Determination of residual 1,4-dioxane in surfactants and cleaning agents using headspace single-drop microextraction followed by gas chromatography-flame ionization detection

Int J Cosmet Sci. 2017 Feb;39(1):36-41. doi: 10.1111/ics.12345. Epub 2016 Jun 23.


Objective: Polyethoxylated surfactants are widely used in the formulation of different cleaning agents such as shampoo, dish washing and hand washing products and lotion formulation. During the production of polyethoxylated surfactants, 1,4-dioxane as a toxic and carcinogenic by-product is formed. A simple low-cost method based on headspace single-drop microextraction combined with gas chromatography-flame ionization detection was developed for the determination of 1,4-dioxane in surfactants and cleaning agents.

Methods: In this method, 1,4-dioxane was extracted from 8.0 mL sample solution into a microdrop of an organic solvent, and then, it was injected to gas chromatography. The effects of such parameters as the solvent type, salt addition, microdrop volume, stirring rate, equilibrium time, extraction time and the temperature of sample solution on the extraction performance were studied and optimized. An ethoxylated surfactant containing 1,4-dioxane was used as the sample for the optimization of the extraction parameters.

Results: The linear range, determination coefficient, limit of detection and relative standard deviation of the method were 0.5-100 μg g-1 , 0.9977, 0.4 μg g-1 and 7.2% (n = 5), respectively. Different real samples including sodium lauryl ether sulphate, sodium lauryl sulphate (SLS), four brands of shampoo, and hand washing and dish washing liquids were analysed by the method. 1,4-Dioxane was detected at the concentration range of 2.4-201 μg g-1 in the samples, except dish washing liquid and SLS.

Conclusion: A new method with the merits of simplicity, low cost, low organic solvent consumption, short analysis time, good repeatability and suitable detection limit was developed for the analysis of 1,4-dioxane in surfactants and cleaning agents.

Keywords: 1,4-dioxane; chemical analysis; cosmetic products; gas chromatography; headspace single-drop microextraction; safety testing.

Publication types

  • Validation Study

MeSH terms

  • Chromatography, Gas / methods*
  • Dioxanes / analysis*
  • Surface-Active Agents / chemistry*


  • Dioxanes
  • Surface-Active Agents
  • 1,4-dioxane