title: Microvolume trace environmental analysis using peak-focusing online solid-phase extraction-nano-liquid chromatography-high-resolution mass spectrometry.
abstract: Online solid-phase extraction was combined with nano-liquid chromatography coupled to high-resolution mass spectrometry (HRMS) for the analysis of micropollutants in environmental samples from small volumes. The method was validated in surface water, Microcystis aeruginosa cell lysate, and spent Microcystis growth medium. For 41 analytes, quantification limits of 0.1-28 ng/L (surface water) and 0.1-32 ng/L (growth medium) were obtained from only 88 μL of sample. In cell lysate, quantification limits ranged from 0.1-143 ng/L or 0.33-476 ng/g dry weight from a sample of 88 μL, or 26 μg dry weight, respectively. The method matches the sensitivity of established online and offline solid-phase extraction-liquid chromatography-mass spectrometry methods but requires only a fraction of the sample used by those techniques, and is among the first applications of nano-LC-MS for environmental analysis. The method was applied to the determination of bioconcentration in Microcystis aeruginosa in a laboratory experiment, and the benefit of coupling to HRMS was demonstrated in a transformation product screening.
authors.affiliation: Eawag, Swiss Federal Institute of Aquatic Science and Technology, 8600, Dübendorf, Switzerland.|Institute of Biogeochemistry and Pollutant Dynamics, ETH Zurich, 8092, Zürich, Switzerland.
authors.forename: Michael A
authors.initials: MA
authors.lastname: Stravs
authors.affiliation: Eawag, Swiss Federal Institute of Aquatic Science and Technology, 8600, Dübendorf, Switzerland.
authors.forename: Jonas
authors.initials: J
authors.lastname: Mechelke
authors.affiliation: Department of Civil and Environmental Engineering, Duke University, Durham, NC, 27708, USA.
authors.forename: P Lee
authors.initials: PL
authors.lastname: Ferguson
authors.affiliation: Eawag, Swiss Federal Institute of Aquatic Science and Technology, 8600, Dübendorf, Switzerland.
authors.forename: Heinz
authors.initials: H
authors.lastname: Singer
authors.affiliation: Eawag, Swiss Federal Institute of Aquatic Science and Technology, 8600, Dübendorf, Switzerland. juliane.hollender@eawag.ch.|Institute of Biogeochemistry and Pollutant Dynamics, ETH Zurich, 8092, Zürich, Switzerland. juliane.hollender@eawag.ch.
authors.forename: Juliane
authors.initials: J
authors.lastname: Hollender
mesh_terms: D002853:Chromatography, Liquid / Q000295:instrumentation*; D004784:Environmental Monitoring / Q000295:instrumentation*; D004867:Equipment Design; D005618:Fresh Water / Q000032:analysis* / Q000382:microbiology*; D057230:Limit of Detection; D046931:Microcystis / Q000302:isolation & purification*; D008904:Miniaturization / Q000295:instrumentation; D018401:Sample Size; D052616:Solid Phase Extraction / Q000295:instrumentation*; D053719:Tandem Mass Spectrometry / Q000295:instrumentation; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D014874:Water Pollutants, Chemical
keywords: Biological samples; Environmental analytics; High-resolution MS; Miniaturization; Nano-LC; Online SPE