Hong, JE Pyo, H Park, SJ Lee, W 2024-01-21T05:04:21Z 2024-01-21T05:04:21Z 2021-09-03 2005-05-10 0003-2670 https://pubs.kist.re.kr/handle/201004/136475 A sensitive and solvent-free procedure for the determination of hydroxy metabolites of polychlorinated biphenyls (PCBs) in urine samples was studied using solid-phase microextraction (SPME) followed by on-fiber silylation and gas chromatography/mass spectrometry (GC/MS) determination. The analytical procedure involved headspace adsorption with coated fiber and headspace derivatization with bis(trimethylsilyl)trifluoroacetamide (BSTFA) in a sample vial. Experimental SPME parameters such as selection of coating material, addition of salt, extraction time and temperature of adsorption were optimized. The optimum extraction conditions for hydroxy-PCBs were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coated fiber at 90 degrees C for 60 min in urine, added 10% sodium chloride. Derivatization of the hydroxy-PCBs with BSTFA was performed on the SPME fiber at 60 degrees C for 10 min. The calibration curves for derivatized forms showed good linearity in the range of 0.01-10 ng mL(-1) and method detection limits proved to be 0.01-0.1 ng mL(-1) in 2 mL of urine. (c) 2005 Elsevier B.V. All rights reserved. English ELSEVIER GAS-CHROMATOGRAPHY PCB METABOLITES WATER 2,4&apos ,5-TRICHLOROBIPHENYL IDENTIFICATION METHYLTHIO METHIONINE CYSTEINE RAT Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine Article 10.1016/j.aca.2005.02.065 1 ANALYTICA CHIMICA ACTA, v.539, no.1-2, pp.55 - 60 ANALYTICA CHIMICA ACTA 539 1-2 55 60 scie scopus 000229175100009 2-s2.0-18344394970 Chemistry, Analytical Chemistry Article GAS-CHROMATOGRAPHY PCB METABOLITES WATER 2,4&apos ,5-TRICHLOROBIPHENYL IDENTIFICATION METHYLTHIO METHIONINE CYSTEINE RAT hydroxy-polychlorinated biphenyl compounds gas chromatography/mass spectrometry derivatization headspace solid-phase microextraction urine