Determination of hydroxy-PCBs in urine by gas chromatography/mass spectrometry with solid-phase extraction and derivatization |
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| Authors: | Jee Eun Hong Song-Ja Park Won Lee |
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| Affiliation: | a Bioanalysis and Biotransformation Research Center, Korea Institute of Science and Technology, P.O. Box 131, Cheongryang, Seoul 136-791, Korea
b Department of Chemistry, Kyunghee University, Seoul 130-701, Korea |
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| Abstract: | A sensitive derivatization and extraction method is proposed for the determination of hydroxy-PCBs in urine. Phenolic hydroxyl groups of PCBs were allowed to react with five different reagents such as iodomethane, iodoethane, iodopropane, BSTFA and MTBSTFA. Propylated products at 100 °C for 30 min showed the best sensitivity with mass selective detector. Extraction recoveries and relative standard deviations of hydroxy-PCBs by SPE using C2 column were in the range of 78.0-112.3% and 2.5-9.6%, respectively. Instrumental detection limits for derivatized hydroxy-PCBs were in the range of 1-2 pg and were 10-1000 times more sensitive than those of non-derivatized hydroxy-PCBs. The correlation coefficients of the linear regression curves exceed 0.99, and the intra- and inter-day precisions were evaluated by RSDs within 10% at the concentrations of 0.4 and 4.0 ng/mL. |
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| Keywords: | Hydroxy-PCBs GC/MS Derivatization SPE Urine |
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