| 18676208 |
Ito R, Kawaguchi M, Honda H, Koganei Y, Okanouchi N, Sakui N, Saito K, Nakazawa H: Hollow-fiber-supported liquid phase microextraction with in situ derivatization and gas chromatography-mass spectrometry for determination of chlorophenols in human urine samples. J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Sep 1;872(1-2):63-7. Epub 2008 Jul 15.
A simple and highly sensitive method that involves hollow-fiber-supported liquid phase microextraction (HF-LPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS) was developed for the determination of chlorophenols (CPs) such as 2,4-dichlorophenol (DCP), 2,4,6-trichlorophenol (TrCP), 2,3,4,6-tetrachlorophenol (TeCP) and pentachlorophenol (PCP) in human urine samples. Human urine samples were enzymatically de-conjugated with beta-glucuronidase and sulfatase. After de-conjugation, HF-LPME with in situ derivatization was performed. After extraction, 2 microl of extract was carefully withdrawn into a syringe and injected into the GC-MS system. The limits of detection (S/N=3) and quantification (S/N> 10) of CPs in the human urine samples are 0.1-0.2 ng ml (-1) and 0.5-1 ng ml (-1), respectively. The calibration curve for CPs is linear with a correlation coefficient of > 0.99 in the range of 0.5-500 ng ml (-1) for DCP and TrCP, and of 1-500 ng ml (-1) for TeCP and PCP, respectively. The average recoveries of CPs (n=6) in human urine samples are 81.0-104.0% (R.S.D.: 1.9-6.6%) with correction using added surrogate standards. When the proposed method was applied to human urine samples, CPs were detected at sub-ng ml (-1) level. |
1(0,0,0,1) |