Determination of diethylstilbestrol in milk using carbon nanotube-reinforced hollow fiber solid-phase microextraction combined with high-performance liquid chromatography.
Determination of diethylstilbestrol in milk using carbon nanotube-reinforced hollow fiber solid-phase microextraction combined with high-performance liquid chromatography.
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DOI：
10.1016/j.talanta.2012.04.021
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发表时间：
2012-08
期刊：
影响因子：
6.1
通讯作者：
Yang Yang-Yang;Juan Chen;Yan-ping Shi
中科院分区：
文献类型：
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作者：
Yang Yang-Yang;Juan Chen;Yan-ping Shi
采用碳纳米管增强中空纤维固相微萃取（CNTs-HF-SPME）结合高效液相色谱（HPLC）对乳制品中己烯雌酚（DES）进行提取和测定。使用溶胶-凝胶技术，用多壁碳纳米管（MWCNT）填充中空纤维的壁孔。在所提出的方法中，DES 通过 MWCNT 选择性萃取，解吸到甲醇中，并通过 HPLC 进行分析。对影响CNTs-HFSPME效率的参数，如中空纤维的长度、萃取和解吸次数、萃取温度、搅拌速率、样品溶液的pH值以及样品溶液中有机溶剂和盐的量进行了研究和优化。在优化的提取条件下，该方法表现出良好的线性（24-960μgL−1）、较低的方法检出限（MDL，5.1μgL−1）以及四种不同浓度下的良好回收率。事实证明，该方法简单、快速、灵敏且无需溶剂，可用于分析乳制品中的 DES。
Carbon nanotube-reinforced hollow fiber solid-phase microextraction (CNTs-HF-SPME) combined with high-performance liquid chromatography (HPLC) was used to extract and determine diethylstilbestrol (DES) in milk products. Wall pores of the hollow fiber were filled with multi-walled carbon nanotubes (MWCNTs) using sol–gel technology. In the proposed method, DES was selectively extracted by MWCNTs, desorbed to methanol, and analyzed by HPLC. The parameters affecting the efficiency of CNTs-HFSPME, such as the length of the hollow fiber, extraction and desorption times, extraction temperature, stirring rate, pH of the sample solution, and the amount of organic solvent and salt in the sample solution, were investigated and optimized. Under the optimized extraction conditions, the method showed good linearity (24–960μgL−1), a low method detection limit (MDL, 5.1μgL−1), and good recoveries at four different concentrations. It was proven to be simple, rapid, sensitive, and solvent free for the analysis of DES in dairy products.