Ferrocene-based nanoporous organic polymer as solid-phase extraction sorbent for the extraction of chlorophenols from tap water, tea drink and peach juice samples.

Ferrocene-based nanoporous organic polymer (Fc-NOP) was used as solid-phase extraction (SPE) adsorbent and showed excellent adsorption capacity for chlorophenols (CPs) compared with commercial C18 and multi-walled carbon nanotubes. Then, a SPE method with Fc-NOP packed cartridge combined with HPLC-UV detection was developed to determine CPs in tap water, black tea drinks and peach juice samples. Under optimal conditions, the detection limits of the method measured at the signal to noise ratio of 3 (S/N = 3) were 0.04-0.06 ng mL-1 for tap water and 0.10-0.20 ng mL-1 for black tea drinks and peach juice samples. Satisfactory method recoveries were achieved in the range of 87.6-119% with relative standard deviations of 3.11-7.83%. Result proved that this method was a sensitive and efficient method for determination of trace CPs in foods. The extraction result for more other compounds confirmed that the developed method had a great application potential for analysis of other trace pollutants in food samples.

Magnetic porous carbon derived from a Zn/Co bimetallic metal-organic framework as an adsorbent for the extraction of chlorophenols from water and honey tea samples.

A novel magnetic porous carbon derived from a bimetallic metal-organic framework, Zn/Co-MPC, was prepared by introducing cobalt into ZIF-8. Magnetic porous carbon that possesses magnetic properties and a large specific surface area was firstly fabricated by the direct carbonization of Zn/Co-ZIF-8. The prepared magnetic porous carbon material was characterized by scanning electron microscopy, transmission electron microscopy, powder X-ray diffraction, N2 adsorption, and vibrating sample magnetometry. The prepared magnetic porous carbon was used as a magnetic solid-phase extraction adsorbent for the enrichment of chlorophenols from water and honey tea samples before high-performance liquid chromatography analysis. Several experimental parameters that could influence the extraction efficiency were investigated and optimized. Under the optimum conditions, good linearities (r > 0.9957) for all calibration curves were obtained with low limits of detection, which are in the range of 0.1-0.2 ng mL(-1) for all the analytes. The results showed that the prepared magnetic porous carbon had an excellent adsorption capability toward the target analytes.

Optimization of Extraction, HPLC and Kinetic Studies for Determination of Some Food Tainting Compounds in Different Food Matrices.

Solid-liquid extraction, ultrasonic-assisted extraction and matrix solid-phase dispersion (MSPD) were optimized and compared in terms of recoveries for the simultaneous extraction of indole (IND) and 2,4-dichlorophenol (DCP) from catfish samples and for the extraction of IND alone from potato samples. Applying high-performance liquid chromatography (HPLC-DAD) procedure using mobile phase of methanol : water (65 : 35) at 280 nm, MSPD was the method of choice for the extraction of IND and DCP from catfish and, also, for IND from potato. The extraction recoveries of MSPD were in the range (97.9-99.7%) and (99.8-100.6%); for IND and DCP, respectively, in catfish samples and (98.4-99.7%) for IND alone in potato samples. Solid-phase extraction (SPE) was chosen the method of choice for the extraction of DCP from fish farms water samples after optimization and comparison with direct sample injection and extraction recoveries were in the range (97.9-100.3%). Kinetics were further studied to follow each of production of IND in catfish during storage at different temperatures and uptake of DCP by tilapia in fish farms water samples using MSPD-HPLC and SPE-HPLC, respectively.

A novel organic-inorganic hybrid monolithic column prepared in-situ in a microchip and its application for the determination of 2-amino-4-chlorophenol in chlorzoxazone tablets.

γ-Alumina nanoparticles (γ-Al2O3) were introduced to the conventional poly(methacrylic acid-co-ethylene glycol dimethacrylate) (MAA-co-EGDMA) monolith to prepare a novel organic-inorganic hybrid monolith, poly(MAA-co-EGDMA)-Al2O3 monolith. The polymerization was induced in-situ with UV irradiation in an ultraviolet transparent polymethyl methacrylate (PMMA) microfluidic chip. The monolith-based solid phase microextraction system was used for the on-line determination of 2-amino-4-chlorophenol (ACP) in chlorzoxazone tablets coupled with an optical fiber spectrophotometer. Several parameters affecting the adsorption/desorption, including sample pH value, sample flow rate, sampling time, eluent flow rate, and eluting time, were investigated in detail. Under the optimized conditions, limit of detection (LOD) and limit of quantification (LOQ) of the method were calculated to be 2.8 and 9.1 µg L(-1), respectively, with the relative standard deviation (RSD) of 3.1%.

Sorption of chlorophenols onto fruit cuticles and potato periderm.

To better understand the interaction mechanisms of plant surfaces with polar organic compounds, sorption of 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol by fruit cuticles (i.e., tomato, apple, and pepper), and potato tuber periderm were investigated. The roles of cuticular components (waxes, cutin, cutan and sugar) on sorption of chlorophenols are quantitatively compared. Cutin and waxes govern the sorption capacity of bulk apple cuticle by hydrophobic interactions. Potato periderm with highest sugar content exhibits the lowest sorption capability for the chlorophenols. With the increase of hydrophobicity (i.e., Kow ) of sorbate, the relative contribution of lipophilic components (wax, cutin and cutan) on total sorption increases, however, the ratios of Koc to Kow decreases due to increasing ionization degree of sorbates.

Isolation and identification of a novel chlorophenol from a cell suspension culture of Helichrysum aureonitens.

A novel chlorophenol, 4-chloro-2-(hepta-1,3,5-triyn-1-yl)-phenol (1), was isolated as the major phenolic compound from the cells of Helichrysum aureonitens suspension cultures. Compound 1 has been proposed to be an intermediate in the acetylene biosynthetic pathway of other acetylenic compounds in Helichrysum spp. The ethanol extract of cell suspension cultures and compound 1 were evaluated for their cytotoxicity against monkey kidney Vero (Vero cells) and human prostate epithelial carcinoma (DU145) cell lines, also, the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) against Mycobacterium tuberculosis H37Rv were determined as well.

Preparation of oil palm empty fruit bunch-based activated carbon for removal of 2,4,6-trichlorophenol: optimization using response surface methodology.

The effects of three preparation variables: CO(2) activation temperature, CO(2) activation time and KOH:char impregnation ratio (IR) on the 2,4,6-trichlorophenol (2,4,6-TCP) uptake and carbon yield of the activated carbon prepared from oil palm empty fruit bunch (EFB) were investigated. Based on the central composite design, two quadratic models were developed to correlate the three preparation variables to the two responses. The activated carbon preparation conditions were optimized using response surface methodology by maximizing both the 2,4,6-TCP uptake and activated carbon yield within the ranges studied. The optimum conditions for preparing activated carbon from EFB for adsorption of 2,4,6-TCP were found as follows: CO(2) activation temperature of 814 degrees C, CO(2) activation time of 1.9h and IR of 2.8, which resulted in 168.89 mg/g of 2,4,6-TCP uptake and 17.96% of activated carbon yield. The experimental results obtained agreed satisfactorily with the model predictions. The activated carbon prepared under optimum conditions was mesoporous with BET surface area of 1141 m(2)/g, total pore volume of 0.6 cm(3)/g and average pore diameter of 2.5 nm. The surface morphology and functional groups of the activated carbon were respectively determined from the scanning electron microscopy and Fourier transform infrared analysis.

Fixed-bed adsorption performance of oil palm shell-based activated carbon for removal of 2,4,6-trichlorophenol.

This study investigated the adsorption potential of oil palm shell-based activated carbon to remove 2,4,6-trichlorophenol from aqueous solution using fixed-bed adsorption column. The effects of 2,4,6-trichlorophenol inlet concentration, feed flow rate and activated carbon bed height on the breakthrough characteristics of the adsorption system were determined. The regeneration efficiency of the oil palm shell-based activated carbon was evaluated using ethanol desorption technique. Through ethanol desorption, 96.25% of the adsorption sites could be recovered from the regenerated activated carbon.

Adsorption isotherms, kinetics, thermodynamics and desorption studies of 2,4,6-trichlorophenol on oil palm empty fruit bunch-based activated carbon.

The adsorption characteristics of 2,4,6-trichlorophenol (TCP) on activated carbon prepared from oil palm empty fruit bunch (EFB) were evaluated. The effects of TCP initial concentration, agitation time, solution pH and temperature on TCP adsorption were investigated. TCP adsorption uptake was found to increase with increase in initial concentration, agitation time and solution temperature whereas adsorption of TCP was more favourable at acidic pH. The adsorption equilibrium data were best represented by the Freundlich and Redlich-Peterson isotherms. The adsorption kinetics was found to follow the pseudo-second-order kinetic model. The mechanism of the adsorption process was determined from the intraparticle diffusion model. Boyd plot revealed that the adsorption of TCP on the activated carbon was mainly governed by particle diffusion. Thermodynamic parameters such as standard enthalpy (DeltaH degrees ), standard entropy (DeltaS degrees ), standard free energy (DeltaG degrees ) and activation energy were determined. The regeneration efficiency of the spent activated carbon was high, with TCP desorption of 99.6%.

Adsorption of p-chlorophenol from aqueous solutions on bentonite and perlite.

The adsorption of p-chlorophenol (p-CP) from aqueous solutions on bentonite and perlite was studied. These materials are available in large quantities in Bulgaria. Model solutions of various concentrations (1-50 mgdm(-3)) were shaken with certain amounts of adsorbent to determine the adsorption capacity of p-CP on bentonite and perlite as well. The influence of several individual variables (initial adsorbate concentration, adsorbent mass) on the rate of uptake of the studied compound on the adsorbent was determined by carrying out experiments at different contact times using the batch adsorber vessel designed according to the standard tank configuration. Rapid adsorption was observed 20-30 min after the beginning for every experiment. After that, the concentration of p-CP in the liquid phase remained constant. The adsorption equilibrium of p-CP on bentonite and perlite was described by the Langmuir and the Freundlich models. A higher adsorption capacity was observed for bentonite (10.63 mgg(-1)) compared to that for perlite (5.84 mgg(-1)).