EDC-NHS交联壳聚糖-聚氧化乙烯-丝素蛋白静电纺丝纳米纤维的制备及生物相容性

孙范忱; 郭静; 杨强; 于跃; 赵亚博

doi:10.13801/j.cnki.fhclxb.20200421.002

EDC-NHS交联壳聚糖-聚氧化乙烯-丝素蛋白静电纺丝纳米纤维的制备及生物相容性

doi: 10.13801/j.cnki.fhclxb.20200421.002

孙范忱^1,,
郭静^{1, 2, ,},
杨强^2,,
于跃^{1, 2,},
赵亚博^1,

1.
大连工业大学　纺织与材料工程学院，大连 116034
2.
辽宁省功能纤维及复合材料工程技术中心，大连 116034

基金项目: 国家自然科学基金(51773024; 51373027)；辽宁省科技创新团队项目(LT2017017)

详细信息

通讯作者:
郭静，博士，教授，博士生导师，研究方向为高分子材料改性和纤维材料加工成型　E-mail：guojing8161@163.com

中图分类号: TB332
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- 被引次数: 0
出版历程
- 收稿日期: 2019-12-04
- 录用日期: 2020-02-02
- 网络出版日期: 2020-04-21
- 刊出日期: 2020-11-15

Preparation and biocompatibility of EDC-NHS crosslinked chitosan-polyethyleneoxide-silk fibroin electrospun nanofibers

SUN Fanchen^1
,,
GUO Jing^{1, 2
, ,},
YANG Qiang^2
,,
YU Yue^{1, 2
,},
ZHAO Yabo^1
,

1.
School of Textile and Material Engineering, Dalian Polytechnic University, Dalian 116034, China
2.
Functional Fiber and its Composite Materials Engineering Technology Research Center of Liaoning Province, Dalian 116034, China

摘要

摘要: 为提高壳聚糖(CS)-丝素蛋白(SF)复合纳米纤维的可纺性，解决其易溶胀从而导致纳米纤维尺寸稳定性较差的问题，采用聚氧化乙烯(PEO)提高纳米纤维的可纺性，用静电纺丝来制备纳米纤维，然后通过1-(3-二甲基氨基丙基)-3-乙基碳化二亚胺(EDC)和 N-羟基丁二酰亚胺(NHS)进行交联改性，制备了CS-PEO-SF三元体系的纳米纤维。利用FTIR、XRD、单纤维强力机、SEM分别表征了CS-PEO-SF纳米纤维的分子间相互作用、结晶性能、纳米纤维的力学性能和形貌，同时考察纳米纤维的溶胀度；利用细胞毒性和细胞培养测试表征了CS-PEO-SF纳米纤维的生物相容性。结果表明：PEO的加入可以有效提高CS-SF的可纺性，CS-PEO-SF纳米纤维的平均直径范围为240~510 nm，各组分纤维形态较好；随着SF含量的增加，CS-PEO-SF纳米纤维结晶性能、拉伸强度和断裂伸长率逐渐增大。经交联后的CS-PEO-SF纳米纤维结晶能力和溶胀度降低，力学性能提高。交联前后CS-PEO-SF纳米纤维均不具毒性，有良好的细胞相容性。
- 壳聚糖 /
- 聚氧化乙烯 /
- 丝素蛋白 /
- 纳米纤维 /
- 交联 /
- 生物相容性
Abstract: In order to improve the spinnability of chitosan (CS)-silk fibroin (SF) composite nanofibers and solve the problem of poor dimensional stability of nanofiber membrane caused by its easy swelling, polyethylene oxide (PEO) was used to improve the spinnability of the composite fibers in this study. Electrospinning was used to prepare CS-PEO-SF nanofibers, which were cross-linked and by 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (EDC) and N-hydroxysuccinimide (NHS). The intermolecular interaction, crystallization properties, mechanical properties and morphology of CS-PEO-SF nanofibers were characterized by FTIR, XRD, single fiber strength machine and SEM. The swelling degree and biocompatibility of CS-PEO-SF nanofibers was also characterized by cytotoxicity and cell culture tests. The results show that the addition of PEO can effectively improve the spinnability of CS-SF. The average diameter of CS-PEO-SF nanofibers is from 240 nm to 510 nm. The fiber morphology of each component is good. With the increase of SF content, the crystalline properties, tensile strength and breaking elongation of CS-PEO-SF nanofibers gradually increase. After crosslinking, the crystallinity and swelling degree of the CS-PEO-SF nanofibers decrease, and the mechanical properties increase. Before and after cross-linking, the CS-PEO-SF nanofibers has no toxicity and has good cell compatibility.
- chitosan /
- polyethylene oxide /
- silk fibroin /
- nanofibers /
- cross-linking /
- biocompatibility

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图 1 碳化二亚胺(EDC)交联反应原理

Figure 1. Principle of carbodiimide (EDC) cross-linking reaction

NHS—N-hydroxysuccinimide

下载: 全尺寸图片幻灯片

图 2 交联前后壳聚糖-聚氧化乙烯-丝素蛋白(CS-PEO-SF)纳米纤维的FTIR图谱

Figure 2. FTIR spectra of chitosan-polyethylene oxide-silk fibroin (CS-PEO-SF) nanofiber before and after cross-linking

下载: 全尺寸图片幻灯片

图 3 CS和交联前后的CS-PEO-SF纳米纤维的XRD图谱

Figure 3. XRD patterns of CS and CS-PEO-SF nanofibers before and after cross-linking

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图 4 加入PEO前后CS-SF纳米纤维的SEM图像

Figure 4. SEM images of CS-SF nanofibers before and after PEO addition

下载: 全尺寸图片幻灯片

图 5 不同SF含量的CS-PEO-SF纳米纤维的SEM图像

Figure 5. SEM images of CS-PEO-SF nanofibers with different SF contents

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图 6 不同SF含量CS-PEO-SF纳米纤维力学性能

Figure 6. Mechanical properties of CS-PEO-SF nanofibers with different SF contents

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图 7 不同质量分数EDC交联CS-PEO-SF纳米纤维的溶胀度

Figure 7. Swelling degree of cross-linked CS-PEO-SF nanofibers with different mass fractions of EDC

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图 8 CS-PEO-SF纳米纤维的细胞毒性

Figure 8. Cytotoxicity of CS-PEO-SF nanofibers

a—Blank; b—CS-PEO-SF1; c—CS-PEO-SF2; d—CS-PEO-SF4; e—CS-PEO-SF6; f—CS-PEO-SF7

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图 9 CS-PEO-SF纳米纤维体外共培养的SEM图像

Figure 9. SEM images of in vitro co-culture of CS-PEO-SF nanofibers

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表 1 纺丝液各成分的质量比

Table 1. Mass ratios of each components of spinning solution

Smaple	CS	PEO	SF
CS-PEO-SF1	10	1	0
CS-PEO-SF2	10	1	1
CS-PEO-SF3	10	1	1.5
CS-PEO-SF4	10	1	2
CS-PEO-SF5	10	1	2.5
CS-PEO-SF6	10	1	3
CS-PEO-SF7	10	1	3
Notes: CS—Chitosan; PEO—Polyethylene oxide; SF—Silk fibroin; CS-PEO-SF6—CS-PEO-SF nanofiber before crosslinking; CS-PEO-SF7—Cross-linked CS-PEO-SF nanofiber.

下载: 导出CSV

表 2 细胞增殖率与细胞毒性水平的对应关系

Table 2. Correspondence between cell proliferation rate and cytotoxicity level

Cell proliferation rate/%	Cytotoxicity level
≥100	0
75–99	1
50–74	2
25–49	3
1–24	4
0	5

下载: 导出CSV

表 3 CS-PEO-SF纳米纤维的平均直径

Table 3. Average diameters of CS-PEO-SF nanofibers

Mass ratio of CS to SF	Average diameter/μm
10∶0	0.24
10∶1.0	0.25
10∶1.5	0.34
10∶2.0	0.42
10∶2.5	0.45
10∶3.0	0.51

下载: 导出CSV

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