聚醚醚酮表面的亲水改性和胶原蛋白固定化

doi:10.7503/cjcu20160120

高等学校化学学报 ›› 2016, Vol. 37 ›› Issue (6): 1154.doi: 10.7503/cjcu20160120

聚醚醚酮表面的亲水改性和胶原蛋白固定化

孙辉^1,², 于庆松¹, 杨彪¹, 许国志^1,²

1. 北京工商大学材料与机械工程学院, 北京 100048
2. 国家塑料制品质量监督检验中心(北京), 北京 100048

收稿日期:2016-02-29 出版日期:2016-06-10 发布日期:2016-05-18
作者简介:联系人简介: 孙辉, 男, 博士, 副教授, 主要从事高分子表面改性及生物质精细化学品的研究. E-mail:cnhsun@yahoo.com
基金资助:
国际标准化组织(ISO)标准项目基金(批准号: 19000551742, 19000551406)、国家自然科学基金(批准号: 31570575)和北京工商大学高分子功能薄膜创新团队项目(批准号: 19008001071)资助

Surface Hydrophilic Modification of Poly(ether ether ketone) and Immobilization of Collagen^†

SUN Hui^1,^2,^*, YU Qingsong¹, YANG Biao¹, XU Guozhi^1,²

1. College of Materials Science and Mechanical Engineering, 100048, China
2. China National Center for Quality Supervision and Test of Plastic Product, Beijing Technology and Business University, Beijing 100048, China

Received:2016-02-29 Online:2016-06-10 Published:2016-05-18
Contact: SUN Hui
Supported by:
† Supported by the International Organization for Standardization(ISO) Standards Projects(Nos.19000551742, 19000551406), the National Natural Science Foundation of China(No.31570575) and the Innovative Research Team of Polymeric Functional Film of Beijing Technology and Business University, China(No.19008001071)

摘要/Abstract

摘要：

采用紫外光接枝法对聚醚醚酮(PEEK)表面进行化学修饰和生物分子固定化. 首先向PEEK表面引入亲水性的丙烯酰胺, 并以此为反应位点通过戊二醛将胶原和胶原蛋白固定在PEEK表面. 用接触角测定仪、扫描电镜、荧光标记和X射线光电子能谱等对改性薄膜进行了表征. 结果表明, PEEK上丙烯酰胺的接枝密度高达50.9 μg/cm²; 改性薄膜表面浸润性显著提高, 水接触角最低降至(22±3)°. 荧光标记胶原固定的PEEK薄膜荧光发射光谱强度最高, 并在X射线光电子能谱中检测到N元素, 表明胶原已固定化, 固定胶原蛋白的浓度为10.2 μg/cm².

关键词: 聚醚醚酮, 胶原, 表面修饰, 荧光标记

Abstract:

Surface modification of poly(ether ether ketone)(PEEK) was performed to increase the surface wettability. Acrylamide(AAm) was grafted on the surface of PEEK film by ultraviolet grafting to improve the hydrophilicity through the introduction of hydrophilic groups. Then, glutaraldehyde was used to immobilize collagen and hydrolyzed collagen on surface of the material. Fluorescein-labelled collagen was also used to verify the immobilization. The surfaces of PEEK film before and after modification were characterized by contact angle meter, scanning electron microscope, fluorescence spectrophotometer and X-ray photoelectron spectrometer. The results show that the surface morphology and the hydrophilicity are changed significantly after surface modification. Polyacrylamide grated on PEEK has a density of as high as 50.9 μg/cm². PEEK-g-PAAm becomes hydrophilic with a decreased water contact angle of (22±3)°. Surface immobilized with hydrolyzed collagen labeled with fluorescein isothiocyanate exhibits strong fluorescence effect. Modified films immobilized with collagen showed nitrogen peak, which was not observed for unmodified PEEK film in X-ray photoelectron spectroscopy, indicating the successful immobilization of collagen. The concentration of collagen immobilized on PEEK was determined to be 10.2 μg/cm².

Key words: Poly(ether ether ketone), Collagen, Surface modification, Fluorescence labeling

中图分类号:

O631

TrendMD:

孙辉, 于庆松, 杨彪, 许国志. 聚醚醚酮表面的亲水改性和胶原蛋白固定化. 高等学校化学学报, 2016, 37(6): 1154.

SUN Hui, YU Qingsong, YANG Biao, XU Guozhi. Surface Hydrophilic Modification of Poly(ether ether ketone) and Immobilization of Collagen^†. Chem. J. Chinese Universities, 2016, 37(6): 1154.

图/表 11

Scheme 1 Structure of PEEK

Scheme 2 Synthetic routes for the immobilization of collagen onto PEEK

Fig.1 Variation of contact angle with irradiation time at different monomer concentrations(A) and comparison of contact angle of PEEK-AAm with(a) or without BP(b)(B)

Fig.2 Images showing the evolution of water contact angle of PEEK-PAAm with irradiation time0.5 mol/L AAm. UV irradiation time/min: (A) 0; (B) 1; (C) 3; (D) 6; (E) 9; (F) 12.

Fig.3 Dependence of grafted PAAm on irradiation time in presence(a)/absence(b) of benzophenone

Fig.4 SEM images of blank PEEK and modified PEEK(A) PEEK; (B) PEEK-PAAm; (C) PEEK-GA; (D) PEEK-Col; (E) PEEK-HC.

Fig.5 UV spectrum of HC-FITC labeled solution

Fig.6 Fluorescence emission spectra of blank and modified PEEKa. PEEK-AAm; b. PEEK-GA; c. PEEK; d. PEEK-Col; e. PEEK-HC-FITC.

Fig.7 XPS overview spectra of PEEK(A) and PEEK-Col(B)

Fig.8 High resolution XPS nitrogen spectra of PEEK(A) and PEEK-Col(B)

Table 1 XPS atomic percentage of PEEK and PEEK-Col

Sample	C(%)	O(%)	N(%)
PEEK	79.55	16.02	0.44
PEEK-Col	64.82	20.51	9.43

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聚醚醚酮表面的亲水改性和胶原蛋白固定化

Surface Hydrophilic Modification of Poly(ether ether ketone) and Immobilization of Collagen^†

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聚醚醚酮表面的亲水改性和胶原蛋白固定化

Surface Hydrophilic Modification of Poly(ether ether ketone) and Immobilization of Collagen†

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Surface Hydrophilic Modification of Poly(ether ether ketone) and Immobilization of Collagen^†