Determination of suspected fragrance allergens in cosmetics by matrix solid-phase dispersion gas chromatography–mass spectrometry analysis

An effective low cost sample preparation methodology for the determination of regulated fragrance allergens in leave-on and rinse-off cosmetics has been developed applying, for the first time, matrix solid-phase dispersion (MSPD) to this kind of analytes and samples. The selection of the most suitable extraction conditions was made using statistical tools such as ANOVA, as well as a factorial multifactor experimental design. These studies were carried out using real cosmetic samples. In the final conditions, 0.5 of sample, previously mixed with 1 g of anhydrous Na2SO4, were blended with 2 g of dispersive sorbent (Florisil), and the MSPD column was eluted with 5 mL of hexane/acetone (1:1). The extract was then analyzed by GC–MS without any further clean-up or concentration step. Accuracy, precision, linearity and detection limits (LODs) were evaluated to assess the performance of the proposed method. Quantitative recoveries (>75%) were obtained and RSD values were lower than 10% in all cases. The quantification limits were well below those set by the international cosmetic regulations, making this multi-component analytical method suitable for routine control. In addition, the MSPD method can be implemented in any laboratory at low cost since it does not require special equipment. Finally, a wide variety of cosmetic products were analyzed. All the samples contained several of the target cosmetic ingredients, with and average number of seven. The total fragrance allergen content was in general quite high, even in baby care products, with values close to or up to 1%, for several samples, although the actual European Cosmetic Regulation was fulfilled.