Determination of atranol and chloroatranol in perfumes using simultaneous derivatization and dispersive liquid–liquid microextraction followed by gas chromatography–mass spectrometry

• The potent allergens atranol and chloroatranol are determined in perfumes by GC–MS.
• LLE is used to clean up the sample solution from lipophilic substances.
• In situ derivatization and DLLME is used to remove polar compounds and concentrate.
• The method presents good analytical features.
• The method has been assayed in four real perfume samples.

A new analytical method based on simultaneous derivatization and dispersive liquid–liquid microextraction (DLLME) followed by gas chromatography–mass spectrometry (GC–MS), for the determination of the allergenic compounds atranol and chloroatranol in perfumes, is presented. Derivatization of the target analytes by means of acetylation with anhydride acetic in carbonate buffer was carried out. Thereby volatility and detectability were increased for improved GC–MS sensitivity. In addition, extractability by DLLME was also enhanced due to a less polar character of the solutes. A liquid–liquid extraction was performed before DLLME to clean up the sample and to obtain an aqueous sample solution, free of the low polar matrix from the essential oils, as donor phase. Different parameters, such as the nature and volume of both the extraction and disperser solvents, the ionic strength of the aqueous donor phase or the effect of the derivatization reagent volume, were optimized. Under the selected conditions (injection of a mixture of 750 μL of acetone as disperser solvent, 100 μL of chloroform as extraction solvent and 100 μL of anhydride acetic as derivatization reagent) the figures of merit of the proposed method were evaluated. Limits of detection in the low ng mL−1 range were obtained. Matrix effect was observed in real perfume samples and thus, standard addition calibration is recommended.

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