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GC-MS ANALYSIS OF VOLATILE COMPOUNDS FROM PINE TAR USING DLLME AND CYTOTOXICITY ASSESSMENT

Merve NESETOGLU, Selen AL, Gulsum ALTIPARMAK-ULBEGI, Aykut KUL, Olcay SAGIRLI

The European Chemistry and Biotechnology Journal - 2026;3(5):14-21

Department of Analytical Chemistry, Faculty of Pharmacy, Istanbul University, Istanbul, Türkiye

 

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 ona 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 %). Monoterpenealcohols 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 umbilicalvein/vascular endothelium cells (HUVEC) using 3-[4,5-dimethylthiazol-2-yl]-5-[3-carboxymethoxyphenyl]-2-[4-sulfophenyl]-2H-tetrazolium (MTS) cell viabilityassay, revealing a low level of toxicity. The resulting chemical fingerprint highlights the biotechnological potential of sesquiterpene scaffolds such as isolongifolene for microbial production and biocatalytic transformations. It also supportsenzyme-based functionalization strategies for isobornyl acetate and borneol, andopens 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 ofpine-tar terpenoids. In addition, the observed low cytotoxicity of pine tar contributes to the preliminary safety assessment of this natural product on humanendothelial cells.