RESUMEN
The determination of benzophenones (BPs) in human urine sample by miniaturized hollow fiber assisted liquid-phase microextraction (HF-LPME) and gas chromatography-mass spectrometry (GC-MS) is described. As analytes, BP, its metabolites benzhydrol (BP-OH) and 2-hydroxybenzophenone (2OH-BP), and its derivatives 2-hydroxy-4-methoxybenzophenone (BP-3) and 2-hydroxy-4-methoxy-4'-methylbenzophenone (BP-10) were selected. The detection limit and the quantification limit of BPs in human urine sample are 5-10 and 20-50 pg mL(-1), respectively. The calibration curve for BPs is linear with correlation coefficient higher than 0.99 in the range of 0.02-10 or 0.05-10 ng mL(-1). The average recoveries of BPs in human urine samples spiked with 0.5 and 5 ng mL(-1) BPs are 89.8-100.2% (RSD: 2.5-9.3%) and 89.3-99.9% (RSD: 2.9-3.7%), respectively. Ten human urine samples were analyzed using the present method. BP-OH and BP-3 were detected in all the samples within the range of 0.24-5.91 and 0.43-5.17 ng mL(-1), respectively. This simple, sensitive, and selective analytical method was successfully applied to the determination of trace amounts of BPs in human urine samples.
Asunto(s)
Benzofenonas/orina , Fraccionamiento Químico/métodos , Cromatografía de Gases y Espectrometría de Masas/métodos , Fármacos Fotosensibilizantes/orina , Benzofenonas/metabolismo , Humanos , Miniaturización , Fármacos Fotosensibilizantes/metabolismo , Reproducibilidad de los Resultados , Sensibilidad y Especificidad , Solventes/química , Factores de TiempoRESUMEN
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 After extraction, 2 microl of extract was carefully withdrawn into a syringe and injected into the GC-MS system.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.
Asunto(s)
Clorofenoles/orina , Cromatografía de Gases y Espectrometría de Masas/métodos , Humanos , Estándares de Referencia , Reproducibilidad de los Resultados , Sensibilidad y EspecificidadRESUMEN
A simple and highly sensitive method that involves miniaturized hollow fiber assisted liquid-phase microextraction (HF-LPME) with in situ acyl derivatization and GC-MS was developed for the determination of benzophenone (BP) and related compounds in human urine samples. The limits of detection (S/N = 3) and quantification (S/N > 10) of BPs in human urine samples are 0.01 to 0.05 and 0.05 to 0.2 ng ml(-1), respectively. The average recoveries of BPs (n = 5) in human urine samples spiked with 10 and 50 ng ml(-1) BPs are 93.1 to 106.7% (RSD: 1.5 to 8.4%) and 96.3 to 101.5% (RSD: 3.0 to 7.7%), respectively. When the proposed method was applied to human urine samples, BPs were detected at the sub ng ml(-1) level.