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Analytical and Bioanalytical Chemistry

, Volume 394, Issue 3, pp 893–901 | Cite as

Solid-phase micro-extraction procedure for the determination of 1,3-dichloro-2-propanol in water by on-fibre derivatisation with bis(trimethylsilyl)trifluoroacetamide

  • Antonia María CarroEmail author
  • Paula González
  • Noelia Fajar
  • Rosa Antonia Lorenzo
  • Rafael Cela
Original Paper

Abstract

The headspace solid-phase micro-extraction technique with on-fibre derivatisation followed by gas chromatography-tandem mass spectrometry has been evaluated for the analysis of 1,3-dichloro-2-propanol in water. An asymmetric factorial design has been performed to study the influence of five experimental factors: extraction time and temperature, derivatisation time and temperature and pH. The best extraction performance is achieved in the headspace mode, with 5 mL stirred water samples (pH 4) containing 1.3 g of NaCl, equilibrated for 30 min at 25 °C, using divinylbenzene-carboxen-polydimethylsiloxane as the fibre coating. On-fibre derivatisation has been used for the first time with 50 µL of bis(trimethylsilyl)trifluoroacetamide at 25 °C during 15 min, leading to effective yields. The proposed method provides high sensitivity, good linearity and repeatability (relative standard deviation of 5.1% for 10 ng mL−1 and n = 5). The limits of detection and quantification were 0.4 and 1.4 ng mL−1, respectively. Analytical recoveries obtained for different water samples were approx. 100%.

Keywords

1,3-Dichloro-2-propanol HS-SPME On-fibre derivatisation GC-MS/MS Water 

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Copyright information

© Springer-Verlag 2009

Authors and Affiliations

  • Antonia María Carro
    • 1
    Email author
  • Paula González
    • 1
  • Noelia Fajar
    • 1
  • Rosa Antonia Lorenzo
    • 1
  • Rafael Cela
    • 1
  1. 1.Dpto. de Química Analítica, Nutrición y Bromatología, Facultad de Química, Instituto de Investigaciones y Análisis Alimentarios (IIAA)Universidad de Santiago de CompostelaSantiago de CompostelaSpain

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