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1.
J Chromatogr A ; 1636: 461756, 2021 Jan 11.
Article in English | MEDLINE | ID: mdl-33333374

ABSTRACT

A miscible-immiscible deep eutectic solvent (DES) containing monoethanolamine/4-methoxyphenol was used as an extraction solvent in a homogeneous liquid-liquid microextraction (HLLME). The method was used to preconcentrate chlorobenzenes in water samples followed by separating and analyzing them by gas chromatography-mass spectroscopy (GC-MS). A special feature of the new extraction method is that a green miscible solvent was used as an extractant in the HLLME method. The developed extraction technique provided enrichment factors in the range of 13.1-42.1 for extraction from only 1.0 mL of the aqueous sample solution. The effects of various experimental parameters were investigated and optimized. The optimal conditions were as follows: vortex time: 30.0 s, bubbling CO2 gas: 1.0 min, salt concentration: 5.0% w/v, rate and time of centrifuge: 4000.0 rpm and 3.0 min, respectively, and DES volume: 30.0 µL. The limit of detections and the limit of quantifications for the four targeted analytes varied from 0.01-0.15 and 0.025-0.5 µg L-1, respectively. The precision and long-term precision tests for the developed method were found to be less than 11.0%. Two real samples, including toilet air freshener and car perfume, were analyzed. The applied DES in the HLLME method provides a fast means of sample preparation for environmental aqueous sample solutions.


Subject(s)
Carbon Dioxide/chemistry , Chlorobenzenes/chemistry , Liquid Phase Microextraction/methods , Solvents/chemistry , Chlorobenzenes/analysis , Chlorobenzenes/isolation & purification , Gas Chromatography-Mass Spectrometry , Limit of Detection , Perfume/chemistry
2.
Mikrochim Acta ; 186(7): 459, 2019 06 20.
Article in English | MEDLINE | ID: mdl-31222415

ABSTRACT

Nanosheets prepared from magnesium oxide, chitosan and graphene oxide (MgO/Chit/GO) were hydrothermally synthesized and used as a sorbent for removal of ciprofloxacin and norfloxacin from aqueous solutions. Residual antibiotics in sample were determined by HPLC/UV instrument. The sorbent was characterized by FTIR, XRD, BET, SEM, and TEM. Its high adsorption capacity is attributed to the high surface area (294 m2.g-1) as compared to bare MgO/chit or bare GO. The pore size of the mesoporous sorbent typically is 15 Å. The adsorption isotherms for the two model antibiotics studied (norfloxacin, ciprofloxacin) can be described with the Langmuir model, and the maximum adsorption capacities are 1111 and 1000 mg.g-1 for ciprofloxacin and norfloxacin, respectively. The analysis of the kinetic data revealed that the synthesized sorbent followed pseudo-second-order kinetics and the maximum equilibrium was at over 120 and 150 min for ciprofloxacin and norfloxacin, respectively. Therefore, it is introduced as an economical, eco- friendly, and high-performance sorbent for removal of antibiotics from aqueous solutions. Graphical abstract Schematic presentation of dispersion of magnesium oxide/chitosan/graphene oxide (MgO/chit/GO) nanosheets in waste water for removal of ciprofloxacin and norfloxacin as water pollutants.


Subject(s)
Anti-Bacterial Agents/isolation & purification , Chitosan/chemistry , Ciprofloxacin/isolation & purification , Norfloxacin/isolation & purification , Solid Phase Extraction/methods , Water Pollutants, Chemical/isolation & purification , Adsorption , Graphite/chemistry , Green Chemistry Technology/methods , Hydrogen-Ion Concentration , Magnesium Oxide/chemistry , Solid Phase Extraction/instrumentation , Water/chemistry
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