Low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the fast determination of phthalate esters in bottled water.

For the first time, a novel low-density solvent-based vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction (LDS-VSLLME) was developed for the fast, simple and efficient determination of six phthalate esters (PEs) in bottled water samples followed by gas chromatography-mass spectrometry (GC-MS). In the extraction procedure, the aqueous sample solution was injected into a mixture of extraction solvent (toluene) and surfactant (cetyltrimethyl ammonium bromide), which were placed in a glass tube with conical bottom, to form an emulsion by the assistance of vortex agitation. After extraction and phase separation by centrifugation, and removal of the spent sample, the toluene extract was collected and analyzed by GC-MS. The addition of surfactant enhanced the dispersion of extraction solvent in aqueous sample and was also favorable for the mass transfer of the analytes from the aqueous sample to the extraction solvent. Moreover, using a relatively less toxic surfactant as the emulsifier agent overcame the disadvantages of traditional organic dispersive solvents that are usually highly toxic and expensive and might conceivably decrease extraction efficiency to some extent since they are not as effective as surfactants themselves in generating an emulsion. With the aid of surfactant and vortex agitation to achieve good organic extraction solvent dispersion, extraction equilibrium was achieved within 1 min, indicating it was a fast sample preparation technique. Another prominent feature of the method was the simple procedure to collect a less dense than water solvent by a microsyringe. After extraction and phase separation, the aqueous sample was removed using a 5-mL syringe, thus leaving behind the extract, which was retrieved easily. This novel method simplifies the use of low-density solvents in DLLME. Under the optimized conditions, the proposed method provided good linearity in the range of 0.05-25 μg/L, low limits of detection (8-25 ng/L) and good enrichment factors up to 290. The proposed method was successfully applied to the extraction of PEs in bottled water samples as a fast, efficient, and convenient method.

Zhang Y ，Lee HK 《-》

Determination of phthalate esters in liquor samples by vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction followed by GC-MS.

A novel method using vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction has been developed for the extraction of phthalate esters (PAEs) in Chinese liquor samples prior to analysis by GC-MS. In the proposed method, a high-density extraction solvent (carbon tetrachloride) was dispersed into samples with the aid of a surfactant (Triton X-100) and vortex agitation, resulting in a short extraction equilibrium (30 s). After centrifugation, a single microdrop of solvent was easily collected for GC-MS analysis. Key factors that affected the extraction efficiency were optimized. Under the optimum conditions, linearity was found in the range from 0.05 to 50 μg/L. Coefficients of determination varied from 0.9938 to 0.9971. LODs, based on an S/N of 3, ranged from 4.9 to 13 ng/L. Enrichment factors varied from 140 to 184. Reproducibility and recoveries were assessed by testing a series of three liquor samples that were spiked with different concentration levels. Finally, the proposed method was successfully applied to the determination of PAEs in 16 Chinese liquor samples. In this work, high-density-solvent vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction was applied for the first time for the extraction of PAEs in Chinese liquor samples and was proved to be simple, rapid, and sensitive.

Leng G ，Chen W ，Zhang M ，Huang F ，Cao Q ... -  《-》

Vortex-assisted micro-solid-phase extraction followed by low-density solvent based dispersive liquid-liquid microextraction for the fast and efficient determination of phthalate esters in river water samples.

A simple and efficient two-step method, vortex-assisted micro-solid-phase extraction (VA-μ-SPE) followed by low-density solvent based dispersive liquid-liquid microextraction (LDS-DLLME) combined with analysis by gas chromatography-mass spectrometry (GC-MS), was developed for the determination of trace level phthalate esters in environmental water samples. The analytes were firstly extracted and preconcentrated by vortex-assisted μ-SPE which was faster than conventional μ-SPE (6min compared to 30min), and then desorbed by ultrasonication into acetonitrile. The latter served as the dispersive solvent in the subsequent LDS-DLLME step which further pre-concentrated the analytes. Six phthalate esters were selected as model compounds for developing and evaluating the method. Some key parameters for VA-μ-SPE and LDS-DLLME, such as sorbent selection and amount, vortex time, ultrasonication solvent and time, extraction solvent type and volume for DLLME, the speed and time of centrifugation, were investigated. Under the most favorable conditions, good limits of detection (as low as 0.006μg/L) and repeatability of extraction (RSDs below 9.2%, n=5) were obtained. The developed method was applied to determine phthalate esters in environmental water samples.

Guo L ，Lee HK 《-》

Green aspects, developments and perspectives of liquid phase microextraction techniques.

Determination of analytes at trace levels in complex samples (e.g. biological or contaminated water or soils) are often required for the environmental assessment and monitoring as well as for scientific research in the field of environmental pollution. A limited number of analytical techniques are sensitive enough for the direct determination of trace components in samples and, because of that, a preliminary step of the analyte isolation/enrichment prior to analysis is required in many cases. In this work the newest trends and innovations in liquid phase microextraction, like: single-drop microextraction (SDME), hollow fiber liquid-phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME) have been discussed, including their critical evaluation and possible application in analytical practice. The described modifications of extraction techniques deal with system miniaturization and/or automation, the use of ultrasound and physical agitation, and electrochemical methods. Particular attention was given to pro-ecological aspects therefore the possible use of novel, non-toxic extracting agents, inter alia, ionic liquids, coacervates, surfactant solutions and reverse micelles in the liquid phase microextraction techniques has been evaluated in depth. Also, new methodological solutions and the related instruments and devices for the efficient liquid phase micoextraction of analytes, which have found application at the stage of procedure prior to chromatographic determination, are presented.

Spietelun A ，Marcinkowski Ł ，de la Guardia M ，Namieśnik J ... -  《-》

Rapid screening of five phthalate esters from beverages by ultrasound-assisted surfactant-enhanced emulsification microextraction coupled with gas chromatography.

Yan H ，Cheng X ，Yan K 《-》