title: Molecular complex-based dispersive liquid-liquid microextraction: analysis of polar compounds in aqueous solution.
abstract: A novel molecular complex-based dispersive liquid-liquid microextraction (DLLME) method was established via hydrogen bond interaction between the extractant and the analytes. In this approach, tri-n-butylphosphate (TBP), a Lewis base, was directly used, instead of the traditional water-immiscible organic solvents, as the extractant for DLLME. The phenols (p-benzenediol, m-benzenediol, o-benzenediol and phenol), which are typical Lewis acids, were successfully extracted from environmental aqueous samples. In addition, phase separation was achieved in a disposable polyethylene pipet with the open and narrow tip upside, for a collection of the above extractant layer, i.e. TBP. To achieve satisfactory extraction performance, several extraction parameters, such as type of extractant solvents, extractant volume, pH of sample solution, ionic strength of sample solution and extraction time, were optimized. Additionally, the proposed method was applied to environmental water samples. Under the optimized conditions, the limits of detection and limits of quantification for the phenols were 7-29 and 25-98 μg/L, respectively. The calibration curves showed good linearity (r(2)≥0.9961) over the investigated concentration range. The repeatability of the method was investigated by evaluating the intra- and inter-day precisions. The relative standard deviations (RSDs) obtained were lower than 11.2% and 13.9% at different concentration levels. The recoveries ranged from 83.2% to 117.8%, with RSDs less than 13.1%. The developed approach provides a new way to facilitate DLLME of organic polar compounds from aqueous solutions. Moreover, it enables a convenient collection of solvent less dense making use of a cheap and disposable polyethylene pipet.
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, China.
authors.forename: Xi-Zhou
authors.initials: XZ
authors.lastname: Hu
authors.forename: Jian-Hong
authors.initials: JH
authors.lastname: Wu
authors.forename: Yu-Qi
authors.initials: YQ
authors.lastname: Feng
mesh_terms: D005591:Chemical Fractionation / Q000379:methods*; D006863:Hydrogen-Ion Concentration; D057927:Hydrophobic and Hydrophilic Interactions; D016014:Linear Models; D010755:Organophosphates / Q000737:chemistry; D010636:Phenols / Q000032:analysis / Q000302:isolation & purification*; D015203:Reproducibility of Results; D045483:Rivers / Q000737:chemistry; D012680:Sensitivity and Specificity; D012722:Sewage / Q000737:chemistry; D014867:Water / Q000737:chemistry*
chemical_list: D010755:Organophosphates; D010636:Phenols; D012722:Sewage; D014867:Water; C009524:tributyl phosphate