Determination of Non-Steroidal Anti-Inflammatory Drugs in Natural Waters Using Off-Line and On-Line SPE Followed by LC Coupled with DAD-MS |
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Authors: | A Kot-Wasik J D?bska A Wasik J Namie?nik |
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Institution: | (1) Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology, 11/12 Narutowicz Str, 80-952 Gdańsk-Wrzeszcz, Poland |
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Abstract: | Two different procedures for simultaneous determination of six NSAIDs (diflunisal, diclofenac, fenoprofen, ibuprofen, naproxen
and tolmetin) in environmental waters are described. Final analysis of target compounds is performed by reversed-phase liquid
chromatography – diode array detection and mass spectrometry (HPLC-DAD and LC-MS), whereas sample preparation is based on
solid-phase extraction (SPE). A variety of sorbents and their respective advantages and disadvantages are discussed. For the
off-line SPE of NSAIDs from water samples, a LiChrolut RP-18 was selected out of all investigated sorbents. In case of on-line
coupling of SPE with chromatographic system LiChrosphere RP-18 was selected as the best one in terms of recovery of NSAIDs
evaluated, RSD and availability. The applicability of the method was also evaluated. Method detection limits were in the range
of 0.7−94 ng L−1. Recoveries ranged from 96 to 109% and relative standard deviations were lower than 5%. The procedures were shown to be linear
over a wide range of concentration, exhibited satisfactory repeatability and accuracy, and reached limits of detection in
the low ng L−1 range. No breakthrough volume was observed neither for off-line SPE (in the studied range of 100, 200, 300, 500, 700, 1000
and 2000 mL of tap water sample) nor for on-line SPE (in the wide range of 10 mL, 20 mL, 30 mL, 50 mL, 70 mL, 100 mL and 200
mL of tap water sample). |
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Keywords: | Column liquid chromatography Solid-phase extraction LC-diode array detection-mass spectrometry On-line and off-line enrichment Water analysis |
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