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Abstract The development of fibrous polymer scaffolds is highly valuable for applications in tissue engineering. Furthermore, there is an extensive body of literature for chemical methods to produce scaffolds that release nitric oxide. However, these methods often use harsh chemistries and leave behind bulk waste. Alkanolamine low‐temperature plasma (LTP) is unexplored and single‐step processing to form nitric oxide (NO) releasing constructs is highly desirable. The major question addressed is whether it is possible to achieve single‐step processing of spun polyester with alkanolamine plasma to achieve nitric oxide releasing capabilities. Herein we report the experiments, processes, and data that support the claim that it is indeed possible to produce such a bio‐functional material for potential biomedical applications, especially in cardiovascular implants. Among the tested alkanolamines, monoethylamine (MEA) plasma treated biomaterial outperformed in comparison with diethanolamine (DEA) and triethanolamine (TEA) in terms of NO release and cellular response.