Rapid magnetic enrichment and sensitive detection of Sudan pollutants with nanoscale zero valent iron-based nanomaterials in combination with liquid chromatography-ultraviolet detector.

In present work, we reported a new nanomaterial nano Fe0 decorated with SiO2 and dopamine by self-assembly method (Fe@SiO2@PDA). A sensitive method for determination of Sudan pollutants in aqueous samples was developed using Fe@SiO2@PDA as magnetic solid phase extraction adsorbents prior to high-performance liquid chromatography with variable wavelength detector. The possible parameters which would affect the enrichment have been optimized. The best parameters were as follows: elutent, 4.5 mL methanol; adsorbent dosage, 30 mg; adsorption time, 20 min; elution time, 18 min; sample pH 7; sample volume, 40 mL. The experimental results demonstrated that Fe@SiO2@PDA exhibited good adsorption properties to Sudan Red dyes. The established method provided excellent linear ranges over 0.01-50 µg L-1 and detection limits ranged from 2.0 to 5.1 ng L-1 for Sudan red I-IV. The developed method was also evaluated with real water samples and the results demonstrated that it was of applicative value owing to its merits including robustness, easy operation, fastness, cheapness and high enrichment efficiency, and had great prospect in environmental fields.

Tetrabromobisphenol A photoelectrocatalytic degradation using reduced graphene oxide and cerium dioxide comodified TiO2 nanotube arrays as electrode under visible light.

Tetrabromobisphenol A, one of the most important brominated retardants, is an typical persistent organic pollutant and it is of great value to develop rapid and effective degradation method. Present study established a photoelectrodegradation method with CeO2 and reduced graphene oxide co-modified TiO2 nanotube arrays (RGO-CeO2-TiO2 NAs), which were successfully synthesized and characterized with scanning electron microscopy (SEM) and Energy Dispersive X Ray Spectrometry (EDX). The SEM Images revealed that the nanotubes had a diameter of about 100 nm and an obvious layer of CeO2 and RGO on the surface of TiO2 nanotube arrays. The EDX data exhibited the presence of Ce element. The results demonstrated that TBBPA was degraded at a high degradation rate constant of 0.0191 min-1, and photogenerated holes played a major role in the degradation reaction. Significant decrease of degradation efficiency was achieved with the presence of EDTA-2Na(hole scavenger), yet while the existence of t-BuOH(OH scavenger) resulted in less inhibition on the degradation. Besides, RGO-CeO2-TiO2 NAs exhibited good stability with rarely decline of degradation efficiency for ten reused runs. All these indicated that RGO-CeO2-TiO2 NAs were a good catalyst with extraordinary catalytic activity and stability for PEC degradation, and would have great potential in the control and removal of pollutants.

Determination of 1-naphthol and 2-naphthol from environmental waters by magnetic solid phase extraction with Fe@MgAl-layered double hydroxides nanoparticles as the adsorbents prior to high performance liquid chromatography.

Magnetic Fe@MgAl-layered double hydroxides (MgAl-LDHs) composite was firstly synthesized by coating MgAl-layered double hydroxides on the surface of the dispersed nanoscale zero valent irons with co-precipitation method and characterized by transmission electron microscopy and X-ray diffraction techniques. The synthesized Fe@MgAl-LDHs nanoparticles were investigated for magnetic solid phase extraction (MSPE) of 1-naphthol and 2-naphthol from the water samples. The elutent containing 1-naphthol and 2-naphthol was analyzed by high performance liquid chromatography with variable wavelength detection (HPLC-UV). Under optimal conditions, there is good linear relationship between the concentration and the peak area in the range of 0.5-200 µgL(-1) with the correlation coefficients (r(2)) above 0.998 for 1-naphthol and 2-naphthol. The limits of detection were 0.22 µgL(-1) and 0.19 µgL(-1) for 1-naphthol and 2-naphthol, respectively, and precisions were both below 2.5% (n=6). The real water analysis demonstrated that the spiked recoveries were in the range of 79.2-80.9% (n=3). All these results indicated that the developed MSPE-HPLC-UV method was proved to be an efficient tool for the analysis of naphthols.

Selenium speciation in tea by dispersive liquid-liquid microextraction coupled to high-performance liquid chromatography after derivatization with 2,3-diaminonaphthalene.

Selenium is an important element for human health, and it is present in many natural drinks and foods. Present study described a new method using dispersive liquid-liquid microextraction prior to high-performance liquid chromatography with a UV variable wavelength detector for the determination of the total selenium, Se(IV), Se(VI), and total organoselenium in tea samples. In the procedure, 2,3-diaminonaphthalene was used as the chelating reagent, 400 µL acetonitrile was used as the disperser solvent and 60 µL chlorobenzene was used as the extraction solvent. The complex of Se(IV) and 2,3-diaminonaphthalene in the final extracted phase was analyzed by high-performance liquid chromatography. The factors influencing the derivatization and microextraction were investigated. Under the optimal conditions, the limit of detection was 0.11 µg/L for Se(IV) and the linearity range was in the range of 0.5-40 µg/L. This method was successfully applied to the determination of selenium in four tea samples with spiked recoveries ranging from 91.3 to 100%.

Dispersive liquid-liquid microextraction combined with high-performance liquid chromatography for the enrichment and sensitive determination of Sudan Red pollutants in water samples.

Sudan Red pollutants have gained more attention in recent years. The present study described a simple and sensitive determination method for Sudan Red pollutants with dispersive liquid-liquid microextraction coupled to high-performance liquid chromatography. Chlorobenzene and ethanol were used as the extraction solvent and disperser solvent, respectively. The possible parameters such as the kind of solvents, ionic strength, and sample pH that could affect the enrichment have been optimized. Under the optimal conditions, the pollutants have been well enriched and the linear ranges of Sudan Red I and II were in the range of 0.3-40 µg/L, and the linear ranges of Sudan Red III and IV were in the range of 1.2-160 µg/L. The detection limits were in the range of 0.18-0.46 µg/L, and the precisions were in the range of 3.7-5.9%. All these demonstrated that the proposed method could be a good alternative for the routine analysis of Sudan Red pollutants in water samples.

Simultaneous determination of nickel, cobalt and mercury ions in water samples by solid phase extraction using multiwalled carbon nanotubes as adsorbent after chelating with sodium diethyldithiocarbamate prior to high performance liquid chromatography.

Multiwalled carbon nanotubes (MWNTs) have been widely used for the enrichment of trace important pollutants in environment because of its large specific surface area, high extraction efficiency, and easy operation. In this study, a solid phase extraction method was established to determine nickel (Ni(2+)), cobalt (Co(2+)) and mercury (Hg(2+)) ions using MWNTs as the adsorbent and sodium diethyldithiocarbamate (DDTC) as the chelating agent. The final analysis was performed on a high performance liquid chromatography (HPLC). The factors that may influence the extraction efficiency were optimized in detail including the type and volume of elution solvent, sample pH, volume of chelating agent solution, and volume of sample solution, etc. The experimental results indicated that good linear relationship between peak area and the concentration of the ions was achieved in the range of 0.1-100µgL(-1), 0.1-50µgL(-1), and 2.7-300µgL(-1) for Ni(2+), Co(2+), and Hg(2+), respectively. The precision was determined by calculating the relative standard deviation (R.S.D.) values that were in the range of 6.2-11.7% under the optimal conditions. The detection limits of Ni(2+), Co(2+), and Hg(2+) were in the range of 0.04-0.9µgL(-1) (S/N=3). The presented method was applied for the determination of the metal ions mentioned above in real water samples, and satisfied results were achieved. All these indicated that proposed method will be a good alternative tool for monitoring the target ions in environmental samples in the future.