Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume 45,
Number 3, March 2007, pp.146-152
On-line SPE–Nano-LC–Nanospray-MS for
Rapid and Sensitive Determination of Perfluorooctanoic Acid and
Perfluorooctane Sulfonate in River Water
Steven Ray Wilson[1], Helle Malerød[1],
Anders Holm[2], Paal Molander[1,3], Elsa Lundanes[1], and Tyge
Greibrokk[1]
[1]Department of Chemistry, University of Oslo, P.O. Box 1033
Blindern, N-0315 Oslo, Norway;
[2]Institute of Immunology, Rikshospitalet University Hospital,
N-0027 Oslo, Norway; and
[3]National Institute of Occupational Health, P.O. Box 8149 Dep.
N-0033 Oslo, Norway
An instrumental set up including on-line solid-phase
extraction, nano-liquid chromatography, and nanospray mass spectrometry
is constructed to improve the sensitivity for quantitation of
perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS)
in surface water. Sample volumes of 1000 µL are loaded onto
a microbore 1.0-mm i.d. ¥ 5 mm, 5 µm Kromasil C18 enrichment
column by a carrier solution consisting of 10mM ammonium acetate
in acetonitrile–water (10:90, v/v) at a flow rate of 250
µL/min, providing on-line analyte enrichment and sample
clean-up. Backflushed elution onto a 0.1-mm i.d. ¥ 150 mm,
3.5 µm Kromasil C18 analytical column is conducted using
an acetonitrile–10mM ammonium acetate solvent gradient from
30% to 70% acetonitrile. Water samples are added with internal
standard (perfluoroheptanoic acid) and filtrated prior to injection.
The mass limits of detection of PFOA and PFOS are 0.5 and 1 pg,
respectively, corresponding to concentration limits of detection
of 500 pg/L and 1 ng/L, respectively. The total time spent on
sample preparation, chromatography, and detection is approximately
12 min per sample. The method was employed for the determination
of PFOS and PFOA in urban river water.
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