SPE-Based Method for Detecting Harmful Textile Residues
Scientists from the University of Valencia in Valencia, Spain recently developed a new solid-phase extraction-based method for determining harmful dyes and additives released from polyester fibers. Their findings were published in the Journal of Chromatography A (1).
Extreme macro of polyester stable fiber on blue background. Selective focus, shallow depth of field. Abstract dreamy background | Image Credit: © Taigi - stock.adobe.com
Textile fibers can be found in everything from clothing and decoration garments to medical equipment. While natural and artificial fiber use in the textile industry has increased in the past 10 years, synthetic fibers from petroleum sources are still the predominant type used, accounting for 60% of total global fiber production. These artificial fibers are often stretchier, more waterproof, and more stain-resistant, making them very consumer-friendly. The most common types of synthetic fiber are nylon and polyester (PES), with polyester having 54% of the global fiber market share in 2021 and nylon having 5% (2).
Persistence and accumulation of these fibers cause concern for their occurrence in the environment. Synthetic fibers present in different environmental matrices influence elevated microplastic global pollution, with 35% of microplastics (MPs) found in the ocean being fibers released during synthetic fabric laundering. In fact, textiles made of plastic fibers can lead to MP fiber shedding at every stage: when they are being worn, washed, or disposed of (3). These leachates (contaminated liquids generated from solid wastes due to physical, chemical, or biological changes) pose dangers to human health if left untreated (4). For example, plastic bioaccumulation in the human body can cause issues like lung cancer, fatigue, and inflammatory bowel disease, among others (5).
In this study, a novel method was developed, validated, and applied to identify and quantify microfibers and other microplastics (MPs) in a hydrolytic alkaline degradation solution (neutralized). The employed solution was utilized in an accelerated degradation simulation of two different types of PES fiber, Afterwards, thirteen compounds were extracted and quantified using solid-phase extraction (SPE) followed by high-performance liquid chromatography coupled to high-resolution mass spectrometry (HPLC–HRMS/MS). The SPE protocol was used to extract additives from seawater-like solutions after degradation simulation of synthetic fibers (real seawater often used for UV exposure degradation in laboratory conditions could be analyzed by the same procedure). After procedures, the method was found to be accurate, precise, linear, and sensitive, as indicated by method validation parameters.
Intra-day (Intra-R) and inter-day (Inter-R) precision ranged from 0.02–6.23% and 0.08–8.85%, respectively, with linearity (R2) values being greater than 0.9980. The limits of detection (LOD = 0.7–3.3 ng mL−1) and quantification (LOQ = 0.5–10 ng mL−1) were also determined. The low values found enabled detection of dyes/additives and other compounds at very low concentrations, showing how sensitive the method is. Further, with precision levels below 10% and recovery within the ranges of 65–120%, the method’s reliability was reinforced.
This newly developed protocol was also applied for determining different leachates of polyester fibers after accelerated hydrolytic degradation. Ten dyes/additives were detected and quantified in the degradation solution of the polyester fibers. Additionally, non-target analysis allowed 55 compounds to be identified in positive ion mode and 24 in negative mode. When filters were applied during data processing, reliable compound matches were ensured.
This method proved to be simple and robust, the scientists wrote, making it a valuable tool for identifying various leachates coming from textile fiber degradation. In the future, this method can be applied to assess the actual contamination status of aquatic ecosystems, specifically those related to the textile industry, and their possible associated toxicities.
References
(1) Soursou, V.; De Falco, F.; Campo, J.; Picó, Y. A Multi-Residue Method Based on Solid Phase Extraction Followed by HPLC-HRMS/MS Analysis for the Determination of Dyes and Additives Released from Polyester Fibres After Degradation. J. Chromatogr. A 2025, 1741, 465629. DOI: 10.1016/j.chroma.2024.465629
(2) Synthetics. Textile Exchange 2022. https://textileexchange.org/synthetics/ (accessed 2025-1-14)
(3) What You Need to Know about Microplastics and Textile. Fibershed 2022. https://fibershed.org/2022/01/11/what-you-need-to-know-about-microplastics-and-textile/ (accessed 2025-1-14)
(4) Leachate. ScienceDirect 2018. https://www.sciencedirect.com/topics/earth-and-planetary-sciences/leachate (accessed 2025-1-14)
(5) Winiarska, E.; Jutel, M.; Zemelka-Wiacek, M. The Potential Impact of Nano- and Microplastics on Human Health: Understanding Human Health Risks. Environ. Res. 2024, 251 (2), 118535. DOI: 10.1016/j.envres.2024.118535
