Determination of 2,6-dichlorobenzamide and its degradation products in water samples using solid-phase extraction followed by liquid chromatography-tandem mass spectrometry.
An analytical method was developed for the determination of 2,6-dichlorobenzamide (BAM) and five degradation products thereof including 2-chlorobenzamide (OBAM), 2,6-dichlorobenzoic acid (DCBA), 2-chlorobenzoic acid (OBA), benzoic acid (BA) and benzamide (BAD) in water samples. Solid-phase extraction was combined with liquid chromatography coupled to tandem mass spectrometry using electrospray ionisation. Groundwater spiked at a concentration of 1.0 microg/L gave recoveries on day 1 between 91 and 102% (relative standard deviation: 2.2-26.5%) for OBAM, BAM, DCBA, BA and OBA, while BAD showed a somewhat lower recovery of 60% (relative standard deviation: 25%). Corresponding figures on day 3 gave recoveries of 97-110% (relative standard deviation: 3-22%) for OBAM, BAM, DCBA, BA and OBA, while BAD had a recovery of 51% (relative standard deviation: 4%). The final SPE-LC-MS/MS method had a LOD(Method) of 0.009, 0.007, 0.010, 0.021, 0.253 and 0.170 microg/L groundwater for BAD, OBAM, BAM, DCBA, BA and OBA and a LOQ(Method) of 0.030, 0.023, 0.035, 0.071, 0.842 and 0.565 microg/L groundwater in the same order of appearance. Analysis of three different Danish groundwaters confirmed the occurrence of BAM at levels exceeding the threshold value of 0.1 microg/L, while no degradation products were found above LOD(Method).
Jensen
Gitte Gotholdt
GG
Section of Toxicology and Environmental Chemistry, Department of Pharmaceutics and Analytical Chemistry, Faculty of Pharmaceutical Science, Copenhagen University, Universitetsparken 2, DK-2100 Copenhagen, Denmark. ggj@farma.ku.dk
Björklund
Erland
E
Simonsen
Allan
A
Halling-Sørensen
Bent
B
D001549:Benzamides / Q000737:chemistry*; D002853:Chromatography, Liquid / Q000379:methods*; D010573:Pesticide Residues / Q000737:chemistry*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000737:chemistry*
D001549:Benzamides; D010573:Pesticide Residues; D014874:Water Pollutants, Chemical; C057454:2,6-dichlorobenzamide