Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, Salamanca, Spain.
J Chromatogr A. 2011 Jul 29;1218(30):4856-62. doi: 10.1016/j.chroma.2011.02.054. Epub 2011 Mar 12.
A method using headspace generation and in situ derivatization with water soluble EDC (1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide) and TFEA (2,2,2-trifluoroethylamine) has been optimized for the determination of ibuprofen (2-(p-isobutylphenyl)propionic acid), one of the most common non-steroid anti-inflammatory drug (NSAIDs) residues in surface and wastewater samples. Derivatization was carried out in the vial of the headspace sampler (HS) in only 15 min, after which instrumental measurements were made with gas chromatography-mass spectrometry (GC-MS). As the injection system, a programmed temperature vaporizer (PTV) in the solvent-vent injection mode is proposed in order to increase the sensitivity of the measurements. The effects of the variables affecting HS generation, the derivatization reaction, and the instrumental PTV conditions were studied. A limit of quantification as low as 32 ng/L was achieved, and repeatability values were below 10%. Accuracy of the method was evaluated using spiked ultrapure water at three concentration levels, obtaining apparent recoveries between 96% and 104%. The proposed method was applied to the quantification of ibuprofen in sea water and urban wastewater samples.
一种使用顶空生成和水溶性 EDC（1-[3-（二甲基氨基）丙基]-3-乙基碳二亚胺）和 TFEA（2,2,2-三氟乙基胺）原位衍生化的方法已被优化，用于测定布洛芬（2-（对异丁基苯基）丙酸），这是表面和废水中最常见的非甾体抗炎药（NSAIDs）残留之一。衍生化仅在顶空采样器（HS）的小瓶中进行 15 分钟，然后使用气相色谱-质谱（GC-MS）进行仪器测量。作为注射系统，提出了溶剂-吹扫进样模式下的程序升温汽化器（PTV），以提高测量的灵敏度。研究了影响 HS 生成、衍生化反应和仪器 PTV 条件的变量的影响。达到了低至 32 ng/L 的定量下限，重复性值低于 10%。使用三个浓度水平的加标超纯水评估了该方法的准确性，得到了 96%至 104%的表观回收率。该方法已应用于海水中和城市废水中布洛芬的定量。
