ISSN print edition: 0366-6352
ISSN electronic edition: 1336-9075
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Determination of aliphatic aldehydes C1–C5 with headspace solid phase microextraction in tap water: derivatization in-solution versus on-fiber

Igor Zakharkiv, Maryna Zui, and Vladimir Zaitsev

Enamine Ltd, Kiev, Ukraine



Received: 8 February 2023  Accepted: 17 September 2023


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.

Keywords: Headspace solid phase microextraction; O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine derivatization; Aliphatic aldehydes C1–C5; Water analysis; GC/FID

Full paper is available at

DOI: 10.1007/s11696-023-03100-y


Chemical Papers 78 (1) 435–445 (2024)

Monday, July 15, 2024

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