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J. Soc. Cosmet. Chem., 43, 207-213 (July/August 1992) Assay of 1,4-dioxane in cosmetic products by solid-phase extraction and GC-MS SANTO SCALIA, FABIO TESTONI, GIUSEPPE FRISINA, and MARIO GUARNERI, Dipartimento di Scienze Farmaceutiche, Universit• di Ferrara, Via Fossato di Mortara i7/i9, 44100 Ferrara (S.S., M.G. ), and Himont Research Centre, Ferrara (F.T., G.F.), Italy. Received January 27, 1992. Synopsis A rapid procedure has been developed for the assay of 1,4-dioxane in cosmetic products by gas chroma- tography selected-ion monitoring mass spectrometry. After solid-phase extraction using Bakerbond silica- and Bakerbond Cx8-disposable cartridges, samples were injected directly into a Poraplot Q capillary col- umn, employing toluene as an internal standard. Recovery of !,4-dioxane from different cosmetic matrices was between 9 !. ! and 93.2%, and the reproducibility of the method was better than 4.3 % relative standard deviation. The minimum quantifiable amount was 3 mg/kg. Of the total commercial cosmetics investigated (n = 25), 56% were found to contain 3.4-!08.4 mg/kg of !,4-dioxane. INTRODUCTION Polyethoxylated surfactants are widely used in shampoo and bath preparations (1) and are generally contained in skin cleansing products and lotion formulations (2). During the polymerization of ethylene oxide to produce the polyoxyethylene moiety of the emulsifiers, 1,4-dioxane may be formed (3-5). Hence, cosmetics containing ethoxylated surfactants may be contaminated by 1,4-dioxane (6-10), which has been shown to be carcinogenic in rats and mice (! 1, 12) and to be absorbed through the intact skin of animals (13). Furthermore, this compound has been classified as a possible carcinogen to humans (14,15). According to the European Economic Community directive on cosmetics (16), !,4-dioxane must not be present in commercial products. Consequently, the assay of this substance in marketed cosmetics is of direct concern to consumers. Published methods for the quantitative determination of 1,4-dioxane in finished cos- metic products are based on gas chromatography (GC) (6) or headspace GC (7,8). These techniques, however, have distinct drawbacks, such as complex and time-consuming sample pre-treatment (6), extremely long equilibrium times (7,8), the need for extensive calibrations (7,8), and unsatisfactory reproducibility and recoveries (6). More recently, an improved GC procedure that requires minimal sample preparation has been reported 207