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2016, vol. 5, br. 1, str. 31-38
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Ispitivanje mogućnosti primene različitih adsorbenasa i smeša rastvarača u pripremi uzoraka ZA GC/GC-MS analizu policikličnih aromatičnih ugljovodonika
The evaluation of different sorbents and solvent mixtures in PAH sample preparation for GC/GC-MS analysis
Projekat: Prirodni proizvodi biljaka i lišajeva: izolovanje, identifikacija, biološka aktivnost i primena (MPNTR - 172047)
Sažetak
Analiza policikličnih aromatičnih ugljovodonika (PAU) u složenim uzorcima zahteva prethodnu pripremu uzoraka. U ovom radu opisana je metoda ekstrakcije dispergovanom čvrstom fazom, kao koraka u pripremi uzoraka. Korišćene su tri smeše rastvarača i tri različita adsorbensa (PSA, C18 i PS-DVB) u cilju određivanja uticaja smeše rastvarača/adsorbensa na tačnost celokupne analize. Recovery-vrednosti varirale su u zavisnosti od adsorbensa i analiziranih jedinjenja. Najveća srednja recovery-vrednost zabeležena je za smešu cikloheksan/aceton - C18 (58.45%), sa najvećim pojedinačnim vrednostima za naftalen (76.05%), fluoranten (80.22%) i benzo[g,h,i]perilen (71.77%). Slične srednje recovery-vrednosti zabeležene su za kombinacije cikloheksan/aceton-PS-DVB (55.50%) i cikloheksan/aceton-PSA (55.30%). Smeša cikloheksana i acetona dala je najviše vrednosti sa sva tri korišćena adsorbensa, pa može biti korišćena u ekstrakciji PAU. Iako recoveryvrednosti nisu na visokom nivou, mogu poslužiti kao osnova za dalja istraživanja, s obzirom na to da PS-DVB, prema saznanjima autora, nije ranije korišćen u pripremi uzoraka za analizu PAU-a.
Abstract
GC/GC-MS-analysis of polycyclic aromatic hydrocarbons (PAHs) in complex samples requires a previous treatment of the samples. In order to establish the effects of sorbents/solvents on the overall accuracy of the method, dispersive solid phase extraction as a method for the sample preparation in PAHs determination is employed using three different solvent mixtures and sorbents (PSA, C18 and PS-DVB). Recovery values are dependent on compound and sorbents. The highest mean recovery was recorded for cyclohexane/acetone-C18 combination (58.45%) which is satisfactory, with the values above 70% for naphthalene (76.05%), fluoranthene (80.22%), pyrene (111.99%) and benzo[g,h,i]perylene (71.77%). Similar recoveries were obtained for cyclohexane/acetone-PS-DVB (55.50%) and cyclohexane/acetone- PSA (55.30%). Cyclohexane/acetone gave the highest recovery values for all three sorbents, so this solvent mixture could be used in PAH extraction from various matrices. Though the obtained recovery values for the investigated sorbent/solvent combinations were not impressive, they might be a good basis for future researches since, as far as we know, PS-DVB was not used in dSPE sample preparation for GC/GC-MS analysis of PAHs.
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