Volume 36, Issue 1 (4-2025)
Studies in Medical Sciences 2025, 36(1): 63-77 |
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Research code: 11535
Ethics code: IR.UMSU.REC.1401.210
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Hamze-Khalifani B, Vardast M R. Development of a Solid Phase Microextraction Method WITH Carbon Fiber for Extraction and Preconcentration of 1,4-Dioxane FROM Cosmetic SAMPLES. Studies in Medical Sciences 2025; 36 (1) :63-77
URL: http://umj.umsu.ac.ir/article-1-6421-en.html
URL: http://umj.umsu.ac.ir/article-1-6421-en.html
Assistant Professor of Medicinal Chemistry, School of pharmacy, Urmia University of Medical Science, Urmia, Iran (Corresponding Author) , mrvardast@gmail.com
Abstract: (386 Views)
Background & Aims: 1,4-Dioxane, a cyclic ether commonly employed in chemical and syntheses processes as a solvent, is now a probable human carcinogen. It is frequently found as a byproduct of detergents and personal care products, so reliable analytical methods to locate and quantify it in cosmetics are important for compliance, regulatory, and public health reasons.
Materials & Methods: We developed an optimized headspace solid-phase microextraction (HS-SPME) method that has the modified carbon fiber as the extraction phase when coupled with GC-FID. The analytical method also allows us to take the best of liquid-liquid extraction and HS-SPME together for better sensitivity in cosmetic matrices.
Results: The method provided adequate sensitivity, detection limit (LOD) of 0.4 μg/kg and quantitation limit (LOQ) of 1.2 μg/kg. The linear dynamic range was 1.5-300 μg/kg, R² > 0.999, precision of 5.8% as RSD at 25 μg/kg, n=6. The carbon fiber modified with aniline/pyrrole/graphene oxide extraction phase had longer extraction times, but was more efficient than conventional fibers due to its π-π modified interactions as well as more areas of contact and surface hydrophobicity. Conclusion: This method for the headspace solid-phase microextration-gas chromatography-flame ionization detection (HS-SPME-GC-FID) provides a sensitive, reliable, and solvent free method for monitoring, locating, and quantifying 1,4-dioxane in cosmetics to comply with regulatory standards of monitoring carcinogens. The modified carbon fiber exhibits exceptional performance for trace-level extraction of this challenging analyte.
Materials & Methods: We developed an optimized headspace solid-phase microextraction (HS-SPME) method that has the modified carbon fiber as the extraction phase when coupled with GC-FID. The analytical method also allows us to take the best of liquid-liquid extraction and HS-SPME together for better sensitivity in cosmetic matrices.
Results: The method provided adequate sensitivity, detection limit (LOD) of 0.4 μg/kg and quantitation limit (LOQ) of 1.2 μg/kg. The linear dynamic range was 1.5-300 μg/kg, R² > 0.999, precision of 5.8% as RSD at 25 μg/kg, n=6. The carbon fiber modified with aniline/pyrrole/graphene oxide extraction phase had longer extraction times, but was more efficient than conventional fibers due to its π-π modified interactions as well as more areas of contact and surface hydrophobicity. Conclusion: This method for the headspace solid-phase microextration-gas chromatography-flame ionization detection (HS-SPME-GC-FID) provides a sensitive, reliable, and solvent free method for monitoring, locating, and quantifying 1,4-dioxane in cosmetics to comply with regulatory standards of monitoring carcinogens. The modified carbon fiber exhibits exceptional performance for trace-level extraction of this challenging analyte.
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