In the present paper, for the first time, the electrochemical behaviour of nicotine metabolite nicotine N-oxide (NNO) on static mercury dropping electrode (SMDE) and mercury meniscus modified silver solid amalgam electrode (m-AgSAE) has been reported. Nicotine N-oxide is reduced forming one peak at the potential -0.78 V on SDME and -0.86 V on m-AgSAE in Britton-Robinson buffer medium at pH 4.5 using cyclic voltammetry (CV). One electron and one proton take part in the reaction of NNO reduction. Calibration graphs for NNO determination using linear sweep voltammetry (LSV) on SDME and square-wave voltammetry (SWV) and differential pulse voltammetry (DPV) on m-AgSAE were obtained. Limit of detection (LOD) is 0.13 μM on SDME, and 0.16 μM (SWV) and 0.29 μM (DPV) on m-AgSAE. Since NNO can be used as an analytical form for nicotine voltammetric determination, so the developed methods were applied for the analysis of pharmaceutical preparations, and the recoveries from 97.3 to 104.6 % were achieved. Also, the elaborated methods were used in the analysis of biological fluids, and tobacco products. The obtained results were compared to those indicated in the certificates of drugs analysis, and to the results, obtained by reference methods (HPLC and GC).
Due to the unexpected detection of chloramphenicol isomer residues in honey, we have studied the hypothesis of unauthorized or unintended use of unregistered veterinary drug preparations. First, we have investigated honey samples in which a discrepancy was observed between the results of the immunological screening methods and the confirmatory liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. In all samples, previously identified to be contaminated with the banned antibiotic chloramphenicol according to LC-MS/MS only, the presence of dextramycin (SS-para isomer of chloramphenicol) was detected by chiral LC-MS/MS. The source of dextramycin in honey was investigated by studying the preparations utilized in apiaries from which the above non-compliant honey samples have been received. In all these preparations (beehive strips applied against the mite Varroa destructor) chloramphenicol was detected in the concentrations ranging from 33 to 34,400 μg kg . Chiral LC-MS/MS demonstrated the presence of chloramphenicol and dextramycin in different ratios, and it was concluded that these preparations can be the source of chloramphenicol and dextramycin residues in honey. These preparations were of foreign production and are not officially registered in accordance with current legislation.
This manuscript presents the results of development and adoption of the confirmatory UPLC- MS/MS method for determination of sulfonamides and trimethoprim residues in whole and powdered cow's milk samples. Sample preparation includes a recovery with water (in the case of milk powder), separation of milk fat by centrifugation at 4 °C, proteins precipitation with acetonitrile using ultrasonic intensification, extraction of analytes with a two-component mixture of organic solvents from weak acidic phosphate buffer solution, concentration of obtained extracts, degreasing and reconstitution with the mobile phase. The use of tandem-mass spectrometric detector in multiple reaction monitoring mode provides high specificity for all ten sulfonamides, which molecules contain the same structural elements, and trimethoprim, as three ion transitions were used for each of the target analytes. The approach of matrix matched calibration on the milk matrix was applied, and it allowed us to disregard taking into consideration the absolute extraction of analytes during sample preparation, as well as the influence of sample matrix components on analytes ionization. The main advantages of the developed technique are simplicity, rapidity and cost effective sample preparation, fast procedure of sample analysis (the time of chromatographic separation is 2.0 min), high selectivity, and sensitivity at the level of ≤ 0.5 μg/kg (as compared with the maximum residues level of sulfonamides in dairy products, viz. 100 μg/kg). According to the European Commission Decision 2002/657/EC, the values of CCα and CCβ for sulfonamides and trimethoprim in milk were calculated. The capability of the method was confirmed on the basis of the established validation parameters, using spiked milk samples and "added – found" approach. The method was tested during the analysis of spiked samples of whole and powdered cow's milk (CV ~ 20%). The developed technique was verified by interlaboratory comparative testing of milk powder samples for sulfonamides content. The UPLC-MS/MS method for the determination of sulfonamides and trimethoprim residues in whole and milk powder samples can be used both for routine laboratory analysis of dairy products and for the examination of suspicious or questionable samples.
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