Determination of 25 preservatives in cosmetics by gas chromatography-tandem mass spectrometry

Abstract

A method was developed for the simultaneous determination of benzoic acid and its esters, parabens, phenoxyisopropanol, chlorphenesin, dehydroacetic acid, 2,6-di-tert-butyl-4-methylphenol, methylchloroisothiazolone, methylisothiazolone and other preservatives in cosmetics by gas chromatography-tandem mass spectrometry (GC-MS/MS). The samples were extracted ultrasonically with a 0.1 mg/mL L(+)-ascorbic acid menthol solution after being spiked with a mixture solution of 2-octanol, phenol and heptachlor as internal standards and anhydrous sodium sulfate as a dehydrating reagent. Finally, the extract was centrifuged, filtered, and then analyzed by GC-MS/MS. The analytes were separated using an HP-5MS capillary column (30 m×0.25 mm×0.25 μm) with a temperature-programming program. The inlet, transfer line and ion source temperatures were set to 260, 250 and 230℃, respectively. Helium (99.999%) was used as the carrier gas at a flow rate of 1 mL/min. The final extract (1 μL) was injected in split mode (10:1). Analysis was performed in the multiple reaction monitoring (MRM) mode. Three types of cosmetics, as well as water, milk and cream as samples were selected to verify the accuracy of the method at four levels. The average spiked recoveries ranged from 82.3% to 119.4% with relative standard deviations (n=6) of less than 14.3%. The limits of detection were lower than 0.99 μg/kg for all the preservatives. The method is sensitive, and reliable for the simultaneous determination of the 25 preservatives in cosmetics. Nonetheless, complementary methods need to be developed for the determination of some other preservatives that cannot be detected by GC-MS/MS.