Research Articles
DOI DOI: 10.62063/ecb-65

GC-MS analysis of volatile compounds from pine tar using DLLME and cytotoxicity assessment

Merve Nesetoglu1, Selen Al1, Gulsum Altiparmak-Ulbegi1, Aykut Kul2, Olcay Sagirli1
  1. 1 Istanbul University
  2. 2 Istanbul University,

Abstract

Pine tar has long been valued for its dermatological and antimicrobial properties; however, its volatile and semi-volatile component profile remains underexplored from a sustainable bioprospecting perspective. In this study, we combined dispersive liquid–liquid microextraction (DLLME) with GC-MS to develop a rapid, green workflow for profiling pine-tar volatiles, achieving greater than or equal to 50-fold enrichment from a 100 mg sample in under 10 min. GC-MS analysis on a TRB-5MS column (90 min gradient) resolved 45 compounds (match ≥ 77 %), with sesquiterpenes accounting for 71.3 % of the total area (isolongifolene 30.3 %; isobornyl acetate 16.0 %; borneol 12.4 %; (+)-longicyclene 12.5 %). Monoterpene alcohols comprised 4.4 %, while minor oxidized derivatives contributed < 3 %.
Compared to conventional hydrodistillation, DLLME reduced chlorinated solvent usage by 90 % and enhanced recovery of high-boiling terpenoids by ~ 25 %. Furthermore, the cytotoxic effect of pine tar was investigated on human umbilical vein/vascular endothelium cells (HUVEC) using 3-[4,5-dimethylthiazol-2-yl]-5[3-carboxymethoxyphenyl]-2-[4-sulfophenyl]-2H-tetrazolium (MTS) cell viability assay, revealing a low level of toxicity. The resulting chemical fingerprint high lights the biotechnological potential of sesquiterpene scaffolds such as isolongifolene for microbial production and biocatalytic transformations. It also supports enzyme-based functionalization strategies for isobornyl acetate and borneol, and opens avenues in sustainable perfumery, pharmaceutical intermediates, and biofuel applications. This semi-quantitative and eco-friendly platform offers a practical foundation for the biotechnological valorization and green production of pine-tar terpenoids. In addition, the observed low cytotoxicity of pine tar contributes to the preliminary safety assessment of this natural product on human endothelial cells.

How to Cite

Nesetoglu, M., Al, S., Altiparmak-Ulbegi, G., Kul, A., & Sagirli, O. (2026). GC-MS analysis of volatile compounds from pine tar using DLLME and cytotoxicity assessment. The European Chemistry and Biotechnology Journal, (5), 14–21. https://doi.org/10.62063/ecb-65
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