Institute of Chemistry and Technical Electrochemistry, Poznan University of Technology, Piotrowo 3, Poznań, Poland.
J Chromatogr A. 2010 Mar 12;1217(11):1761-6. doi: 10.1016/j.chroma.2010.01.054. Epub 2010 Jan 25.
Dispersive liquid-liquid microextraction (DLLME) coupled with high-performance liquid chromatography with fluorescence detector was applied for the determination of alkylphenols and their short-chained ethoxylates in water samples. Development of DLLME procedure included optimisation of some important parameters such as kind and volume of extracting and dispersing solvents. Under optimised conditions 50 microL of trichloroethylene in 1.5 mL of acetone were rapidly injected into 5 mL of a water sample. After centrifuging the organic phase containing the analytes was taken for evaporation with a gentle nitrogen purge and reconstituted to 50 microL of acetonitrile. The aliquot of this solution was analysed with the use of HPLC. For octylphenol (OP) and octylphenol ethoxylates (OPEOs) linearity was satisfactory in the range 8-1000 microg L(-1) and for nonylphenol (NP) and nonylphenol ethoxylates (NPEOs) linearity was in the range from 50 to about 3000 microg L(-1). Limit of quantitation was 0.1 microg L(-1) for OP and OPEOs and 0.3 microg L(-1) for NP and NPEOs. Satisfactory recoveries between 66 and 79% were obtained for environmental samples. The results showed that DLLME is a simple, rapid and sensitive analytical method for the preconcentration of trace amounts of alkylphenols and their ethoxylates in environmental water samples.
分散液液微萃取（DLLME）结合高效液相色谱荧光检测器用于测定水样中的烷基酚及其短链乙氧基化物。DLLME 方法的开发包括优化一些重要参数，如萃取和分散溶剂的种类和体积。在优化条件下，将 50μL 三氯乙烯快速注入 1.5mL 丙酮中，然后迅速注入 5mL 水样中。离心后，将含有分析物的有机相用温和的氮气吹扫蒸发，并重新溶解在 50μL 乙腈中。将该溶液的等分试样用 HPLC 进行分析。对于辛基酚（OP）和辛基酚乙氧基化物（OPEOs），在 8-1000μg/L 范围内具有良好的线性关系，对于壬基酚（NP）和壬基酚乙氧基化物（NPEOs），在 50-3000μg/L 范围内具有良好的线性关系。OP 和 OPEOs 的定量限为 0.1μg/L，NP 和 NPEOs 的定量限为 0.3μg/L。环境样品的回收率在 66-79%之间，结果令人满意。结果表明，DLLME 是一种简单、快速、灵敏的分析方法，可用于环境水样中痕量烷基酚及其乙氧基化物的预浓缩。
