Determination of 1,3-dichloropropanol in soy sauce and related products by headspace gas chromatography with mass spectrometric detection: Interlaboratory study

Sarah Hasnip*, Colin Crews, Nicholas Potter, Paul Brereton, Henri Diserens, Jean Marie Oberson, B. Baigrie, N. Byrd, D. J. Campbell, H. Diserens, L. Hageman, F. Hollywood, Y. Noro, P. Nyman, H. Wehage

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

10 Citations (Scopus)

Abstract

An intel-laboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d 5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96-130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9-23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9-35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

Original languageEnglish
Pages (from-to)1404-1412
Number of pages9
JournalJournal of AOAC International
Volume88
Issue number5
Publication statusPublished - 01 Sep 2005

ASJC Scopus subject areas

  • Analytical Chemistry
  • Food Science
  • Environmental Chemistry
  • Agronomy and Crop Science
  • Pharmacology

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