Development and validation of ultra-high performance supercritical fluid chromatography method for quantitative determination of nine sunscreens in cosmetic samples

Abstract

A fast and simple utra-high performance supercritical fluid chromatography (UHPSFC) method has been developed for the determination of nine sunscreens (UV filters), namely 2-ethylhexyl-2-hydroxybenzoate (ES), ethylhexyl-methoxycinnamate (EMC), benzophenone-3 (BZ3), octocrylene (OCR), bis-ethylhexyloxyphenol-methoxyphenyl triazine (EMT), butyl-methoxydibenzoyl-methane (BDM), diethylamino-hydroxybenzoyl-hexyl-benzoate (DHB), ethylhexyl-triazone (ET), and diethylhexyl-butamido-triazone (DBT) in cosmetic samples. The separation was achieved with Acquity UPC2 Torus 2-PIC (100 × 3.0 mm, 1.7 μm) column. The influence of key chromatographic parameters on resolution was evaluated. The optimal mobile phase was a gradient mixture of carbon dioxide and methanol containing ammonium acetate, at flow rate 1.2 mL min−1. The back-pressure of the system was set to 150 bar and the temperature to 40 °C. The compounds were determined with diode-array detection at 280 nm, 305 nm and 340 nm depending on absorbance maxima. The proposed UHPSFC method provided separation of the nine target sunscreens within 2.5 min without labor-consuming sample pretreatment procedure. The method was validated according to the concept of the total error and the accuracy profile. The inter-laboratory reproducibility was evaluated between two independent laboratories (in France and Czech Republic). The reliability of the developed method was shown by application to commercial sunscreen-containing cosmetic sample obtained from French market. The measured limits of quantification showed the suitability of the proposed method for determination of UV filters considering the European Union requirements.