-
[show abstract]
[hide abstract]
ABSTRACT: Triphenylamine (TPA)-functionalized magnetic microspheres (Fe(3)O(4)/SiO(2)/TPA) were prepared and applied as solid phase extraction (SPE) adsorbents for the analysis of polycyclic aromatic hydrocarbons (PAHs) in environmental samples in combination with high-performance liquid chromatography (HPLC). The magnetic solid-phase extraction (MSPE) conditions affecting the extraction efficiency were optimized, including elution solvent, standing time, amount of sorbent, and salt concentration. Due to the strong π-π conjugate effect between the benzene rings of TPA and PAHs, high extraction efficiency was achieved with spiked recoveries of 80.21-108.33% and relative standard deviations (RSD) of less than 10%. Good linearities (R(2) > 0.997) for all calibration curves were obtained with low limits of detection (LOD) of 0.25, 0.5, 0.5, 3.75, 0.2 and 0.04 ng L(-1) for anthracene, fluoranthene, pyrene, chrysene, benzo[b]fluoranthene and benzo[k]fluoranthene, respectively. The achieved results indicate the applicability of Fe(3)O(4)/SiO(2)/TPA as MSPE adsorbents.
The Analyst 04/2012; 137(11):2716-22. · 4.23 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: Titanium wire-based solid phase extraction (SPE) is developed for the analysis of six different polycyclic aromatic hydrocarbons in water samples with coupling with high performance liquid chromatography. The adsorbent is a Ti wire on which TiO(2) nanotubes are first formed by anodization and then Au nanoparticles and n-octadecanethiol are modified. The surface composition and structure of the adsorbent were characterized in detail using field emission scanning electron microscope and Fourier transform infrared spectroscopy. The main parameters affecting the extraction efficiency, such as the volume of the organic modifier, extraction time, elution solvent, and desorption time were optimized. Good linearities ranging from 0.025 to 30 μg L(-1) with correlation coefficients (R(2)) ranging from 0.9964 to 0.9999 and low limits of detection were obtained in spiked water samples. Furthermore, this method was successfully applied in the analysis of real river water samples with recoveries in the range of 75.33-115.83% and relative standard deviations ranging from 4.85 to 10.77%. The developed SPE can be a particularly convenient means of sample pretreatment for environmental water samples.
The Analyst 09/2011; 136(22):4774-9. · 4.23 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: Magnetic microsphere confined ionic liquid was synthesized by covalently bonding N-methylimidazolium on magnetic microspheres. The functionalized magnetic microspheres were characterized by Fourier transform infrared (FT-IR) spectrometry, thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The prepared material was used for the preconcentration of three chlorophenols (CPs) in water combined with high-performance liquid chromatography (HPLC). Several conditions that probably affected the extraction efficiency such as standing time, eluent and its volume, sample pH and volume, were optimized. Under the optimal conditions, good recoveries (70.3-88.8%) were achieved with satisfactory relative standard deviations (RSDs) of less than 6.0%. The limits of detection for the three CPs were 0.20-0.35 μg L(-1). The results indicated that the ionic liquid-functionalized magnetic microspheres show significant promise for the analysis of CPs in environmental samples.
Journal of Environmental Monitoring 02/2011; 13(2):440-5. · 1.99 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: C18-functionalized magnetic microspheres synthesized in a three-stage system and characterized by Fourier transform infrared (FTIR) spectroscopy and SEM were applied for clean-up and enrichment of polycyclic aromatic hydrocarbons (PAHs) in soil samples combined with ultrasonication extraction. Magnetic solid-phase extraction (MSPE) parameters, such as elution solvents, amounts of sorbents, enrichment time and organic modifier, were optimized together with ultrasonication time and extraction solvents. Under the optimal conditions, the developed method provided spiked recoveries of 63.2-92.8% with RSDs of less than 6.4% and limits of detection were 0.5-1.0 ng/g. This new method provides several advantages, such as high extraction efficiency, convenient extraction procedure and short analysis times. Finally, the method was successfully applied to the determination of polycyclic aromatic hydrocarbons in soil samples.
Journal of Separation Science 02/2011; 34(6):716-23. · 2.73 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: In this paper, ionic liquid (IL)-coated magnetic Fe(3)O(4) nanoparticles (NPs) as an adsorbent of mixed hemimicelles solid-phase extraction (SPE) was investigated for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) from environmental samples. Due to the high surface area and excellent adsorption capacity of the Fe(3)O(4) NPs after modification with ILs, satisfactory extraction recoveries can be achieved with only 80 mg Fe(3)O(4) NPs, 50 mg IL, 300 mL solution at pH = 10 and 10 min for equilibration. A comprehensive study of the adsorption conditions such as the amount of Fe(3)O(4) NPs and ILs, the solution pH, ionic strength, standing time, breakthrough volume, and desorption solvents was presented. The extraction ability of different coating agents, such as 1-hexadecyl-3-methylimidazolium bromide (C(16)mimBr), 1-decyl-3-methylimidazolium bromide (C(10)mimBr) and cationic surfactant cetyltrimethylammonium bromide (CTAB) was also compared. Under the optimized conditions, the recoveries for the water samples analysis were between 76 and 105% with relative standard deviations (RSDs) ranging from 3.9 to 6.9%, and the recoveries for soil samples were between 73 and 104% with RSDs ranging from 1.0 to 6.3%. In this method, only a small amount of C(16)mimBr (50 mg) and Fe(3)O(4) NPs (80 mg) was needed to obtain satisfactory recoveries.
The Analyst 09/2010; 135(9):2426-33. · 4.23 Impact Factor
-
[show abstract]
[hide abstract]
ABSTRACT: Recently, amino acid ionic liquids (AAILs) have attracted much research interest. In this paper, we present the first application of AAILs in chiral separation based on the chiral ligand exchange principle. By using 1-alkyl-3-methylimidazolium L-proline (L-Pro) as a chiral ligand coordinated with copper(II), four pairs of underivatized amino acid enantiomers-dl-phenylalanine (dl-Phe), dl-histidine (dl-His), dl-tryptophane (dl-Trp), and dl-tyrosine (dl-Tyr)-were successfully separated in two major chiral separation techniques, HPLC and capillary electrophoresis (CE), with higher enantioselectivity than conventionally used amino acid ligands (resolution (R(s))=3.26-10.81 for HPLC; R(s)=1.34-4.27 for CE). Interestingly, increasing the alkyl chain length of the AAIL cation remarkably enhanced the enantioselectivity. It was inferred that the alkylmethylimidazolium cations and L-Pro form ion pairs on the surface of the stationary phase or on the inner surface of the capillary. The ternary copper complexes with L-Pro are consequently attached to the support surface, thus inducing an ion-exchange type of retention for the dl-enantiomers. Therefore, the AAIL cation plays an essential role in the separation. This work demonstrates that AAILs are good alternatives to conventional amino acid ligands for ligand-exchange-based chiral separation. It also reveals the tremendous application potential of this new type of task-specific ILs.
Chemistry 09/2009; 15(38):9889-96. · 5.93 Impact Factor
