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Determination of beta-blockers and beta(2)-agonists in sewage by solid-phase extraction and liquid chromatography-tandem mass spectrometry. [J Chromatogr A] Journal article

 
TitleDetermination of beta-blockers and beta(2)-agonists in sewage by solid-phase extraction and liquid chromatography-tandem mass spectrometry.
Author(s)Lee HB, Sarafin K, Peart TE 
InstitutionAquatic Ecosystem Protection Research Division, Water Science and Technology Directorate, Science and Technology Branch, Environment Canada, 867 Lakeshore Road, Burlington, Ontario L7R 4A6, Canada.
SourceJ Chromatogr A 2007 Mar 16.
AbstractA method using solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed for the determination of 12 beta-blockers and beta(2)-agonists in wastewater samples. Extraction of the drugs was effected by an Oasis MCX cartridge with a strong cation resin adsorbent. Matrix coextractives were removed from the SPE cartridge by methanol prior to the elution of the drugs with a mixture of dichloromethane, 2-propranol, and ammonium hydroxide. The extract was analyzed by LC-MS/MS with electrospray ionization operating in the positive mode. Recovery of the 12 compounds was in most cases better than 85% at the fortification levels of 500 and 50ng/L, with standard deviations between 3 and 7%. Based on a concentration factor of 250, the method detection limits ranged from 6 to 11ng/L for the target compounds. No degradation of these drugs in spiked sewage effluent samples was observed over a storage period of 7 days at 4 degrees C in the dark. Many beta-blockers were detected in the 14 wastewater samples collected from seven Canadian sewage treatment plants; those occurring at the highest concentrations were atenolol, acebutolol, sotalol, and metroprolol, with overall median concentrations of 1370, 339, 282, and 257ng/L, respectively. However, there was only a small decrease in the median concentrations of these beta-blockers between the primary and final effluent, suggesting that these drugs are not easily removed by the sewage treatment processes. As a result of selective extraction and effective removal of coextractives, no matrix effect was observed for the samples during LC-MS/MS analyses.
LanguageENG
Pub Type(s)JOURNAL ARTICLE
PubMed ID17408682
  
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