Validation and Collaborative Studies of Headspace Gas Chromatography-Mass Spectrometry for Determination of 1,4-Dioxane in Cosmetic Samples

Abstract

Abstract Background 1,4-Dioxane (1,4-D) is a byproduct of the synthesis of surfactants, typically found in some cosmetics products such as shampoo, toothpaste, and soap. The presence of 1,4-D in cosmetics products is limited to a certain amount since 1,4-D is classified as a probable human carcinogen. Objective This present study was intended to validate static headspace gas chromatography-mass spectrometry (HS GC-MS) for the determination of 1,4-D in cosmetics products. Methods The condition of HS and GC-MS was optimized to get the best condition for analysis of 1,4-D using 1,4-dioxane-d8 (1,4-D-d8) as internal standard (IS). The developed method was validated by evaluating the key performance characteristics, including specificity, linearity, limit of detection (LoD), limit of quantification (LoQ), accuracy, and precision. Results The results showed that HS GC-MS was specific since the peaks of the selected ion monitoring (SIM) mode could be separated and confirmed at m/z 88 and m/z 96 for 1,4-D and 1,4-D-d8, respectively. The method was linear over the concentration range of 0.1287–1.2875 µg/mL, with R2 > 0.999 and RSD residuals <2.0. A collaborative study was conducted on this method, with 10 participating laboratories from four countries. The outcome of this study was found to be accurate and precise, as evidenced by the excellent recoveries ranging from 94.6% to 102.1%, and with good reproducibility with RSD values ranging from 0.2 to 1.1%. The collaborative studies exhibited that all data reported by 10 participating laboratories in four countries were inliers without any extreme values observed either in mean or RSD values Conclusions HS GC-MS is found to be fit and suitable for the determination of trace level of 1,4-D in cosmetics products. Highlights The HS GC-MS method could be proposed as a standard method for quantitative analysis of 1,4-D in cosmetics products since the collaborative studies indicated that the developed method meet the requirement in “Guidelines for Collaborative Study Procedures to Validate Characteristics of a Method of Analysis.”