Guo Jie-Hong, Li Xing-Hong, Cao Xue-Li, Li Yan, Wang Xi-Zhi, Xu Xiao-Bai
State Key Laboratory of Environmental Chemistry and Eco-toxicology, Research Center of Eco-Environment Sciences, Chinese Academy of Sciences, Beijing, China.
J Chromatogr A. 2009 Apr 10;1216(15):3038-43. doi: 10.1016/j.chroma.2009.02.021. Epub 2009 Feb 13.
In this study, dispersive liquid-liquid microextraction (DLLME) combined with ultra-high-pressure liquid chromatography (UHPLC)-tunable ultraviolet detection (TUV), has been developed for pre-concentration and determination of triclosan (TCS), triclocarban (TCC) and methyl-triclosan (M-TCS) in aqueous samples. The key factors, including the kind and volume of extraction solvent and dispersive solvent, extraction time, salt effect and pH, which probably affect the extraction efficiencies were examined and optimized. Under the optimum conditions, linearity of the method was observed in the range of 0.0500-100 microg L(-1) for TCS, 0.0250-50.0 microg L(-1) for TCC, and 0.500-100 microgL(-1) for M-TCS, respectively, with correlation coefficients (r(2))>0.9945. The limits of detection (LODs) ranged from 45.1 to 236 ng L(-1). TCS in domestic waters was detected with the concentration of 2.08 microg L(-1). The spiked recoveries of three target compounds in river water, irrigating water, reclaimed water and domestic water samples were achieved in the range of 96.4-121%, 64.3-84.9%, 77.2-115% and 75.5-106%, respectively. As a result, this method can be successfully applied for the rapid and convenient determination of TCS, TCC and M-TCS in real water samples.
在本研究中，已开发出分散液液微萃取（DLLME）结合超高压液相色谱（UHPLC）-可调紫外检测（TUV）的方法，用于水样中三氯生（TCS）、三氯卡班（TCC）和甲基三氯生（M-TCS）的预浓缩和测定。研究并优化了可能影响萃取效率的关键因素，包括萃取溶剂和分散溶剂的种类及体积、萃取时间、盐效应和pH值。在最佳条件下，该方法对TCS的线性范围为0.0500 - 100 μg L⁻¹，对TCC为0.0250 - 50.0 μg L⁻¹，对M-TCS为0.500 - 100 μg L⁻¹，相关系数（r²）>0.9945。检测限（LODs）范围为45.1至236 ng L⁻¹。检测到生活用水中TCS的浓度为2.08 μg L⁻¹。在河水、灌溉水、再生水和生活用水样品中，三种目标化合物的加标回收率分别在96.4 - 121%、64.3 - 84.9%、77.2 - 115%和75.5 - 106%之间。结果表明，该方法可成功应用于实际水样中TCS、TCC和M-TCS的快速便捷测定。
