能进行检测、分析、表征；The surface morphology, physicochemical properties and mechanical properties of the prepared hydrophilic polylactic acid surgical suture were detected, analyzed and characterized; 亲水性测试是在标准温湿度环境下进行，即温度为20℃±1℃，相对湿度为65％，测试纤维吸湿性；The hydrophilicity test is carried out in a standard temperature and humidity environment, that is, the temperature is 20°C ± 1°C, and the relative humidity is 65% to test the hygroscopicity of the fibers; 用JSM-6510LA型扫描电子显微镜观察亲水聚乳酸手术缝合线的表面形态；The surface morphology of the hydrophilic polylactic acid surgical suture was observed with a JSM-6510LA scanning electron microscope; 结论：亲水性聚乳酸手术缝合线的吸湿率为0.6206％，相比改性前吸湿率提高26.27％。Conclusion: The moisture absorption rate of the hydrophilic polylactic acid surgical suture is 0.6206%, which is 26.27% higher than that before modification.
CN201810911852.4A 2018-08-10 2018-08-10 A kind of preparation method of hydrophily polylactic acid operation suture thread Pending CN109106972A (en)

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CN111529752B (en) * 2020-04-15 2021-07-16 东华大学 A kind of variable cross-section porous band suture for promoting tendon healing and preparation method thereof
CN113730644A (en) * 2021-09-13 2021-12-03 苏州大学 Suture line with gel coating and preparation method thereof
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CN110665045A (en) * 2019-10-17 2020-01-10 王时灿 Absorbable suture for obstetrics and gynecology department and preparation method thereof
CN111529752B (en) * 2020-04-15 2021-07-16 东华大学 A kind of variable cross-section porous band suture for promoting tendon healing and preparation method thereof
CN113730644A (en) * 2021-09-13 2021-12-03 苏州大学 Suture line with gel coating and preparation method thereof
CN116218718A (en) * 2023-01-04 2023-06-06 上海乾界生物科技有限公司 Bacteria for decomposing oil

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Application publication date: 20190101