CN108653816A - 一种采用静电纺丝制备双层人工抗菌修复膜的方法 - Google Patents
一种采用静电纺丝制备双层人工抗菌修复膜的方法 Download PDFInfo
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Abstract
本发明公开了一种采用静电纺丝制备双层人工抗菌修复膜的方法，包括以下步骤：(1)、将聚己内酯加入氯仿溶液搅匀后加入纳米锌；(2)、将纳米羟基磷灰石置于氯仿与丙酮的混合溶液中，超声波将其分散，然后加入聚乳酸搅搅匀；(3)、先将外层纺丝液配置好加入到注射器内，接收距离10‑20cm，调节电压为10‑15KV，调节流速，启动设备，开始纺丝，结束后，将内层纺丝液放入注射器内，接收距离10‑20cm，调节电压10‑18KV，调节流速，启动设备，在外层修复膜上继续纺丝，得到双层抗菌修复膜。本发明独创性的在静电纺丝中加入了纳米锌以及采用了双层纺丝膜的架构，将抗菌消炎能力提高了50～60％，可以快速引导骨生长和自动降解的功能。
Description
技术领域
本发明涉及牙科骨组织修复领域，涉及一种采用静电纺丝设备制备双层人工抗菌修复膜的方法一种。
背景技术
静电纺丝技术是一种独特的纳米纤维制造技术，最早于1897年由Rauleigh发现，于1914年由Zeleny详细研究，并于1934年由Formhals获得专利。近10多年来，静电纺丝技术凭借其电纺纳米材料的独特优势引发了人们大量的关注和研究，并已被广泛应用到多个领域，包括有组织工程、生物传感器、伤口敷料、药品递送和固定化酶等。至今，静电纺丝技术已经在骨再生、血管再生、周围神经再生、皮肤再生等诸多组织再生领域获得了突破和进展，并被认为是最有希望在组织再生领域取得重大成果的技术。
牙种植手术中拔牙窝、牙槽嵴缺损、骨开裂型和洞穿型缺损等问题都会影响种植体与骨的结合，限制种植体的应用。引导骨再生技术(Guided bone regeneration,GBR)的出现在一定程度上解决了上述难题。GBR技术是在1991年，由Dahlin和Lindhe提出，其原理是将膜置于骨缺损处，利用膜的物理屏障功能将骨缺损处与周围组织隔离，创造一个相对封闭的环境，由于上皮细胞和成纤维细胞迁移速度较快，而成骨细胞迁移速度较慢，通过这种方式来达到促进骨缺损区的愈合的目的。
聚己内酯以及聚乳酸有很好的生物相容性，并且在体内可以完全溶解，安全无毒。而纳米羟基磷灰石有较好的化学活性和生物相容性，而且对于骨组织的修复和引导生长有很好的促进作用，并对提升纳米膜的强度也有很大的作用。修复膜有内外两层，内膜引导骨生长，外膜抑菌消炎，但是目前修复膜的抗菌消炎能力较差，导致导骨生长和自动降解速度较为缓慢。
发明内容
本发明要解决的技术问题是克服现有技术中修复膜的抗菌消炎能力较差，导致导骨生长和自动降解速度较为缓慢的缺陷，提供一种采用静电纺丝制备双层人工抗菌修复膜的方法。
为了解决上述技术问题，本发明提供了如下的技术方案：
一种采用静电纺丝制备双层人工抗菌修复膜的方法，包括以下步骤：
(1)、外层纺丝液的制备：
称取一定量的聚己内酯加入氯仿溶液中混合，并充分搅拌；将一定浓度的纳米锌溶液倒入上述溶液中，并充分混合搅拌；
(2)、内层纺丝液的制备
称取一定量的纳米羟基磷灰石置于氯仿与丙酮的混合溶液中，超声波将其分散，然后加入一定量的聚乳酸，搅拌混匀两小时；
(3)、双层人工抗菌修复膜的制备
采用静电纺丝设备，先将外层纺丝液配置好加入到注射器内，接收距离10-20cm，调节电压为10-15KV，调节流速，启动设备，开始纺丝，结束后，将内层纺丝液放入注射器内，接收距离10-20cm，调节电压10-18KV，调节流速，启动设备，在外层修复膜上继续纺丝，得到双层抗菌修复膜。
进一步的，外层纺丝液中聚己内酯的加入量为氯仿质量的10～15wt％。
进一步的，外层纺丝液中纳米锌的加入量为0.08～2％。
进一步的，内层纺丝液中氯仿与丙酮的体积比为2:1。
进一步的，内层纺丝液中纳米羟基磷灰石和聚乳酸的总质量为氯仿和丙酮质的5～10wt％。
进一步的，所述外层纺丝液的液体流速为0.5～2mL/h；所述内层纺丝液的液体流速为0.5～2mL/h。
吸取2mL的外层纺丝液到规格为5mL的注射器中，然后将注射器安置在供液系统中的接收装置上；其中，所述接收装置的规格为包有20cm×30cm铝箔的钢板；调节供液系统中的控制器，使注射器的溶液流量为0.5-2mL/h，针头与接收装置之间的距离为10-20cm，环境温度为25℃；将高压电源的正极接到针头上，负极接在接收装置上，设置电纺电压为10-15KV；开启高压电源，然后启动供液系统中的控制器，在静电场力作用下，纺丝液飞向接收装置的过程中被拉伸，随着溶液的挥发，最终形成无纺布形式的纤维膜。
更换注射器内的纺丝液，吸取2mL的内层纺丝液到规格为5mL的注射器中，然后将注射器安置在供液系统中的接收装置上；其中，所述接收装置的规格为包有20cm×30cm铝箔的钢板；调节供液系统中的控制器，使注射器的溶液流量为0.5-2mL/h，针头与接收装置之间的距离为10-20cm，环境温度为25℃；将高压电源的正极接到针头上，负极接在接收装置上，设置电纺电压为10-18KV；开启高压电源，然后启动供液系统中的控制器，在静电场力作用下，纺丝液飞向接收装置的过程中被拉伸，随着溶液的挥发，最终在内膜上形成无纺布形式的纤维膜。
本发明所达到的有益效果是：本发明独创性的在静电纺丝中加入了纳米锌以及采用了双层纺丝膜的架构，将抗菌消炎能力提高了50～60％，可以快速引导骨生长和自动降解的功能。
具体实施方式
以下对本发明的优选实施例进行说明，应当理解，此处所描述的优选实施例仅用于说明和解释本发明，并不用于限定本发明。
实施例1
一种采用静电纺丝制备双层人工抗菌修复膜的方法，包括以下步骤：
(1)、外层纺丝液的制备：
称取7.5g聚己内酯及量取50mL氯仿，边搅拌边缓慢将聚己内酯加入氯仿溶液中，室温下置于磁力搅拌器上搅拌8h至溶液完全呈粘稠、透明状，再加入0.04mL的纳米锌溶液继续搅拌2h，即得10％的静电纺丝液；
(2)、内层纺丝液的制备
配置纺丝液溶剂氯仿：丙酮＝2:1(V/V)，取50mL，加入纳米羟基磷灰石(nHA)0.7g，超声20min，再加入2.8g聚乳酸，磁力搅拌2h，得到7％的内层纺丝液；
(3)、双层人工抗菌修复膜的制备
采用静电纺丝装置，接收装置接地后，控制接收距离为13cm，注射器内装入内层纺丝液，电压为14kv，调节液体流速为0.3mL/h，20号平针头，得到厚度约为1mm的纤维膜，然后更换注射器内层纺丝液为外层纺丝液，接受距离为15cm，电压为10kv，调节液体流速1mL/h，得到总厚度为2mm的双层静电纺丝纤维膜。
实施例2
一种采用静电纺丝制备双层人工抗菌修复膜的方法，包括以下步骤：
(1)、外层纺丝液的制备：
称取11.25g聚己内酯及量取50ml氯仿，边搅拌边缓慢将聚己内酯加入氯仿溶液中，室温下置于磁力搅拌器上搅拌8h至溶液完全呈粘稠、透明状，再加入0.04ml的纳米锌溶液继续搅拌2h，即得15％的静电纺丝液
(2)、内层纺丝液的制备
配置纺丝液溶剂氯仿：丙酮＝2:1(V/V)，取50ml，加入纳米羟基磷灰石(nHA)0.5g，超声20min。再加入2.0g聚乳酸，磁力搅拌2h，得到5％的内层纺丝液。
(3)、双层人工抗菌修复膜的制备
采用静电纺丝装置，接收装置接地后，控制接收距离为10cm，注射器内装入内层纺丝液，电压为15kv，调节液体流速为0.3ml/h，20号平针头，得到厚度约为1mm的纤维膜，然后更换注射器内层纺丝液为外层纺丝液，接受距离为10cm，电压为18kv，调节液体流速1ml/h，得到总厚度为2mm的双层静电纺丝纤维膜。
实施例3
一种采用静电纺丝制备双层人工抗菌修复膜的方法，包括以下步骤：
(1)、外层纺丝液的制备：
称取7.5g聚己内酯及量取50ml氯仿，边搅拌边缓慢将聚己内酯加入氯仿溶液中，室温下置于磁力搅拌器上搅拌8h至溶液完全呈粘稠、透明状，再加入0.04ml的纳米锌溶液继续搅拌2h，即得10％的静电纺丝液
(2)、内层纺丝液的制备
配置纺丝液溶剂氯仿：丙酮＝2:1(V/V)，取50ml，加入纳米羟基磷灰石(nHA)0.7g，超声20min。再加入2.8g聚乳酸，磁力搅拌2h，得到7％的内层纺丝液。
(3)、双层人工抗菌修复膜的制备
采用静电纺丝装置，接收装置接地后，控制接收距离为15cm，注射器内装入内层纺丝液，电压为10kv，调节液体流速为0.3ml/h，20号平针头，得到厚度约为1mm的纤维膜，然后更换注射器内层纺丝液为外层纺丝液，接受距离为20cm，电压为15kv，调节液体流速1ml/h，得到总厚度为2mm的双层静电纺丝纤维膜。
实施例4
(1)、外层纺丝液的制备：
称取11.25g聚己内酯及量取50ml氯仿，边搅拌边缓慢将聚己内酯加入氯仿溶液中，室温下置于磁力搅拌器上搅拌8h至溶液完全呈粘稠、透明状，再加入0.04ml的纳米锌溶液继续搅拌2h，即得15％的静电纺丝液
(2)、内层纺丝液的制备
配置纺丝液溶剂氯仿：丙酮＝2:1(V/V)，取50ml，加入纳米羟基磷灰石(nHA)0.5g，超声20min。再加入2.0g聚乳酸，磁力搅拌2h，得到5％的内层纺丝液。
(3)、双层人工抗菌修复膜的制备
采用静电纺丝装置，接收装置接地后，控制接收距离为20cm，注射器内装入内层纺丝液，电压为14kv，调节液体流速为0.3ml/h，20号平针头，得到厚度约为1mm的纤维膜，然后更换注射器内层纺丝液为外层纺丝液，接受距离为15cm，电压为10kv，调节液体流速1ml/h，得到总厚度为2mm的双层静电纺丝纤维膜。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，包括以下步骤：
(1)、外层纺丝液的制备：
称取一定量的聚己内酯加入氯仿溶液中混合，并充分搅拌；将一定浓度的纳米锌溶液倒入上述溶液中，并充分混合搅拌；
(2)、内层纺丝液的制备
称取一定量的纳米羟基磷灰石置于氯仿与丙酮的混合溶液中，超声波将其分散，然后加入一定量的聚乳酸，搅拌混匀两小时；
(3)、双层人工抗菌修复膜的制备
采用静电纺丝设备，先将外层纺丝液配置好加入到注射器内，接收距离10-20cm，调节电压为10-15KV，调节流速，启动设备，开始纺丝，结束后，将内层纺丝液放入注射器内，接收距离10-20cm，调节电压10-18KV，调节流速，启动设备，在外层修复膜上继续纺丝，得到双层抗菌修复膜。
2.如权利要求1所述的采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，外层纺丝液中聚己内酯的加入量为氯仿质量的10～15wt％。
3.如权利要求1或2所述的采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，外层纺丝液中纳米锌的加入量为0.08～2％。
4.如权利要求1所述的采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，内层纺丝液中氯仿与丙酮的体积比为2:1。
5.如利要求4所述的采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，内层纺丝液中纳米羟基磷灰石和聚乳酸的总质量为氯仿和丙酮质的5～10wt％。
6.如权利要求1所述的采用静电纺丝制备双层人工抗菌修复膜的方法，其特征在于，所述外层纺丝液的液体流速为0.5～2mL/h；所述内层纺丝液的液体流速为0.5～2mL/h。
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| CN112755254A (zh) * | 2021-01-18 | 2021-05-07 | 河南农业大学 | 一种具有抗菌作用的气管插管的制备方法 |
| CN114164562A (zh) * | 2021-08-12 | 2022-03-11 | 新疆大学 | PCL/ZnO-CSLE/PLA双层纳米纤维膜、其制备方法及应用 |
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