Charles University, Faculty of Pharmacy in Hradec Králové, Department of Analytical Chemistry, Ak. Heyrovského 1203, 500 05, Hradec Králové, Czech Republic.
University of Orleans, Institute of Organic and Analytical Chemistry (ICOA), CNRS UMR 7311, Pôle de Chimie, rue de Chartres, BP 6759, 45067, Orleans Cedex 2, France.
Anal Chim Acta. 2018 Nov 30;1034:184-194. doi: 10.1016/j.aca.2018.06.013. Epub 2018 Jun 8.
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 UPC 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. 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.
已开发出一种快速且简单的超高性能超临界流体色谱 (UHPSFC) 方法，用于测定九种防晒霜（紫外线滤光剂），即 2-乙基己基-2-羟基苯甲酸酯（ES）、乙基己基甲氧基肉桂酸酯（EMC）、二苯酮-3（BZ3）、奥克立林（OCR）、双-乙基己氧基苯酚甲氧基二苯并三嗪（EMT）、丁基甲氧基二苯甲酰基甲烷（BDM）、二乙基氨基羟基苯甲酰基己基苯甲酸酯（DHB）、乙基己基三嗪酮（ET）和二乙基己基丁酰胺基三嗪酮（DBT）在化妆品样品中的含量。分离是在 Acquity UPC Torus 2-PIC（100×3.0mm，1.7μm）柱上实现的。评估了关键色谱参数对分辨率的影响。最佳流动相为含有乙酸铵的二氧化碳和甲醇的梯度混合物，流速为 1.2mL min。系统的背压设定为 150bar，温度设定为 40°C。根据吸光度最大值，化合物在 280nm、305nm 和 340nm 处用二极管阵列检测法测定。所提出的 UHPSFC 方法在 2.5min 内提供了九种目标防晒霜的分离，无需繁琐的样品预处理程序。该方法根据总误差和准确度概况的概念进行了验证。在法国和捷克共和国的两个独立实验室之间评估了实验室间重现性。通过应用于从法国市场获得的含有商业防晒霜的化妆品样品，证明了所开发方法的可靠性。所测定量限表明，考虑到欧盟要求，该方法适用于测定紫外线滤光剂。
