Determination of perchlorate from tea leaves using quaternary ammonium modified magnetic carboxyl-carbon nanotubes followed by liquid chromatography-tandem quadrupole mass spectrometry.

The novel quaternary ammonium modified magnetic carboxyl-carbon nanotubes (QA-Mag-CCNTs) have been synthesised and characterized. QA-Mag-CCNTs were applied in magnetic dispersive solid phase extraction (Mag-dSPE) for preconcentration of perchlorate from tea leaves prior to liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) analysis. The Mag-dSPE procedure for preconcentration of perchlorate succeed in overcoming the flaw (containing target analyte randomly) of commercially available SPE cartridge. Under optimal conditions, the results showed higher extraction efficiency of QA-Mag-CCNTs, with recoveries between 85.2% and 107%. And the satisfactory precision with inter-day and intra-day RSD values were lower than 8.0%. Furthermore, QA-Mag-CCNTs were evaluated for reuse up to 20 times. The limit of quantification (LOQ) for perchlorate was 8.21 ng kg-1. The developed method was successfully applied in tea leaves for food-safety risk monitoring in Zhejiang province, China. The results showed the concentrations of perchlorate in 229 out of 240 collected samples were in the range of 0.082-988 µg kg-1. It was confirmed that QA-Mag-CCNTs were highly effective materials used for preconcentration of perchlorate.

Three-dimensional ionic liquid-ferrite functionalized graphene oxide nanocomposite for pipette-tip solid phase extraction of 16 polycyclic aromatic hydrocarbons in human blood sample.

Polycyclic aromatic hydrocarbons (PAHs) are ubiquitously found in the environment and have been proved to be prospectively associated with the risk of cancer. In this study, a simple method based on pipette-tip solid phase extraction (PT-SPE) and gas chromatography-mass spectrometry (GC-MS) has been firstly developed for the determination of 16 PAHs in human whole blood. Three-dimensional ionic liquid-ferrite functionalized graphene oxide nanocomposite (3D-IL-Fe3O4-GO) was used as sorbent in PT-SPE. Compared with conventional SPE method, the PT-SPE method was solvent-saving (1.0 mL), reusable (at least 10 times) and required less blood sample (200 µL). Affecting parameters on extraction efficiency were investigated and optimized. Under the optimized conditions, a good linearity was obtained and the recoveries of 16 PAHs at three spiked levels ranged from 85.0% to 115%. The limits of quantification (LOQs) were in the range of 0.007-0.013 µg/L. Furthermore, the developed method was successfully applied to the analysis of 16 PAHs in 14 human blood samples. The results showed that the predominant PAHs in human whole blood was low-molecular-weight PAHs, with the rank order phenanthrene (PHE)> naphthalene (NAP)> fluorene (FLU)> fluoranthene (FLT)> pyrene (PYR). Because of its simplicity, accuracy and reliability, the PT-SPE method combined with GC-MS demonstrated the applicability for clinical analysis and provided more information for PAHs exposure studies.

Sorption of wastewater containing reactive red X-3B on inorgano-organo pillared bentonite.

Bentonite is a kind of natural clay with good exchanging ability. By exchanging its interlamellar cations with various soluble cations, such as quaternary ammonium cations and inorganic metal ions, the properties of natural bentonite can be greatly improved. In this study, hexadecyltrimethylammonium bromide (HDTMA), CaCl(2), MgCl(2), FeCl(3), AlCl(3) were used as organic and inorganic pillared materials respectively to produce several kinds of Ca-, Mg-, Fe-, Al-organo pillared bentonites. Sorption of reactive red X-3B on them was studied to determine their potential application as sorbents in wastewater treatment. The results showed that these pillared bentonites had much improved sorption properties, and that the dye solutions' pH value had some effect on the performance of these inorgano-organo pillared bentonites. Isotherms of reactive X-3B on these pillared bentonites suggested a Langmuir-type sorption mechanism.

Adsorption of direct green B on mixed hydroxy-Fe-Al pillared montmorillonite with large basal spacing.

Through cation-exchanging of montmorillonite, mixed hydroxy Fe-Al-pillared montmorillonites with large basal spacing were synthesized. The application of these mixed hydroxy Fe-Al-pillared montmorillonites as adsorbents in the areas of environmental protection and pollution control was investigated. Adsorption of Direct Green B, an organic dye, on OH--Fe--, OH--Al--, OH--Fe--Al-- pillared montmorillonites was studied. Results showed that these pillared montmorillonites had much better adsorption properties than traditional Na-organo-montmorillonite. It was also found that pH of the solutions had great effect on the performance of these hydroxy-metal pillared montmorillonites in treating the wastewater containing Direct Green B.

Preparation and characterization of mixed hydroxy-Fe-Al pillared montmorillonite with large basal spacing.

Mixed hydroxy-Al-Fe pillared montmorillonites with large basal spacing were successfully prepared through cation-exchanging of Na+ - montmorillonite with mixed hydroxy-Al and hydroxy-Fe pillaring solutions made from hydrolysis of corresponding metal salts, followed by calcination to convert hydroxy-Al and hydroxy-Fe into intercalated polycations. According to XRD analysis, the basal spacing d(001) of pillared products dramatically enlarged from 12.7 A in the Na-montmorillonite to 81 A in the hydroxy-Fe -montmorillonite and 77.5 A in mixed hydroxy-Al-Fe-montmorillonite. The N2 BET surface areas of the pillared montmorillonites also greatly increased to more than 200 m2/g as compared to about 27 m2/g for the Na-montmorillonite. IR analysis of hydroxy-Fe, and mixed hydroxy-Al-Fe pillared montmorillonites revealed a new absorption vibration at 1384 cm(-1) wavelength. XRF elemental analysis data also showed a high content of Fe2O3 in the hydroxy-Fe pillared montmorillonite.