红外光谱法快速测量维生素E/超高分子量聚乙烯粉体中维生素E的含量

doi:10.3964/j.issn.1000-0593(2025)07-1900-06

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摘要：维生素E掺杂改性的超高分子量聚乙烯（VE/UHMWPE）在医用领域有重要的应用。由VE/UHMWPE粉料压塑成型的人工关节已在临床使用，得益于VE的抗氧化性延长了该类型人工关节在体内的植入时间。因此研究VE/UHMWPE粉料中VE的实际添加量对人工关节的保护具有关键性的指导意义。为此，用傅里叶变换红外光谱（FTIR）对VE/UHMWPE粉体中的VE进行快速定量分析方法展开了研究。借助红外压片模具利用热压法将五种不同VE标称浓度的VE/UHMWPE粉料制成不同厚度的试样圆片，用透射模式进行红外测试并收集谱图。所有试样的光谱数据均采用OMNIC软件进行数据处理，FTIR解析时以峰形、峰位和峰强变化筛选定性或定量特征峰。根据数据分析结果表明，试样在1 260和1 210 cm^-1处的特征峰归属于VE分子结构中C—O醚键的伸缩振动和苯环上C—O键的伸缩振动，二者峰面积大小与VE含量有直接关系，可记作目标峰；在2 020和1 360 cm^-1处的特征峰归属于UHMWPE链上—CH₂—的弯曲振动峰和碳链末端亚甲基的伸缩振动，二者常被用作参比峰。对试样在1 260、1 210、2 020和1 360 cm^-1的特征峰进行峰面积积分，计算目标峰与参比峰的比值即I_{1 210/2 020}、I_{1 260/2 020}、I_{1 210/1 360}和I_{1 260/1 360}指数，将结果进行统计分析。分析测试结果的精密度、重复性用相对标准偏差（RSD）来判定。结果显示，用40～80 mg粉料压片制成的圆片试样效果最佳，重复性试验的RSD值小于5%；以I_{1 210/1 360}指数作定量分析评价参数准确性最佳，RSD值小于3%。该法为VE/UHMWPE粉体中实际VE的含量快速无损检测应用提供了参考。

关键词：红外光谱法；超高分子量聚乙烯；维生素E；定量分析

Abstract：Vitamin E doped modified ultra-high molecular weight polyethylene (VE/UHMWPE) has important applications in the medical field. Artificial joints formed by compression molding of VE/UHMWPE powder have been clinically used, and the antioxidant properties of VE have extended the implantation time of this type of artificial joint in vivo. Therefore, studying the amount of VE added in VE/UHMWPE powder has crucial guiding significance for protecting artificial joints. This paper investigated a method for rapid quantitative analysis of VE in VE/UHMWPE powders by Fourier transform infrared spectroscopy (FTIR).Five VE/UHMWPE powders with different VE concentrations were made into discs of different thicknesses using the hot press method, and infrared testing was performed in transmission mode. All spectral data of the samples were analyzed and studied by OMNIC. The characteristic peaks of VE located at 1 210 and 1 260 cm^-1 were used as target peaks, and the absorption peaks at 2 020 and 1 360 cm^-1 in UHMWPE were used as reference peaks, calculating I_{1 210/2 020}, I_{1 260/2 020}, I_{1 210/1 360} and I_{1 260/1 360}, respectively, and statistically analyzed. The precision and repeatability of results were determined using relative standard deviation (RSD). The results indicated that: sample preparation with 40~80 mg of powder gave the best results, with RSD values <5% in the repeatability test; the I_{1 210/1 360} index was used as the evaluation parameter for quantitative analysis with the best accuracy and RSD value <3%. The method provides a reference for the application of rapid nondestructive testing of the actual VE content in VE/UHMWPE powders.

Key words：Infrared spectroscopy; Ultra-high molecular weight polyethylenepowder; Vitamin E; Quantitative analysis

收稿日期: 2024-07-24 修订日期: 2025-01-23

中图分类号:

O657.3

基金资助: 国家自然科学基金项目（12375357），工信部生物医用材料创新任务揭榜挂帅项目（人工关节用高交联超高分子量聚乙烯（含/无VE）材料开发及产业化）资助

通讯作者: 鲁曼丽 E-mail: lumanli@sinap.ac.cn

作者简介: 胡志杰，1983年生，北京安通忆泰医疗科技有限公司工程师 e-mail: huzhijie@bjatyt.com

引用本文:

胡志杰，鲁曼丽，田继利，张文礼，王谋华. 红外光谱法快速测量维生素E/超高分子量聚乙烯粉体中维生素E的含量[J]. 光谱学与光谱分析, 2025, 45(07): 1900-1905.
HU Zhi-jie, LU Man-li, TIAN Ji-li, ZHANG Wen-li, WANG Mou-hua. Rapid Measurement of Vitamin E in Vitamin E/Ultra-High Molecular Weight Polyethylene Powders by Infrared Spectroscopy. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2025, 45(07): 1900-1905.

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