CN115387156B - 一种硅基材料抗菌性保护膜的制备方法 - Google Patents
一种硅基材料抗菌性保护膜的制备方法 Download PDFInfo
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- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
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- D—TEXTILES; PAPER
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
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- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
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- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
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Abstract
本发明提供了一种硅基材料抗菌性保护膜的制备方法。该法包括表面氧化修饰所述硅基材料形成表面抗菌膜,然后再用富含氨基长链化合物溶液处理固定抗菌膜。所述表面氧化修饰中,环氧基硅烷化试剂为3‑缩水甘油丙基三甲氧基硅烷(GPTMS)、3‑环氧丙氧基丙基二甲基乙氧基硅烷(GPDMES)、3‑(2,3)‑环氧丙基甲基二甲氧甲基硅烷(GPDMMS)、或3‑(2,3)环氧丙氧基丙基三甲氧基硅烷(GPTS)。所述富含氨基长链化合物包括壳聚糖、多聚赖氨酸、多聚组氨酸、聚亚乙基亚胺或聚烯丙基胺。本发明提供的滤纸接种大肠杆菌(8099)密度为1.8×105CFU/样,接种金黄色葡萄球菌(ATCC 6538)密度为1.9×105CFU/样,观察培养0h、18h后的细菌数量,计算得抑菌活性大于5.7,抑菌率为99%。
Description
技术领域
本发明涉及一种具有抗菌性保护膜的制备方法,具体讲涉及一种硅基材料抗菌性保护膜的制备方法。
背景技术
在全集成分子诊断分析中,基于硅基滤纸法的全血等体液样本保存已逐渐发展并得到应用,然而在应用过程中,长期保存过程的体液样本会产生细菌繁殖问题。比如FTA血卡等在长期保存血液等复杂样本时,需要在滤纸纤维上预先保存干燥的防腐剂等成分,此类操作既增加了样本制备纯化的流程和难度,同时残留试剂也会对后续的分析等检测造成不利影响,为了解决这一问题,因此需要增强硅基材料的抗菌性能,现有的构建抗菌型硅材料的方法分为无机抗菌剂、有机抗菌剂和天然抗菌剂三大类。无机抗菌剂包括金属离子型和光催化型,金属离子型有银系列、锌系列和铜系列,其中通过物理吸附、离子交换等方法,将具有抗菌性能的银、铜、锌等金属(或金属离子)固定在氟石、硅胶等多孔材料的表面制成抗菌剂;光催化型主要是锐钛矿型纳米TiO2,其杀菌能力源自于其光催化活性;无机类抗菌剂成本高同时抗菌效应缓慢,同时由于采用吸附方式固定抗菌膜,材料稳定性较差。有机类抗菌剂多以季铵盐、有机硅季铵盐类等为主,主要依靠其阳离子基团实现对各种细菌及真菌等抑菌杀菌作用,此类抗菌剂有选择性的抑制核酸扩增聚合酶同核酸分子的结合,降低聚合酶扩增效率及核酸检测灵敏度。天然抗菌剂包括甲壳质、壳聚糖和昆虫抗菌性蛋白质等动物的提取物,具有很好的生物反应相容性,但是直接涂覆修饰方式会造成抗菌性能不稳定。
因此,需要提供一种硅基材料表面膜的构建方法,来满足人们对于提高硅基材料表面的抗菌性能的需要,同时又能保证材料兼具有较好的生物反应相容性。
发明内容
本发明的目的是提供可用于硅基材料抗菌性提高的修饰工艺,同时兼具有良好的核酸分析生物相容性。
本发明的特征在于提高硅基纤维表面抗菌性。本发明提供的方法中,首先通过环氧基硅烷活化硅基材料表面,再通过与氨基长链接枝共聚,实现固定硅基表面的抗菌涂覆膜。
本发明提供了一种硅基材料抗菌性保护膜的制备方法,所述方法包括,于液相条件下,用环氧基硅烷处理所述硅基材料表面;用富含氨基长链化合物溶液处理经环氧基硅烷处理的所述硅基材料表面。
所述环氧基硅烷包括:3-缩水甘油丙基三甲氧基硅烷((3-Glycidyloxypropyl)trimethoxysilane,GPTMS)、3-环氧丙氧基丙基二甲基乙氧基硅烷((3-Glycidoxypropyl)dimethylethoxysilane,GPDMES)、3-(2,3)-环氧丙基甲基二甲氧甲基硅烷((3-Glycidoxypropyl)dimethoxymet-hylsilane,GPDMMS)、或3-(2,3)环氧丙氧基丙基三甲氧基硅烷(3-(2,3-Epoxypropoxy)propyltrimethoxysilane,GPTS)。
所述富含氨基长链化合物包括:壳聚糖、多聚赖氨酸、多聚组氨酸、聚亚乙基亚胺或聚烯丙基胺。
所述液相为由所述环氧基硅烷、水、乙醇或异丙醇制得的液相,该液相含按质量百分比计的0.4%~0.6%所述环氧基硅烷。
用环氧基硅烷的所述处理包括,于45℃~55℃下、以115~125rpm的转速摇动下浸泡20~30h后,再用水、乙醇或异丙醇清洗两次,20℃~30℃下晾干或55℃~65℃烘干。
按质量百分比计,所述富含氨基长链化合物溶液为0.05%~0.5%浓度的氨基的聚合物溶液。
用富含氨基长链化合物溶液的所述处理包括,所述用富含氨基长链化合物溶液为含按质量百分比计的0.020%~0.030%的壳聚糖、pH值为4.5~5.5、温度为4.5℃~55℃的PBS缓冲液;于该缓冲溶液中,在115~125rpm的转速下摇动23~24h浸泡实现与壳聚糖分子的共价接枝后,用去离子水洗涤滤纸,再于55~65℃烘箱中烘干。
所述硅基材料包括含二氧化硅、有机硅化合物及表面可羟基化硅基的滤纸/膜、石英纤维、玻璃纤维、硅树脂、硅橡胶、硅纤维素和聚硅酸纤维。
较之最接近的现有技术,本发明提供的技术方案具有以下优异效果:
本发明提供的技术方案利用环氧基硅烷的环氧基团与带氨基化合物形成共价结合,致使所得的硅基材料不仅具有好的生物相容性特性,而且也具有优异的抑菌抗菌效果。
附图说明
图1为氨基修饰的抗菌硅基纤维表面示意图;
图2为核酸扩增相容性测试。
具体实施方式
所述具有抗菌性保护膜的硅基材料为滤纸。所述滤纸包括玻璃纤维、石英纤维材质的滤纸或滤膜。另有说明除外,本说明书中的浓度均以质量百分比表征。
实施例1、制备具有抗菌性保护膜的硅基材料为滤纸。
1)、表面环氧化滤纸
将滤纸在按质量百分比计浓度为0.5%的GPTS(3-(2,3)环氧丙氧基丙基三甲氧基硅烷,3-(2,3-Epoxypropoxy)propyltrimethoxysilane)的50℃下的异丙醇中、以120rpm转的速度摇动条件下浸泡24h后,再用异丙醇清洗两次,25℃下晾干或60℃烘干实现对所述滤纸表面的环氧基硅烷化处理,得表面环氧基硅烷化抗菌膜的滤纸。
2)、固定所得的表面环氧基硅烷化抗菌膜
将所得的表面环氧基硅烷化抗菌膜的滤纸浸泡于50℃下的、壳聚糖浓度为0.025%的、pH值为5.0的PBS缓冲液中,并在120rpm的转速下摇动24h与壳聚糖分子实现共价接枝后,用去离子水洗涤滤纸,再于60℃烘箱中烘干即得如图1所示的表面膜固化的抗菌膜滤纸。
实施例2、制备具有抗菌性保护膜的硅基材料为滤纸。
1)、表面环氧化滤纸
将滤纸在按质量百分比计浓度为2.5%的GPTS(3-(2,3)环氧丙氧基丙基三甲氧基硅烷,3-(2,3-Epoxypropoxy)propyltrimethoxysilane)的50℃下的异丙醇中、以120rpm转的速度摇动条件下浸泡16h后,再用异丙醇清洗两次,25℃下晾干或60℃烘干实现对所述滤纸表面的环氧基硅烷化处理,得表面环氧基硅烷化抗菌膜的滤纸。
2)、固定所得的表面环氧基硅烷化抗菌膜
将所得的表面环氧基硅烷化抗菌膜的滤纸浸泡于50℃下的、壳聚糖浓度为0.05%的、pH值为5.0的PBS缓冲液中,并在120rpm的转速下摇动24h与壳聚糖分子实现共价接枝后,用去离子水洗涤滤纸,再于60℃烘箱中烘干即得如图1所示的表面膜固化的抗菌膜滤纸。
实施例3、制备具有抗菌性保护膜的硅基材料为滤纸。
1)、表面环氧化滤纸
将滤纸在按质量百分比计浓度为5%的GPTMS(3-缩水甘油丙基三甲氧基硅烷,(3-Glycidyloxypropyl)trimethoxysilane)的50℃下的异丙醇中、以120rpm转的速度摇动条件下浸泡24h后,再用异丙醇清洗两次,25℃下晾干或60℃烘干实现对所述滤纸表面的环氧基硅烷化处理,得表面环氧基硅烷化抗菌膜的滤纸。
2)、固定所得的表面环氧基硅烷化抗菌膜
将所得的表面环氧基硅烷化抗菌膜的滤纸浸泡于50℃下的、壳聚糖浓度为0.05%的、pH值为5.0的PBS缓冲液中,并在120rpm的转速下摇动24h与壳聚糖分子实现共价接枝后,用去离子水洗涤滤纸,再于60℃烘箱中烘干即得如图1所示的表面膜固化的抗菌膜滤纸。
实施例4、制备具有抗菌性保护膜的硅基材料为滤纸。
1)、表面环氧化滤纸
将滤纸在按质量百分比计浓度为0.5%的GPTMS(3-缩水甘油丙基三甲氧基硅烷,(3-Glycidyloxypropyl)trimethoxysilane)的50℃下的乙醇中、以120rpm转的速度摇动条件下浸泡24h后,再用乙醇清洗两次,25℃下晾干或60℃烘干实现对所述滤纸表面的环氧基硅烷化处理,得表面环氧基硅烷化抗菌膜的滤纸。
2)、固定所得的表面环氧基硅烷化抗菌膜
将所得的表面环氧基硅烷化抗菌膜的滤纸浸泡于50℃下的、壳聚糖浓度为0.05%的、pH值为5.0的PBS缓冲液中,并在120rpm的转速下摇动24h与壳聚糖分子实现共价接枝后,用去离子水洗涤滤纸,再于60℃烘箱中烘干即得如图1所示的表面膜固化的抗菌膜滤纸。
实施例5、制备具有抗菌性保护膜的硅基材料为滤纸。
1)、表面环氧化滤纸
将滤纸在按质量百分比计浓度为2%的GPTS(3-(2,3)环氧丙氧基丙基三甲氧基硅烷,3-(2,3-Epoxypropoxy)propyltrimethoxysilane)的50℃下的乙醇中、以120rpm转的速度摇动条件下浸泡24h后,再用乙醇清洗两次,25℃下晾干或60℃烘干实现对所述滤纸表面的环氧基硅烷化处理,得表面环氧基硅烷化抗菌膜的滤纸。
2)、固定所得的表面环氧基硅烷化抗菌膜
将所得的表面环氧基硅烷化抗菌膜的滤纸浸泡于50℃下的、壳聚糖浓度为0.025%的、pH值为5.0的PBS缓冲液中,并在120rpm的转速下摇动24h与壳聚糖分子实现共价接枝后,用去离子水洗涤滤纸,再于60℃烘箱中烘干即得如图1所示的表面膜固化的抗菌膜滤纸。
本发明制得的石英纤维滤纸抗菌性的检测。
依据GB/T 20944.2-2007《纺织品抗菌性能的评价》第2部分吸收法检测滤纸的抗菌性。将石英纤维滤纸及标准棉布均裁剪为18mm×18mm大小同一种规格的两种式样,在两种式样上均接种大肠杆菌(8099)密度为1.8×105CFU/样,接种金黄色葡萄球菌(ATCC6538)密度为1.9×105CFU/样,观察培养0h、18h后的细菌数量,分别计算两种式样的抑菌活性值和抑菌率。检测结果如下表1所示:
表1本发明实施例1~5的硅基材料滤纸与现有的标准布的抑菌活性和抑菌率
检测结果表明,本发明实施例1、2制得的式样对大肠杆菌和金黄色葡萄球菌抗菌性均可达97%以上;实施例3、4、5对大肠杆菌和金黄色葡萄球菌抗菌性>99%。
实施例6~10的制备滤纸方法的与上述实施例1相同,但所用的环氧基硅烷化试剂与富含氨基长链化合物有别,其效果分别列于下表2:
表2本发明实施例6~10的硅基材料滤纸的抑菌活性和抑菌率
备注:GPTMS(3-缩水甘油丙基三甲氧基硅烷,(3-Glycidyloxypropyl)trimethoxysilane)、GPDMES(3-环氧丙氧基丙基二甲基乙氧基硅烷,(3-Glycidoxypropyl)dimethylethoxysilane)、GPDMMS(3-(2,3)-环氧丙基甲基二甲氧甲基硅烷,
(3-Glycidoxypropyl)dimethoxymet-hylsilane)、GPTS(3-(2,3)环氧丙氧基丙基三甲氧基硅烷,
3-(2,3-Epoxypropoxy)propyltrimethoxysilane)
检测本发明制得的硅基纤维滤纸的核酸扩增相容性。
本发明用PCR(Real-time Quantitative Polymerase Chain Reaction)定量分析所得滤材的生物相容性特性。在PCR体系中,加入过量SYBR荧光染料,在SYBR荧光染料特异性地掺入DNA双链后,会发射出荧光信号,而链中未掺入SYBR染料的分子不会发射任何荧光信号,使荧光信号的增加与PCR产物的增加完全同步。以反应管内的荧光信号至设定的循环阈值(Cycle threshold,Ct值)时所经历的循环次数为标准,来比较各材料间PCR扩增生物相容性差异。
聚合物酶链反应体系包括各0.425μL的一对引物(10μM),12.5μL的Power 2×SYBRreal-time PCR premixture(BioTeke)和0.125μL 50μg/μL BSA,以及11.525μL去离子水。
下表3为本发明实施例1~10的滤纸与无修饰硅基纤维滤纸、无硅基纤维滤纸的Ct值(1ng标准品核酸扩增后)测试结果。
表3本发明实施例1~10的滤纸与无修饰硅基纤维滤纸、无硅基纤维滤纸的Ct值
如图2中可见,经过本发明修饰后的硅基纤维滤纸,有良好的PCR扩展生物相容性,以1ng标准品核酸扩增后Ct值为例,未修饰硅基纤维滤纸同无硅基纤维滤纸组的ΔCt=1.9,即未修饰硅基纤维扩增效率仅为无硅基纤维滤纸组的1/21.9×100%=27%,而实施例1至实施例10的滤纸较之无硅基纤维滤纸组的ΔCt为0.01~0.65,扩增效率在64%~99%之间。
结果表明本发明修饰材料在核酸扩增聚合物酶生物相容性上有明显优势。
最后应当说明的是:以上实施例仅用以说明本发明的技术方案而非对其限制,尽管参照上述实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解:依然可以对本发明的具体实施方式进行修改或者等同替换,而未脱离本发明精神和范围的任何修改或者等同替换,其均应涵盖在本发明的权利要求保护范围之内。
Claims (4)
1.一种硅基材料抗菌性保护膜的制备方法,其特征在于,所述方法包括,于液相条件下,用环氧基硅烷处理所述硅基材料表面;用富含氨基长链化合物溶液处理经环氧基硅烷处理的所述硅基材料表面;
用环氧基硅烷的所述处理包括,于45℃~55℃下、以115~125rpm的转速摇动下浸泡20~30h后,再用水、乙醇或异丙醇清洗两次,20℃~30℃下晾干或55℃~65℃烘干;
用富含氨基长链化合物溶液的所述处理包括,所述用富含氨基长链化合物溶液为含按质量百分比计的0.020%~0.030%的壳聚糖、pH值为4.5~5.5、温度为50℃的PBS缓冲液;于该缓冲液中,在115~125rpm的转速下摇动23~24h浸泡实现与壳聚糖分子的共价接枝后,用去离子水洗涤硅基材料,再于55~65℃烘箱中烘干。
2.如权利要求1的一种硅基材料抗菌性保护膜的制备方法,其特征在于,
所述环氧基硅烷包括:3-缩水甘油丙基三甲氧基硅烷((3-Glycidyloxypropyl)trimethoxysilane,GPTMS)、3-环氧丙氧基丙基二甲基乙氧基硅烷((3-Glycidoxypropyl)dimethylethoxysilane,GPDMES)、3-(2,3)-环氧丙基甲基二甲氧甲基硅烷((3-Glycidoxypropyl)dimethoxymet-hylsilane,GPDMMS)、或3-(2,3)环氧丙氧基丙基三甲氧基硅烷(3-(2,3-Epoxypropoxy)propyltrimethoxysilane,GPTS)。
3.如权利要求1的一种硅基材料抗菌性保护膜的制备方法,其特征在于,所述液相为由所述环氧基硅烷、水、乙醇或异丙醇制得的液相,该液相含按质量百分比计的0.4%~0.6%所述环氧基硅烷。
4.如权利要求1的一种硅基材料抗菌性保护膜的制备方法,其特征在于,所述硅基材料包括含二氧化硅、有机硅化合物及表面可羟基化硅基的滤纸/膜、石英纤维、玻璃纤维、硅树脂、硅橡胶、硅纤维素和聚硅酸纤维。
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