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Hollow fiber liquid phase microextraction as a preconcentration and clean-up step after pressurized hot water extraction for the determination of non-steroidal anti-inflammatory drugs in sewage sludge

Saleh, Abolfazl; Larsson, Estelle LU ; Yamini, Yadollah and Jönsson, Jan Åke LU (2011) In Journal of Chromatography A 1218(10). p.1331-1339
Abstract
A method for the quantitative determination of non-steroidal anti-inflammatory drugs (NSAIDs) in sewage sludge was developed and validated. The target compounds were extracted using pressurized hot water extraction (PHWE) and then purified and preconcentrated by three-phase hollow fiber liquid phase microextraction (HF-LPME) followed by LC-ESI-MS analysis. The PHWE was optimized with regard to the pH of solvent as well as other operational parameters. The optimum conditions were 0.01 M NaOH as the extraction solvent, temperature of 120 degrees C, pressure of 100 bar, static time 5 min, 5 cycles, flush volume 90% and purge time 60s. Spike recoveries for sludge samples spiked at 200 ng g(-1) were in the range of 101-109% but for the native... (More)
A method for the quantitative determination of non-steroidal anti-inflammatory drugs (NSAIDs) in sewage sludge was developed and validated. The target compounds were extracted using pressurized hot water extraction (PHWE) and then purified and preconcentrated by three-phase hollow fiber liquid phase microextraction (HF-LPME) followed by LC-ESI-MS analysis. The PHWE was optimized with regard to the pH of solvent as well as other operational parameters. The optimum conditions were 0.01 M NaOH as the extraction solvent, temperature of 120 degrees C, pressure of 100 bar, static time 5 min, 5 cycles, flush volume 90% and purge time 60s. Spike recoveries for sludge samples spiked at 200 ng g(-1) were in the range of 101-109% but for the native drugs in non-spiked sludge samples, recoveries were 38.9%, 59.8%, 90.3% and 47.8% for ketoprofen, naproxen, diclofenac and ibuprofen, respectively. Donor phase pH, ionic strength and extraction time were optimized for HF-LPME after PHWE. The optimum conditions were 2h extraction at pH 1.5 without salt addition. Enrichment factors in the range of 947-1213 times were achieved (extraction recoveries were 23.6-30.3%) for HF-LPME after PHWE. The matrix effect on the ionization of drugs in LC-ESI-MS was also investigated. The results show that there is a smaller matrix effect (-8.9% to +14.6%) in comparison with other published values obtained using solid phase extraction (SPE) for clean-up after pressurized liquid extraction (PLE). Method detection limits (MDLs) and method quantification limits (MQLs) for different drugs were in the range of 0.4-3.7 ng g(-1) and 1.5-12.2 ng g(-1) in dried sludge samples, respectively. The characteristics of the proposed method were compared with those of other published works. The considerably lower ion suppression/enhancement and minimum use of organic solvents (a few microliters of di-n-hexyl ether) in the sample preparation step are two highlighted advantages of the proposed method in comparison with previously published works. The method was applied to determine NSAIDs in sewage sludge from Kallby wastewater treatment plant (Lund, Sweden) in April, June. August and October 2010. The highest concentration level was recorded for ibuprofen in the April sewage sludge sample (588 ng g(-1)) and all of the selected NSAIDs were detected in all the samples analyzed. (C) 2011 Elsevier B.V. All rights reserved. (Less)
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Contribution to journal
publication status
published
subject
keywords
Pressurized hot water extraction, Hollow fiber liquid-phase, microextraction, Non-steroidal anti-inflammatory drugs, Sewage sludge, Liquid chromatography-mass spectrometry
in
Journal of Chromatography A
volume
1218
issue
10
pages
1331 - 1339
publisher
Elsevier
external identifiers
  • wos:000288186900002
  • scopus:79951511219
ISSN
0021-9673
DOI
10.1016/j.chroma.2011.01.011
language
English
LU publication?
yes
id
789d9d25-2f77-43d6-b290-b025a09dcf81 (old id 1868353)
date added to LUP
2011-04-19 12:28:19
date last changed
2017-11-12 03:42:21
@article{789d9d25-2f77-43d6-b290-b025a09dcf81,
  abstract     = {A method for the quantitative determination of non-steroidal anti-inflammatory drugs (NSAIDs) in sewage sludge was developed and validated. The target compounds were extracted using pressurized hot water extraction (PHWE) and then purified and preconcentrated by three-phase hollow fiber liquid phase microextraction (HF-LPME) followed by LC-ESI-MS analysis. The PHWE was optimized with regard to the pH of solvent as well as other operational parameters. The optimum conditions were 0.01 M NaOH as the extraction solvent, temperature of 120 degrees C, pressure of 100 bar, static time 5 min, 5 cycles, flush volume 90% and purge time 60s. Spike recoveries for sludge samples spiked at 200 ng g(-1) were in the range of 101-109% but for the native drugs in non-spiked sludge samples, recoveries were 38.9%, 59.8%, 90.3% and 47.8% for ketoprofen, naproxen, diclofenac and ibuprofen, respectively. Donor phase pH, ionic strength and extraction time were optimized for HF-LPME after PHWE. The optimum conditions were 2h extraction at pH 1.5 without salt addition. Enrichment factors in the range of 947-1213 times were achieved (extraction recoveries were 23.6-30.3%) for HF-LPME after PHWE. The matrix effect on the ionization of drugs in LC-ESI-MS was also investigated. The results show that there is a smaller matrix effect (-8.9% to +14.6%) in comparison with other published values obtained using solid phase extraction (SPE) for clean-up after pressurized liquid extraction (PLE). Method detection limits (MDLs) and method quantification limits (MQLs) for different drugs were in the range of 0.4-3.7 ng g(-1) and 1.5-12.2 ng g(-1) in dried sludge samples, respectively. The characteristics of the proposed method were compared with those of other published works. The considerably lower ion suppression/enhancement and minimum use of organic solvents (a few microliters of di-n-hexyl ether) in the sample preparation step are two highlighted advantages of the proposed method in comparison with previously published works. The method was applied to determine NSAIDs in sewage sludge from Kallby wastewater treatment plant (Lund, Sweden) in April, June. August and October 2010. The highest concentration level was recorded for ibuprofen in the April sewage sludge sample (588 ng g(-1)) and all of the selected NSAIDs were detected in all the samples analyzed. (C) 2011 Elsevier B.V. All rights reserved.},
  author       = {Saleh, Abolfazl and Larsson, Estelle and Yamini, Yadollah and Jönsson, Jan Åke},
  issn         = {0021-9673},
  keyword      = {Pressurized hot water extraction,Hollow fiber liquid-phase,microextraction,Non-steroidal anti-inflammatory drugs,Sewage sludge,Liquid chromatography-mass spectrometry},
  language     = {eng},
  number       = {10},
  pages        = {1331--1339},
  publisher    = {Elsevier},
  series       = {Journal of Chromatography A},
  title        = {Hollow fiber liquid phase microextraction as a preconcentration and clean-up step after pressurized hot water extraction for the determination of non-steroidal anti-inflammatory drugs in sewage sludge},
  url          = {http://dx.doi.org/10.1016/j.chroma.2011.01.011},
  volume       = {1218},
  year         = {2011},
}