Celeiro Maria, Acerbi Ruben, Kabir Abuzar, Furton Kenneth G, Llompart Maria
CRETUS Institute, Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, Universidade de Santiago de Compostela, E-15782, Santiago de Compostela, Spain.
International Forensic Research Institute, Department of Chemistry and Biochemistry, Florida International University, Miami, FL-33199, USA.
Anal Chim Acta X. 2019 Dec 17;4:100038. doi: 10.1016/j.acax.2019.100038. eCollection 2020 Mar.
A novel method based on fabric phase sorptive extraction (FPSE) followed by gas chromatography-tandem mass spectrometry (GC-MS/MS) has been validated for the simultaneous determination of 11 UV filters (ethylhexyl salicylate, benzyl salicylate, homosalate, benzophenone-3, isoamylmethoxycinnamate, 4-methylbenzylidenecamphor, methyl anthranilate, etocrylene, 2-ethylhexylmethoxycinnamate, 2-ethylhexyl -dimethylaminobenzoate, and octocrylene), in natural and recreational waters. Major experimental parameters affecting FPSE procedure have been optimized to obtain the highest extraction efficiency. Different types and sizes of sol-gel coated FPSE media, sample volume, extraction time, and type and volume of desorption solvent were evaluated. The optimal conditions involved the use of a (2.0 × 2.5) cm FPSE device with PDMS based coating for the extraction of 20 mL of water for 20 min. The quantitative desorption of the target compounds was performed with 0.5-1 mL of ethyl acetate. The method was satisfactorily validated in terms of linearity, precision, repeatability and reproducibility. Recovery studies were performed at different concentration levels in real water matrices to show its suitability, obtaining mean values about 90% and satisfactory precision. LODs were at the low ng L in all cases. Finally, the validated FPSE-GC-MS/MS method was applied to different real samples, including environmental water (lake, river, seawater) and recreational water (swimming-pool), where 8 out of the 11 studied compounds were detected at concentrations between 0.12-123 μg L. FPSE is proposed as an efficient and simple alternative to other extraction and microextraction techniques for the analysis of UV filters in waters. Since no matrix effects were observed, quantification could be carried out by conventional calibration with standard solutions, without the need to perform the complete FPSE procedure, thus allowing a higher throughput in comparison with other microextraction techniques.
一种基于织物相吸附萃取（FPSE）结合气相色谱-串联质谱（GC-MS/MS）的新方法已得到验证，可用于同时测定天然水和娱乐用水中的11种紫外线过滤剂（乙基己基水杨酸酯、苄基水杨酸酯、胡莫柳酯、二苯甲酮-3、异戊基甲氧基肉桂酸酯、4-甲基亚苄基樟脑、邻氨基苯甲酸甲酯、依茨基林、2-乙基己基甲氧基肉桂酸酯、2-乙基己基二甲基氨基苯甲酸酯和奥克立林）。已对影响FPSE过程的主要实验参数进行了优化，以获得最高的萃取效率。评估了不同类型和尺寸的溶胶-凝胶涂层FPSE介质、样品体积、萃取时间以及解吸溶剂的类型和体积。最佳条件包括使用尺寸为(2.0×2.5) cm、基于聚二甲基硅氧烷（PDMS）涂层的FPSE装置，萃取20 mL水20分钟。目标化合物的定量解吸使用0.5 - 1 mL乙酸乙酯进行。该方法在线性、精密度、重复性和再现性方面得到了令人满意的验证。在实际水样的不同浓度水平上进行了回收率研究，以证明其适用性，获得的平均值约为90%，精密度良好。所有情况下的检测限均处于低纳克/升水平。最后，经过验证的FPSE-GC-MS/MS方法应用于不同的实际样品，包括环境水（湖泊、河流、海水）和娱乐用水（游泳池），在所研究的11种化合物中，有8种在0.12 - 123 μg/L的浓度范围内被检测到。对于水中紫外线过滤剂的分析，FPSE被认为是一种高效且简单的替代其他萃取和微萃取技术的方法。由于未观察到基质效应，可通过使用标准溶液进行常规校准来进行定量，无需执行完整的FPSE程序，因此与其他微萃取技术相比具有更高的通量。
