Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1217, Issue 17, Pages 2925-2932Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2010.02.057
Keywords
Microextraction by packed sorbents (MEPSs); UV filters; Polycyclic musk compounds; Large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS)
Funding
- Ministerio de Educacion y Ciencia
- Ministerio de Innoyacion y Ciencia
- E.U. [CTQ2009-08377]
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An at-line analysis protocol is presented that allows the determination of four UV filters, two polycyclic musk compounds and caffeine in water at concentration level of ng L-1. The fully automated method includes analytes enrichment by Microextraction by packed sorbent (MEPS) coupled directly to large volume injection-gas chromatography-mass spectrometry. Two common SPE phases, C8 and C18, were examined for their suitability to extract the target substances by MEPS. The analytes were extracted from small sample volumes of 800 mu L. with recoveries ranging from 46 to 114% for the C8-sorbent and 65-109% for the C18-sorbent. Limits of detection between 34 and 96 ng L-1 enable the determination of the analytes at common environmental concentration levels. Both sorbents showed linear calibration curves for most of the analytes up to a concentration level of 20 ng mL(-1). Carryover was minimized by washing the sorbents 10 times with 100 mu L. methanol. After this thorough cleaning, the MEPS are re-used and up to 70 analyses can be performed with the same sorbent. The fully automated microextraction GC-MS protocol was evaluated for the influence of matrix substances typical for wastewater. Dilution of samples prior to MEPS is recommended when the polar caffeine is present at high concentration. Real water samples were analyzed by the MEPS-GC-MS method and compared to standard SPE. (C) 2010 Elsevier B.V. All rights reserved.
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