title: Low-density solvent-based solvent demulsification dispersive liquid-liquid microextraction for the fast determination of trace levels of sixteen priority polycyclic aromatic hydrocarbons in environmental water samples.
abstract: For the first time, the low-density solvent-based solvent demulsification dispersive liquid-liquid microextraction was developed for the fast, simple, and efficient determination of 16 priority polycyclic aromatic hydrocarbons (PAHs) in environmental samples followed by gas chromatography-mass spectrometric (GC-MS) analysis. In the extraction procedure, a mixture of extraction solvent (n-hexane) and dispersive solvent (acetone) was injected into the aqueous sample solution to form an emulsion. A demulsification solvent was then injected into the aqueous solution to break up the emulsion, which turned clear and was separated into two layers. The upper layer (n-hexane) was collected and analyzed by GC-MS. No centrifugation was required in this procedure. Significantly, the extraction needed only 2-3 min, faster than conventional DLLME or similar techniques. Another feature of the procedure was the use of a flexible and disposable polyethylene pipette as the extraction device, which permitted a solvent with a density lighter than water to be used as extraction solvent. This novel method expands the applicability of DLLME to a wider range of solvents. Furthermore, the method was simple and easy to use, and some additional steps usually required in conventional DLLME or similar techniques, such as the aforementioned centrifugation, ultrasonication or agitation of the sample solution, or refrigeration of the extraction solvent were not necessary. Important parameters affecting the extraction efficiency were investigated in detail. Under the optimized conditions, the proposed method provided a good linearity in the range of 0.05-50 μg/L, low limits of detection (3.7-39.1 ng/L), and good repeatability of the extractions (RSDs below 11%, n=5). The proposed method was successfully applied to the extraction of PAHs in rainwater samples, and was demonstrated to be fast, efficient, and convenient.
authors.affiliation: Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
authors.forename: Liang
authors.initials: L
authors.lastname: Guo
authors.forename: Hian Kee
authors.initials: HK
authors.lastname: Lee
mesh_terms: D005591:Chemical Fractionation / Q000295:instrumentation / Q000379:methods*; D004655:Emulsions; D008401:Gas Chromatography-Mass Spectrometry; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis / Q000302:isolation & purification*; D012997:Solvents / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D004655:Emulsions; D011084:Polycyclic Aromatic Hydrocarbons; D012997:Solvents; D014874:Water Pollutants, Chemical