Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008, Salamanca, Spain.
Anal Bioanal Chem. 2011 Jan;399(2):945-53. doi: 10.1007/s00216-010-4339-7. Epub 2010 Oct 28.
Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption-gas chromatography-mass spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature) were optimised using a Box-Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben (22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated wastewater.
搅拌棒吸附萃取结合原位衍生反应和热解吸-气相色谱-质谱联用成功地应用于水样中对羟基苯甲酸酯（甲基对羟基苯甲酸酯、异丙基对羟基苯甲酸酯、正丙基对羟基苯甲酸酯、丁基对羟基苯甲酸酯和苄基对羟基苯甲酸酯）、三氯生和甲基三氯生的测定。这种方法通过在提取过程中同时进行衍生化反应，以简单的方式提高了 GC 的提取效率和灵敏度。原位衍生化反应在碱性条件下用乙酸酐进行。通过 Box-Behnken 实验设计优化了热解吸参数（冷聚焦温度、解吸流量、解吸时间、解吸温度）。除了甲基对羟基苯甲酸酯（22%）外，所有分析物的回收率均高于 79%。该方法的检测限在 0.64 至 4.12ng/L 之间，具有良好的重现性和准确性。该方法用于测定自来水中和未经处理和处理后的废水中分析物的可行性已得到验证。
