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

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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.

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

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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

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Acknowledgments

The United States Environmental Protection Agency, through its Office of Research and Development, funded and managed the research described here. It has been subjected to the Agency’s peer and administrative review and has been approved for publication. Mention of trade names or commercial products in this paper does not constitute endorsement or recommendation by the EPA.

This information is distributed solely for the purpose of pre-dissemination peer review under applicable information quality guidelines. It has not been formally disseminated by EPA. It does not represent and should not be construed to represent any Agency determination or policy.

The authors thank Matt Landis (EPA) for collecting the samples.

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Authors and Affiliations

  1. Office of Research and Development, National Exposure Laboratory, Environmental Sciences Division, United States Environmental Protection Agency, 944 E. Harmon Ave., Las Vegas, NV, 89119, USA

    Patrick D. DeArmond

  2. Student Services Contractor, United States Environmental Protection Agency, 944 E. Harmon Ave., Las Vegas, NV, 89119, USA

    Amanda L. DiGoregorio

  3. U.S. Environmental Protection Agency, P.O. Box 93478, Las Vegas, NV, 89193-3478, USA

    Patrick D. DeArmond

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  1. Patrick D. DeArmond
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  2. Amanda L. DiGoregorio
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Correspondence to Patrick D. DeArmond.

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DeArmond, P.D., DiGoregorio, A.L. Characterization of liquid chromatography-tandem mass spectrometry method for the determination of acrylamide in complex environmental samples. Anal Bioanal Chem 405, 4159–4166 (2013). https://doi.org/10.1007/s00216-013-6822-4

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  • DOI: https://doi.org/10.1007/s00216-013-6822-4

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