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Determination of aliphatic aldehydes C1–C5 with headspace solid phase microextraction in tap water: derivatization in-solution versus on-fiber

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Short-chain aliphatic aldehydes are hazardous environmental pollutants and important biomarkers of various diseases. The development of effective methods for the determination of short-chain aliphatic aldehydes in samples with complex matrices remains an urgent task owing to their harmful effects on living organisms. To choose the optimal method of sample preparation, two types of derivatization of C1–C5 aliphatic aldehydes, in-solution and on-fiber, with O-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine are compared in this work in combination with headspace solid phase microextraction and GC/FID detection. Research on a limited number of analytes of one homologous series, C1–C5 aliphatic aldehydes, and detailed optimization of microextraction and derivatization parameters can significantly increase the extraction recovery, enrichment factors, and improve the sensitivity of the method. It was demonstrated that headspace solid phase microextraction with in-solution derivatization is more effective than with on-fiber derivatization. The extraction recovery of C3–C5 aldehydes was above 70%, and the enrichment factor was more than 7.5 × 103 for C1–C5 aldehydes. The developed method allows to detect C1–C5 aliphatic aldehydes with limits of detection from 100 to 400 ng L−1. The method is simple and fast, and meets the requirements of “green chemistry.” Tap water was analyzed for aliphatic aldehydes C1–C5 using the developed method. It was shown that the formaldehyde concentration was less than the environmental quality standards for fresh water (EU). In addition, it has been established that the formation of oximes takes place simultaneously on-fiber and in-solution during headspace solid phase microextraction with on-fiber derivatization. Primarily, it concerns the derivatives of short-chain aliphatic aldehydes.

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The authors would like to thank the LLC “ALSI-CHROM”, Kyiv, Ukraine, especially, Dr. Esaulenko Andriy, Director of the LLC “ALSI-CHROM” for financial support of this research.

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Correspondence to Maryna Zui.

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Zakharkiv, I., Zui, M. & Zaitsev, V. Determination of aliphatic aldehydes C1–C5 with headspace solid phase microextraction in tap water: derivatization in-solution versus on-fiber. Chem. Pap. 78, 435–445 (2024).

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