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Analysis of alcohol ethoxylates and alkylamine ethoxylates in agricultural soils using pressurised liquid extraction and liquid chromatography–mass spectrometry

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Abstract

Nonionic surfactants e.g. alcohol ethoxylates (AEOs) and alkylamine ethoxylates (ANEOs) are commonly utilised as adjuvants in pesticide formulations to enhance their effectiveness. In this study, analytical methods for AEO and ANEO determination in soil samples using pressurised liquid extraction (PLE) were developed and used in connection with LC–MS. The recovery of the method, which was highly dependent on the soil properties, varied in the range 47–106% for AEO and 27–109% for ANEO. Detection limits (LOD) were 7–13 µg kg−1 for AEO and 24–43 µg kg−1 for ANEO. The developed method has been applied to determine AEOs and ANEOs in surface soil samples from fields sprayed with glyphosate herbicides. Tallowalkylamine ethoxylates (an ANEO) were detected in the soil before and after pesticide application, with increasing concentrations after treatment. The highest concentration in the soil samples was observed for the ANEO homologues with the longest ethoxy chains; in the clay soil the concentration decreased with the length of the ethoxy chain. ANEOs added to pesticide formulations as a technical mixture will, as demonstrated in this study, behave as individual homologues, which is reflected in their behaviour in the environment.

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Abbreviations

AEO:

Alcohol ethoxylates

ANEO:

Alkylamine ethoxylates

APEO:

Alkylphenol ethoxylates

APCI:

Atmospheric pressure chemical ionisation

ASE:

Accelerated solvent extraction

CEC:

Cationic exchange capacity

LC–MS:

Liquid chromatography–mass spectrometry

LOD:

Limit of detection

MAE:

Microwave-assisted extraction

PLE:

Pressurised liquid extraction

SD:

Standard deviation

SIM:

Selected-ion monitoring

SPE:

Solid-phase extraction

TEA:

Triethylamine

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Acknowledgements

The Danish EPA and the Danish Research Agency has supported this work financially. The authors thank Mary-Ann Chrillesen for technical assistance. Thanks to Andreu Taberner, University of Lleida and Josep Soldevila, Cooperativa d'Artesa for helping to find the fields applied in this study.

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Author notes

  1. Kristine A. Krogh

    Present address: Section of Environmental Chemistry, Institute of Analytical Chemistry, Danish University of Pharmaceutical Sciences, Universitetsparken 2, 2100, Copenhagen Ø, Denmark

Authors and Affiliations

  1. National Environmental Research Institute (NERI), Department of Atmospheric Environment, P.O. Box 358, 4000, Roskilde, Denmark

    Kristine A. Krogh, Betty Bügel Mogensen & Karl V. Vejrup

  2. Section of Environmental Chemistry, Institute of Analytical Chemistry, Danish University of Pharmaceutical Sciences, Universitetsparken 2, 2100, Copenhagen Ø, Denmark

    Bent Halling-Sørensen

  3. Laboratory of Soil Science, Faculty of Pharmacy, University of Barcelona, Av. de Joan XXIII, s/n, 08028, Barcelona, Spain

    Amparo Cortés

  4. Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18–26, 08034, Barcelona, Spain

    Damià Barceló

Authors
  1. Kristine A. Krogh
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  2. Betty Bügel Mogensen
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  3. Bent Halling-Sørensen
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  4. Amparo Cortés
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  5. Karl V. Vejrup
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Correspondence to Kristine A. Krogh.

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Krogh, K.A., Mogensen, B.B., Halling-Sørensen, B. et al. Analysis of alcohol ethoxylates and alkylamine ethoxylates in agricultural soils using pressurised liquid extraction and liquid chromatography–mass spectrometry. Anal Bioanal Chem 376, 1089–1097 (2003). https://doi.org/10.1007/s00216-003-2062-3

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  • DOI: https://doi.org/10.1007/s00216-003-2062-3

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