Liquid-liquid microextraction with hydrophobic deep eutectic solvent followed by magnetic phase separation for preconcentration of antibiotics.

This study describes a miniaturized approach for liquid-liquid microextraction based on mass transfer into low volume of deep eutectic solvent and magnetic phase separation, using specially produced magnetic chromium dioxide nanoparticles with a hydrophobic surface layer of fatty acids. The nanoparticles modified with fatty acid helped to recover low volumes of viscous hydrophobic deep eutectic solvent-based extract reproducibly and easily (up to 10 µL) in a microextraction procedure with the application of magnetic forces. It was demonstrated that the collector properties depend on nanoparticles' surface and magnetic characteristics. The developed approach was implemented for the separation and preconcentration of trace fluoroquinolone antibiotics from environmental waters prior to their determination by high-performance liquid chromatography with fluorometric detection as a model analytical task. The limits of detection, calculated from a blank test based on 3σ, were 0.01 µg L-1 for ofloxacin, 0.02 µg L-1 for lomefloxacin and fleroxacin, and 0.04 µg L-1 for norfloxacin. The procedure provides significant solvent reduction and high enrichment factors. The approach is green, which is proved by the analytical eco-scale assessment tool with the total score equal to 85 out of 100.

The strategy for organic dye and antibiotic photocatalytic removal for water remediation in an example of Co-SnO2 nanoparticles.

A challenging problem to create an efficient photocatalyst suitable for industrial water remediation, aiming to remove cyclic organic compounds attracts increasing attention. The current study aimed to clarify a few "dark spots" in the field, namely to find out if it is possible to make an efficient photocatalyst activated with visible light by using a simple and cheap strategy and what are the key factor impacting its efficiency. In this work, a new procedure to obtain spherical nanoparticles with the same average size but different amounts of oxygen vacancies and defects and dopant concentrations was developed. The approach based on hydrothermal treatment was suggested to obtain rod-shaped nanoparticles. The systematic study of photocatalytic behavior on the example of oxytetracycline and methylene blue degradation under visible light of widely available LED lamp was performed. Based on chemical and computational experiments the main factor affecting the process efficiency was determined.

A synergistic effect of hydrophobic deep eutectic solvents based on terpenoids and carboxylic acids for tetracycline microextraction.

Hydrophobic deep eutectic solvents were investigated for tetracycline microextraction. It was found that a deep eutectic solvent consisting of thymol and octanoic acid provided a synergistic effect on tetracycline extraction. In this paper, a novel liquid-liquid microextraction procedure for the HPLC-DAD determination of tetracyclines in milk samples was proposed.

Effect of surfactant coating of Fe3O4 nanoparticles on magnetic dispersive micro-solid phase extraction of tetracyclines from human serum.

A procedure for separation and preconcentration of tetracyclines from human serum samples involving magnetic dispersive micro-solid phase extraction was proposed. The extraction efficiency of different tetracyclines was improved with the use of the surfactant coated Fe3O4 magnetic nanoparticles. Sorption mechanism was presented, and the potential use of magnetic Fe3O4 nanoparticles coated with different surfactants for tetracyclines adsorption was demonstrated for the first time. The procedure involved nanoparticle floating in a liquid sample phase for analyte extraction followed by elution and determination by high performance liquid chromatography with diode array detection. Influence of the main involved parameters was studied, the system was dimensioned accordingly. The analytical curves were linear in the ranges of 0.25-10 mg L-1 for tetracycline and 0.10-10 mg L-1 for oxytetracycline or doxycycline. Limits of detection were estimated (IUPAC, 3 concept) as 0.08 mg L-1 for tetracycline, and 0.03 mg L-1 for oxytetracycline or doxycycline. The proposed procedure proved to be fast (10 min), simple (two stages), inexpensive (10 mg of nanoparticles) and was applied to human serum samples. Unlike previously synthesized nanoparticles for tetracyclines separation, the surfactant-coated Fe3O4 nanoparticles can be easily prepared with widely available and low-cost reagents. Moreover, elution of the analytes was accomplished in absence of organic solvents by an aqueous chelating agent solution.

Homogeneous liquid-liquid microextraction based on primary amine phase separation: A novel approach for sample pretreatment.

A homogeneous liquid-liquid microextraction procedure based on primary amine phase separation was developed as a novel approach for the pretreatment of biological fluids. The procedure assumes primary amine dissolution in the aqueous sample phase, resulting in the creation of a homogeneous sample solution followed by phase separation and analyte extraction in the presence of a polar, water-miscible organic solvent. The phenomenon of primary amine phase separation from homogeneous aqueous solution in the presence of a polar, water-miscible organic solvent was studied in detail and applied for separation and preconcentration in chemical analysis for the first time. The suggested approach was used for the HPLC-UV determination of meropenem as a proof-of-concept analyte in human plasma and serum samples. Under optimal conditions, the detector response of meropenem was linear in the concentration range of 0.1-100.0 mg L-1. The limit of detection was calculated from a blank test based on 3σ, was 0.03 mg L-1.

An automated salting-out assisted liquid-liquid microextraction approach using 1-octylamine: On-line separation of tetracycline in urine samples followed by HPLC-UV determination.

An automated salting-out assisted liquid-liquid microextraction (SALLME) procedure based on a flow system was developed as new approach for pretreatment of complex sample matrix. In this procedure 1-octylamine was investigated as novel extractant for the SALLME. The procedure involved aspiration of the 1-octylamine and sample solution into a mixing chamber of a flow system followed by their air-bubble mixing resulting to isotropic solution formation. To provide phase separation a salting-out agent solution was added into the mixing chamber. After phase separation, the micellar 1-octylamine phase containing analyte was mixed with methanol and transported to a HPLC-UV system. To demonstrate the efficiency of the suggested approach, the automated procedure was applied for the HPLC-UV determination of tetracycline as a proof-of-concept analyte in human urine samples. Under the optimal conditions, the detector response of the analytes was linear in the concentration ranges of 0.5-20 mg L-1. The limit of detection, calculated from a blank test based on 3σ, was 0.17 mg L-1. The results demonstrate that the developed approach is highly cost-effective, simple and rapid.