Analytical and Bioanalytical Chemistry

, Volume 405, Issue 12, pp 4159–4166

Characterization of liquid chromatography-tandem mass spectrometry method for the determination of acrylamide in complex environmental samples

Research Paper

DOI: 10.1007/s00216-013-6822-4

Cite this article as:
DeArmond, P.D. & DiGoregorio, A.L. Anal Bioanal Chem (2013) 405: 4159. doi:10.1007/s00216-013-6822-4

Abstract

This work describes the characterization of a solid-phase extraction (SPE) and liquid-chromatography-tandem mass spectrometry-based method for the analysis of acrylamide (AA) in complex environmental waters. The method involved the SPE of AA using activated carbon, and the AA was detected with tandem mass spectrometry after separating on an ion exclusion high-performance liquid chromatography column. The method incorporated two labeled AA standards for quantification using isotope dilution and to assess absolute extraction recovery. The method was evaluated for inter- and intra-day precision and accuracy. The method was both accurate (i.e., <30 % error) and precise (i.e., <20 % relative standard deviation), with absolute extraction recoveries averaging 37 %. The mass spectrometry provided excellent sensitivity, with instrumental limits of detection and quantitation values of 23 and 75 pg, respectively. The method detection limit was determined to be 0.021 μg/L. The analysis of AA was successfully performed in real-world samples that contained total dissolved solids concentrations ranging from 23,600 to 297,000 mg/L and AA concentrations ranging from 0.082 to 1.0 μg/L.

https://static-content.springer.com/image/art%3A10.1007%2Fs00216-013-6822-4/MediaObjects/216_2013_6822_Figa_HTML.gif
Figure

Product ion spectra of, from top to bottom, acrylamide, acrylamide-1-13C, and acrylamide-2,3,3-d3. The predominant peak in each spectrum was used for quantitation

Keywords

AcrylamideLiquid chromatography-tandem mass spectrometryIon exclusionActivated carbonSolid-phase extraction

Abbreviations

AA

Acrylamide

AA-13C

Acrylamide-1-13C

AA-d3

Acrylamide-2,3,3-d3

HPLC

High-performance liquid chromatography

LC-MS/MS

Liquid chromatography-tandem mass spectrometry

LOD

Limit of detection

LOQ

Limit of quantitation

MDL

Method detection limit

MRM

Multiple reaction monitoring

SPE

Solid-phase extraction

TDS

Total dissolved solids

TSS

Total suspended solids

Copyright information

© Springer-Verlag Berlin Heidelberg (outside the USA) 2013

Authors and Affiliations

  1. 1.Office of Research and Development, National Exposure Laboratory, Environmental Sciences DivisionUnited States Environmental Protection AgencyLas VegasUSA
  2. 2.Student Services ContractorUnited States Environmental Protection AgencyLas VegasUSA
  3. 3.U.S. Environmental Protection AgencyLas VegasUSA