An improved fabric‐phase sorptive extraction (FPSE) protocol has been developed and validated herein for the simple, fast, sensitive and green determination of seven parabens—methyl paraben, ethyl paraben, propyl paraben, butyl paraben, isopropyl paraben, isobutyl paraben and benzyl paraben—in human urine samples by HPLC–DAD. The mobile phase consisted of ammonium acetate (0.05 m) and acetonitrile, while total analysis time was 13.2 min. Sol–gel poly (tetrahydrofuran) coated FPSE membrane resulted in optimum extraction sensitivity for the seven parabens. The novel FPSE medium as well as the improved and faster sample preparation procedure resulted in lower limit of detection and quantitation values in comparison with previously reported methods. The separation was carried out using an RP‐HPLC method with a Spherisorb C₁₈ column and a flow rate of 1.4 ml/min. The validation of the analytical method was carried out by means of linearity, precision, accuracy, selectivity, sensitivity and robustness. For all seven parabens, the limits of detection and quantitation were 0.003 and 0.01 μg/ml, respectively. Relative recovery rates were between 86.3 and 104%, while RSD values were <12.6 and 19.3% for within‐ and between‐day repeatability, respectively. The method was subsequently applied to real human urine samples.

中文翻译：

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一种改进的织物相吸附萃取方案，用于通过HPLC-DAD测定人尿中的七种对羟基苯甲酸酯

本文开发并改进了织物相吸附萃取（FPSE）方案，用于简单，快速，灵敏且绿色地测定7种对羟基苯甲酸酯-对羟基苯甲酸甲酯，对羟基苯甲酸乙酯，对羟基苯甲酸丙酯，对羟基苯甲酸丁酯，对羟基苯甲酸异丙酯，对羟基苯甲酸异丁酯和苄基对羟基苯甲酸酯-通过HPLC-DAD在人尿液样品中。流动相由乙酸铵（0.05 m）和乙腈，而总分析时间为13.2分钟。溶胶凝胶聚四氢呋喃涂层的FPSE膜对7种对羟基苯甲酸酯具有最佳的提取灵敏度。与以前报道的方法相比，新颖的FPSE培养基以及改进和更快的样品制备程序可降低检测和定量值的下限。使用RP‐HPLC方法和Spherisorb C _{18进行分离}柱和1.4 ml / min的流速。分析方法的验证是通过线性，精密度，准确性，选择性，灵敏度和鲁棒性进行的。对于所有七个对羟基苯甲酸酯，检出限和定量限分别为0.003和0.01μg/ ml。日内和日间重复性的相对回收率分别在86.3％和104％之间，而RSD值分别<12.6％和19.3％。该方法随后应用于真实的人类尿液样本。