Vol 73, No 6 (2018)

A review of methods for the assessment of the fractional distribution of organic substances in natural waters is presented. The problem is usually solved by combining methods of separation into fractions with those of the quantitative determination of substances in the fractions obtained. There is also an original approach based on a combination of methods of membrane filtration and oxythermography; an example of using this approach is presented.

Thermal lens spectrometry was used to study Langmuir–Blodgett films of a weakly absorbing Nafion polyelectrolyte membrane on the surface of inert polyethylene terephthalate (PET) and glass substrates and to estimate the amount of Nafion (number of layers) using a change in the thermal characteristics of the sample. The sensitivity of thermal lens measurements at the wavelength of the exciting radiation 532.0 nm is comparable to that of solid-state spectrophotometry in the region of the maximum absorbance of Nafion (275 nm). However, the high locality of thermal lens spectrometry (the area of the signal generation zone is 100 μm²) ensures the estimation of the uniformity of the deposition of the polyelectrolyte layer. To increase the absorbance of the layer of the applied polyelectrolyte, the latter is saturated with a colored compound (ferroin). The adsorption of ferroin into the Nafion layer on the PET surface was confirmed; the absorbance of ferroin in the Nafion layer is in the range of 1 × 10–5^–5 × 10^–4 units of absorbance, which corresponds to the surface concentration of ferroin 1 × 10^–11–4 × 10^–10 mol/cm².

Compositions of rare mineral phases containing precious metals (PMs) in samples from Natalka, Pavlik, Vetrenskoe, and Degdekan gold ore deposits (North-East of Russia) are studied by scintillation atomic emission spectrometry (SAES) and electron probe microanalysis (scanning electron microscopy and electron probe X-ray microanalysis, SEM–EPMA). The SAES method found dozens and hundreds of particles carrying gold, silver, and all platinum-group elements as native metals, intermetallides and solid solutions, arsenides, antimonites, sulfoarsenides, tellurides, selenides, etc. The variety of the elemental compositions of PM species (mineral phases) found by SAES significantly exceeds the list of minerals found previously by SEM–EPMA because of different natures of optical and X-ray spectra. The sizes of PM particles calculated by the SAES method and measured by SEM–EPMA are similar. The SAES data on the total concentrations of PMs satisfactorily agree with the results of inductively coupled plasma mass spectrometry.

The fixed dose combination of azilsartan medoxomil potassium and chlorthalidone has been introduced for the effective treatment of hypertension. In the present work a rapid, simple and accurate stability indicating ultra HPLC assay method has been developed. The separation of azilsartan medoxomil, chlorthalidone and their degradation products were accomplished on an Acquity UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) column using mobile phase combination of 0.02% trifluoroacetic acid in water and acetonitrile in gradient mode. The forced degradation products were identified using liquid chromatography‒electrospray ionisation-quadrupole time of flight-tandem mass spectrometry (LC‒ESIQTOF–MS/MS) and accurate mass experiments. The in silico toxicities of the degradation products for both the drugs were evaluated. The proposed method was validated as per the ICH Q2 (R1) guideline for selectivity, linearity, precision, accuracy and robustness.

A rapid screening and determination of 150 veterinary drugs of various classes in milk by UHPLC–high-resolution quadrupole time-of-flight mass spectrometry is proposed. One gram of milk was used for the analysis; the precipitation of proteins and extraction were performed with acetonitrile; the extract was analyzed without purification or preconcentration. Veterinary drugs were identified by accurate masses of analyte ions produced by electrospray ionization, their retention time, and the pattern of ion isotope distribution (mSigma). The quantitative analysis of the detected analytes was carried out by the standard addition method. The limits of detection were 0.1–0.5 ng/g; the analytical ranges were (0.1)1–500 ng/g; the duration of screening was 20–30 min; and the analysis time was 30–40 min. The relative standard deviation of the results for all analytes did not exceed 15%.

This paper reports the use of multiple square wave voltammetry (MSWV) in the development of a simple, sensitive, fast and low-cost electroanalytical procedure for the diquat herbicide detection in different samples employing a custom-made gold microelectrode (Au-ME). The experimental and voltammetric parameters were optimized, and the use of eight pulses superimposed in each step in the MSWV yielded the detection limits two orders of magnitude greater than those obtained by SWV or previously published chromatographic procedures. Also, the Au-ME allied to MSWV was used to determine diquat in beetroot, onion, peach, environmental water and river sediments. All samples were spiked, and the obtained recovery percentage values were satisfactory for the analytical procedure, showing that Au-ME and MSWV is a suitable tool for diquat residues detection in complex samples.

The uncertainty of measurement for well-known neurotransmitters like serotonin, noradrenalin and gamma-aminobutyric acid (GABA), glutamate and melatonin hormone with high performance liquid chromatography−fluorescence detection was calculated after the method validation. Two methods were developed for the determination of the neurotransmitters. A derivatization step was performed for the determination of GABA and glutamate. Sensitivity, method detection limit, limit of quantification, linearity, recovery, interday and intraday precision values were calculated. Low detection limit values were obtained especially for the determination of GABA and glutamate. Then, bottom-up approach was used to calculate measurement uncertainty. The critical stages of the method were evaluated. The major sources of the uncertainty budget were calibration curves, stock solution and recovery. The calculated percentage relative uncertainty values for the compounds changed between 10.1 and 16.7.

In Figure 4: should read “Nitric acid (0.1 M)” instead of “Nutric acid (0.1 M)”

Figure 6 should be: