Layered double hydroxide nanoparticles for a smartphone digital image colorimetry-based determination of fluoride ions in water, milk and dental products.

A novel smartphone digital image colorimetry-based approach was developed for fluoride ion determination, using layered double hydroxide (LDH) nanoparticles (Mg2Al(OH)7) as sorbents for analyte preconcentration and as a source of a central metal ion for a colored complex formation. A cotton rotating disk provided effective retention of the LDH nanoparticles during solid-phase microextraction and elution, excluding time-consuming centrifugation process. In the proposed procedure, the nanoparticles acted as aluminum ion source for alizarin complexone-Al3+-F- complex formation. An image of Eppendorf tube, containing the colored complex solution was obtained by a smartphone and converted, using the RGB model for fluoride ion determination. The procedure had a linear range of 0.20-20 mg L-1 with a limit of detection of 0.06 mg L-1. The developed procedure provided effective fluoride separation from various matrices for its determination by a smartphone without additional sample pretreatment.

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.

Flow method based on liquid-liquid extraction using deep eutectic solvent for the spectrofluorimetric determination of procainamide in human saliva.

In the current study, liquid-liquid extraction, using deep eutectic solvent (DES) as a "green" extraction solvent, was coupled with a stepwise injection system for the first time. The suggested approach was applied for the development of spectrofluorimetric method for procainamide determination. The method is based on aspiration of saliva sample and DES (choline chloride with glycerol at a 1:2M ratio) solution into the mixing chamber of a flow system, followed by injection of acetonitrile into the mixed DES-sample solution. The extraction process and final phase separation were then promoted by air-bubbling. After phase separation, the DES phase, containing the extracted procainamide, was transported to a spectrofluorimetric detector. The excitation and emission wavelengths were set at 280nm and 347nm, respectively. The calibration plot was linear in the range of 5×10-6 to 5×10-5molL-1. The limit of detection, calculated as 3σ of a blank test (n=10), was found to be 1.5×10-6molL-1. The developed method was successfully applied for the determination of procainamide in human saliva samples, and the analytical results agreed rather well with the results obtained by the reference HPLC-UV method.

Automated sugaring-out liquid-liquid extraction based on flow system coupled with HPLC-UV for the determination of procainamide in urine.

A fully automated sugaring-out assisted liquid-liquid extraction procedure was suggested. The procedure was based on the separation of the acetonitrile phase, containing a target analyte from the homogeneous sample solution after injection of sugaring-out reagent (glucose) into a mixing chamber of the flow system. Air bubbling was used to promote the extraction process and phase separation. After the fast phase separation in the mixing chamber, the acetonitrile phase containing the target analyte was transferred to an HPLC-UV system. Under the optimal conditions, the detector response of procainamide was linear in the concentration range of 6×10-7-4×10-5molL-1. The limit of detection, calculated from a blank test based on 3σ, was 2×10-7molL-1. The proposed method was successfully applied for the determination of procainamide in human urine samples and the analytical results agreed fairly well with the results obtained by reference CE method.