Departamento de Medio Ambiente, Instituto Nacional de Investigación y Tecnología Agraria y Alimentaria (INIA), Carretera de la Coruña 7, 28040, Madrid, Spain.
Anal Bioanal Chem. 2016 Nov;408(28):8013-8023. doi: 10.1007/s00216-016-9899-8. Epub 2016 Sep 10.
A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid-liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-μ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated FeO nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated FeO nanoparticles were selected in order to simplify and make more cost-effective the procedure. DLLME was carried out at pH 3, during 2 min, followed by the addition of the nanoparticles for D-μ-SPE employing 1 min in the extraction. Analysis of spiked water samples of different sources gave satisfactory recovery results for all the compounds with detection limits ranging from 7 to 180 ng l. Finally, the procedure was applied in tap, well, and river water. Graphical abstract Diagram of the extraction method using magnetic nanoparticles (MNPs).
一种快速提取程序，用于测定水样中的五种内分泌干扰化合物，雌酮、乙炔基雌二醇、双酚 A、三氯生和 2-乙基己基水杨酸酯。分析包括两步提取程序，即分散液液微萃取（DLLME）与分散微固相萃取（D-μ-SPE）相结合，使用磁性纳米粒子，然后在气相色谱与三重四极杆质谱联用仪的进样口进行原位衍生化。评估并比较了在萃取过程中使用未涂层或油酸盐涂层 FeO 纳米粒子作为吸附剂的情况。通过实验设计优化了萃取过程中的主要参数。选择未涂层的 FeO 纳米粒子以简化和降低成本效益程序。在 pH 3 下进行 DLLME，持续 2 分钟，然后加入纳米粒子进行 D-μ-SPE，萃取时间为 1 分钟。对不同来源的加标水样进行分析，所有化合物的检测限均为 7 至 180ng/L，回收率结果令人满意。最后，该方法应用于自来水、井水和河水。
