title: Application of pressure-assisted electrokinetic injection-tandem mass spectrometry in the determination of perchlorate in water and soil samples.
abstract: A new method for the determination of perchlorate in water and soil samples using on-line enrichment in a capillary zone electrophoresis-mass spectrometry is presented. The target analytes in the sample solutions were introduced into the capillary column by pressure-assisted electrokinetic injection (PAEKI) with the simultaneous application of -18 kV and +50 mbar external pressure to the sample vial at the capillary inlet for 4 min. The injected sample zone was flushed out with a running buffer and analyzed by a tandem mass spectrometer in a negative selected reaction monitoring mode. The influence of the matrix in both water and soil samples was eliminated by a clean-up step by passing the sample through Ba/Ag/H cartridges. The method showed good linearity in the dynamic range of 20 to 1000 ng/L, and achieved a detection limit of 18.7 ng/L for water samples and 3.3 ng/g for soil samples, respectively. The recovery of perchlorate in spiked samples, at three different levels, ranged over 79-127%. The method reproducibility was found to be 11% RSD for water samples and 7% RSD for soil samples. Perchlorate was found in 25 out of 28 water samples analyzed, with the levels ranging from 19.8 to 192 ng/L, and was not detected in the 10 soil samples analyzed.
authors.affiliation: Exposure and Biomonitoring Division, Environmental Health Science and Research Bureau, Health Canada, Ottawa, ON, Canada. rocio.aranda-rodriguez@hc-sc.gc.ca
authors.forename: Rocio
authors.initials: R
authors.lastname: Aranda-Rodriguez
authors.forename: Zhiyun
authors.initials: Z
authors.lastname: Jin
authors.forename: Jiping
authors.initials: J
authors.lastname: Zhu
authors.forename: Yong-Lai
authors.initials: YL
authors.lastname: Feng
mesh_terms: D053000:Analytic Sample Preparation Methods; D019075:Electrophoresis, Capillary; D004785:Environmental Pollutants / Q000032:analysis* / Q000302:isolation & purification; D007267:Injections; D010472:Perchlorates / Q000032:analysis* / Q000302:isolation & purification; D011312:Pressure; D015203:Reproducibility of Results; D012987:Soil / Q000737:chemistry*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry*
chemical_list: D004785:Environmental Pollutants; D010472:Perchlorates; D012987:Soil; D014867:Water; C494474:perchlorate