Campillo Natalia, Viñas Pilar, Marín Javier, Hernández-Córdoba Manuel
Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence 'Campus Mare Nostrum', University of Murcia, E-30100 Murcia, Spain.
Bioanalysis. 2017 Feb;9(4):369-379. doi: 10.4155/bio-2016-0217. Epub 2017 Jan 19.
Two important markers of oxidative stress, glyoxal and methylglyoxal, are preconcentrated from human urine by surfactant-assisted dispersive liquid-liquid microextraction and separated by LC-fluorescence.
METHODS/RESULTS: Derivatization was carried out overnight with 0.8 mM 2,3-diaminonaphthalene at 4°C. For surfactant-assisted dispersive liquid-liquid microextraction, 500 µl buffer solution (pH 10.5) and 25 µl 0.03 M Triton X-114 were added to 2.5 ml of the sample and the mixture was made up to 10 ml before the rapid injection of 75 µl 1-undecanol (extractant solvent) and 0.5 ml ethanol (dispersant solvent).
The method can be applied to analyze glyoxal and methylglyoxal in urine with LOD of 13 and 16 ng/l, respectively, and recoveries in the 88-103% range.
通过表面活性剂辅助分散液液微萃取法对人尿液中的两种重要氧化应激标志物乙二醛和甲基乙二醛进行预富集,并采用液相色谱-荧光法进行分离。
方法/结果:在4℃下,用0.8 mM 2,3-二氨基萘进行过夜衍生化。对于表面活性剂辅助分散液液微萃取,向2.5 ml样品中加入500 μl缓冲溶液(pH 10.5)和25 μl 0.03 M Triton X-114,将混合物定容至10 ml,然后快速注入75 μl 1-十一醇(萃取溶剂)和0.5 ml乙醇(分散溶剂)。
该方法可用于分析尿液中的乙二醛和甲基乙二醛,检测限分别为13和16 ng/l,回收率在88-103%范围内。