Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine

被引：19

作者：

Hong, JE

Pyo, H

Park, SJ ^{[1
]}

Lee, W

机构：

[1] Korea Inst Sci & Technol, Bioanal & Biotransformat Res Ctr, Seoul 136791, South Korea

[2] Kyung Hee Univ, Dept Chem, Seoul 130701, South Korea

来源：

ANALYTICA CHIMICA ACTA | 2005年 / 539卷 / 1-2期

关键词：

hydroxy-polychlorinated biphenyl compounds; gas chromatography/mass spectrometry; derivatization; headspace; solid-phase microextraction; urine;

D O I：

10.1016/j.aca.2005.02.065

中图分类号：

O65 [分析化学];

学科分类号：

070302 ; 081704 ;

摘要：

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.

引用

页码：55 / 60

页数：6

共 27 条

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