Biogenic amines (BAs) can be found in various foods, such as cheese, wine, and chocolate. The consumption of a sufficient quantity of BA can lead to symptoms including headaches, hypertonia, and diarrhea. For this reason, the amount of BA in food is regulated in many countries. A new method for the determination of biogenic amines in wine has been proposed, which involves derivatizing BA with p-toluene sulfonyl chloride (TsCl) and using K2S2O8 to reduce the matrix effect. The derivatives of putrescine, cadaverine, histamine, and tyramine with TsCl were synthesized and characterized by 1H NMR spectroscopy. Separation of BA derivatives was performed using a reversed-phase high-performance liquid chromatography (RP-HPLC). The chromatographic system was equipped with a reversed-phase C8 column and a diode array detector. This method was validated to analyze the above-mentioned biogenic amines simultaneously in red and white wine samples. The detection limits for putrescine, cadaverine, histamine, and tyramine in wine samples were 0.0248 mg·L−1, 0.0645 mg·L−1, 0.346 mg·L−1 and 0.00866 mg·L−1, respectively. The calibration curves showed good linearity (r > 0.999), and biogenic amines recovery varied from 83.0 to 110%. The proposed method demonstrates high sensitivity, straightforward sample preparation, and rapid analysis time.
Objectives. To develop a method for the determination of hypochlorite, chloride, chlorite, chlorate, and perchlorate ions in solution; to determine the limits of detection and quantitation for ClO−, Cl−, ClO2−, ClO3−, and ClO4− ions; to evaluate the applicability of the developed method and its suitability for disinfectant analysis.Methods. Ionic chromatography using a conductometric detection system in isocratic elution mode.Results. The method developed for chromatographic determination of chlorine-containing ions can be used to quantify the content of hypochlorite, chloride, chlorite, chlorate, and perchlorate ions. In isocratic elution mode at 7.5 mM NaOH and a flow rate of 0.4 mL/min, the content of chlorine-containing ions can be determined with high sensitivity. The presented method does not require the use of expensive equipment for the ultrasensitive analysis of the studied compounds.Conclusions. A novel method for the simultaneous determination of hypochlorite, chloride, chlorite, chlorate, and perchlorate ions in case of their combined presence is proposed. The technique can be used to carry out routine control of the content of these disinfectant components during use, increasing their effectiveness at the same time as managing associated toxicological risks.
16 November 2025 in Materials Chemistry and Physics
Solid paraffin briquettes are one of the most modern types of rodenticide baits, because they protect it from the environmental exposure and do not reduce palatability of rodents. This paper proposes a simple universal method for the determination of brodifacoum, bromadiolone and difenacoum in solid briquettes, which are a mixture of paraffin, poison and filler, which can be used as grain, flour and the like. The difficulty in the analysis of baits containing paraffin, is to get rid of it. For this, we propose to use hexane-acetonitrile extraction in the system. Paraffin dissolves in hexane, while brodifacoum, bromadiolone and difenacoum do not. The resulting two-phase system was separated using a separatory funnel and the bottom fraction was collected. If any fillers were present in the sample, they were filtered until the mixture was separated, the residue was washed with acetonitrile. Before introducing the sample into the chromatograph, it was filtered twice with PTFE filters with a porosity of 0.45 µm. The best separation was achieved using a Thermo Acclaim® Surfactant column using acetonitrile and 0.1 M aqueous ammonium acetate solution (pH 5.4) as the mobile phase in a gradient elution mode. All three poisons were detected at a wavelength of 264 nm. This method has a sensitivity of 0.028 mg. The linearity range is from 0.00067 to 0.01%. The recovery rate for bromadiolone is 94%, for brodifacoum, 98%, and for difenacoum, 90%.