한빛사 논문
Abstract
Hyunjeong Jua,b, Byungjoo Kima, Jeongkwon Kimb, Song-Yee Baeka,*
a Division of Chemical and Medical Metrology, Korea Research Institute of Standards and Science, Yuseong, Daejeon 34113, South Korea
b Department of Chemistry, Chungnam National University, Yuseong, Daejon 34134, South Korea
*Corresponding author : Song-Yee Baek
Abstract
We developed an isotope-dilution gas chromatography/high-resolution mass spectrometry (ID-GC/HRMS) method for the accurate quantification of four polycyclic aromatic hydrocarbons (PAHs) in olive oil. The clean-up steps were optimized to sufficiently remove co-extracted olive oil matrix using the EZ-POP-NP dual-layer and NH2 solid-phase extraction (SPE) cartridges. However, the cleaned sample still contained some matrix residues, which caused a measurement bias. When 13C-labeled PAHs were used as the internal standards instead of deuterated PAHs, the recovery results improved in both low- and high-resolution MS. Furthermore, the HRMS analysis facilitated to obtain more accurate results. The accuracy and precision of the optimized ID-GC/HRMS method were validated using PAH-fortified (0.5, 3, and 6 μg/kg) olive oil. The recoveries and relative standard deviations obtained for all the PAHs/levels were 98.4-101 % and ∼1 %, respectively. Measurement uncertainties were generally within 5 % (with a 95 % confidence level).
Keywords : PAHs; olive oil; Method validation; ID-GC-HRMS; 13C-labeled internal standard; matrix effect; measurement bias
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