•A multi-class multi-residue analytical method for veterinary drugs was developed.•A total of 132 veterinary drugs from almost 15 classes were investigated.•A magnetic hypercrosslinked ...polystyrene-based MSPE was developed.•The methodology was applied to the trace drug analysis of milk.
A quantitative multi-class multi-residue analytical method was developed for the determination of veterinary drugs in milk by high-performance liquid chromatography – tandem mass spectrometry (HPLC-MS/MS). A total of 132 veterinary drugs investigated belonged to almost 15 classes including sulfonamides, β-lactams, tetracyclines, quinolones, macrolides, nitrofurans, nitroimidazoles, phenicols, lincosamides, pleuromutilins, macrocyclic lactones, quinoxaline antibiotics, benzimidazoles, anthelmintics, coccidiostats and some others. A magnetic solid-phase extraction procedure was developed using magnetic hypercrosslinked polystyrene (HCP/Fe3O4) for the sample preparation prior to HPLC-MS/MS without deproteinization step. The results indicated recoveries of 85–107% for 14 sulfonamides, 85–120% for 13 β-lactams, 89–115% for 4 tetracyclines, 82–119% for 14 quinolones, 82–115% for 8 macrolides, 97–109% for 4 nitrofurans, 84–115% for 10 nitroimidazoles, 89–114% for 3 phenicols, 86–111% for 3 lincosamides, 97–102% for 2 pleuromutilins, 72–88% for 4 macrocyclic lactones, 87–104% for 4 quinoxaline antibiotics, 76–119% for 21 benzimidazoles, 79–115% for 12 anthelmintics, 81–118% for 12 coccidiostats and 75–119 % for 5 unclassified drugs, with relative standard deviations (RSDs) of less than 20%, and the LOQs ranged from 0.05 to 1 μg kg−1. This methodology was then applied to field-collected real milk samples and trace levels of some veterinary drugs were detected.
In this study, aqueous two-phase systems (ATPSs) containing a cationic and anionic surfactants mixture were used for the preconcentration of the synthetic food dyes Allura Red AC, Azorubine, Sunset ...Yellow, Tartrazine, and Fast Green FCF. A rapid, simple, low cost, affordable, and environmentally friendly methodology based on microextraction in ATPSs, followed by spectrophotometric/colorimetric determination of the dyes, is proposed. The ATPSs are formed in mixtures of benzethonium chloride (BztCl) and sodium N-lauroylsarcosinate (NaLS) or sodium dihexylsulfosuccinate (NaDHSS) under the molar ratio close to equimolar at the total surfactant concentration of 0.01-0.20 M. The density, viscosity, polarity, and water content in the surfactant-rich phases at an equimolar ratio BztCl:NaA were determined. The effects of pH, total surfactant concentration, dye concentration, and time of extraction/centrifugation were investigated, and the optimum conditions for the quantitative extraction of dyes were established. The smartphone-based colorimetric determination was employed directly in the extract without separating the aqueous phase. The analytical performance (calibration linearity, precision, limits of detection and quantification, reproducibility, and preconcentration factor) and comparison of the spectrophotometric and smartphone-based colorimetric determination of dyes were evaluated. The method was applied to the determination of dyes in food samples and food-processing industrial wastewater.
Dispersive liquid–liquid microextraction (DLLME) is one of the most promising methods of the microextraction preconcentration of organic compounds. This method is eco-friendly, simple, and universal; ...in comparison with conventional extraction, the consumption of the reagents and solvents, the time of extraction, and the cost of analysis in this method are reduced. For a short time from the moment of the appearance of DLLME in 2006, analysts developed numerous versions, differing by the method of dispersion, the nature of the extractant and by combinations with other methods of sample preparation and methods of the subsequent determination of the preconcentrated substances. The popularity of the method among the analysts is attested in a great number of reviews summarized in this publication.
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•An overview on recent trends in the sample preparation and determination of sulfonamides is given.•A comparison of different methods of real samples preparation is made.•The general ...chromatographic and other methods of SAs determination are discussed.•Examples of SAs determination in different matrices are given.
Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid–liquid and solid-phase extraction, dispersive liquid–liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed.
An aqueous two-phase system (ATPS) based on benzethonium chloride (BztCl) and sodium dihexyl sulfosuccinate (NaDHSS) was proposed for the first time for liquid-liquid microextraction of Cd(II), ...Co(II), Cu(II), Mn(II), Ni(II), and Pb(II) followed by ICP-OES determination. The mixture of cationic and anionic surfactants, BztCl and NaDHSS, showed liquid-liquid phase separation at the molar ratio of 1:1, and the total surfactant concentration of 0.01-0.2 mol L
forming ATPS that was investigated in the extraction process. The extraction efficiency for Cd(II), Co(II), Mn(II), Ni(II), and Pb(II) was nearly 100 %, and for Cu(II) - not lower than 88 % in the presence of 8-hydroxyquinoline as a complexing agent. The surfactant-rich phase containing analytes was subjected to back-extraction with 0.2 M HNO
before ICP-OES measurements. The preconcentration in the proposed BztCl-NaDHSS-H
O ATPS for 30 s and the high degree of back-extraction, which was achieved in 1 min, significantly reduced the sample preparation time, matrix effects and provided low LODs in the range of 0.04-1.0 μg L
, the preconcentration factor was 120. The analysis of a certified reference material sample of surface water and the real samples of tap, sea, and waste water verified the method accuracy.
A rapid multi-residue LC-MS/MS method for the identification and determination of banned veterinary drugs in honey was developed. A total of 31 investigated veterinary drugs belonging to 4 classes ...including nitrofurans metabolites, nitroimidazoles, amphenicols, and quinolones were quantified by LC-MS/MS with ESI using one single injection. The sample preparation included treatment with 5-nitro-2-furaldehyde (5-NFA) in a thermostated ultrasonic bath (80 °C, 0.5М НСl, 20 min) to liberate matrix-bound residues of nitrofurans. Magnetic hypercrosslinked polystyrene (HCP/Fe3O4) was proposed for the solid-phase extraction and clean-up of target analytes prior to LC-MS/MS analysis. To evaluate and validate the performance of method, the criteria of the Decision (EC) no 2002/657 were applied. The LOQs of the examined analytes range from 0.3 to 1 μg kg-1, which indicates good sensitivity to quantify the target compounds in honey. The recoveries of veterinary drugs from 1 g of honey with 50 mg of the sorbent are 97-109% for nitrofuran metabolites, 84-115% for nitroimidazoles, 86-103% for amphenicols, and 97-118% for quinolones. The relative standard deviations of intra-day and inter-day precision analyses (RSD) are less than 16%. This methodology was applied to real honey samples and trace levels of some veterinary drugs were detected.
Single-drop microextraction (SDME) and hollow-fiber membrane microextraction (HFME) belong to methods of the liquid-phase microextraction preconcentration of organic compounds. These methods are ...characterized by the low consumption of organic solvents, high preconcentration factors, simplicity, low cost, ease of combination with various chromatographic methods; processes of preconcentration and sample injection are combined in a single device. Since the emergence of SDME (1996) and HFME (1999), a large number of versions have been developed that differ in the preconcentration technique, nature of the extractants used, and combinations with methods for the subsequent determination of the preconcentrated substances. The popularity of these methods among the analysts is evidenced by many reviews that we have summarized in this publication.
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•Formation of silver nanoparticles by flavonoid reduction was studied.•A role of different type flavonoids during AgNPs green synthesis was revealed.•Effects of a flavonoid nature and ...concentration, and other factors were studied.•A method for the spectrophotometric determination of flavonoids has been developed.•The method was applied for the analysis of biologically active food additives.
Formation of plasmonic silver nanoparticles by flavonoid reduction was studied. Effects of the nature and the concentration of a flavonoid and a stabilizer, composition of the solution and the interaction time were revealed. It was found that quercetin, dihydroquercetin, rutin and morin produced an intense surface plasmon resonance band of silver nanoparticles at 415nm which was linearly related to the concentration of a flavonoid, while chrysin, naringenin and naringin did not produce any remarkable changes. It was used for the spectrophotometric determination of the former four flavonoids with the detection limits of 0.03; 0.06; 0.09 and 0.1μgmL−1, respectively. The developed method was applied for the determination of flavonoids in biologically active food additives.
One of the possible ways for using silver nanoparticles (AgNPs) in spectrophotometry is their application for the determination of oxidizing agents, based on oxidative destruction of these ...nanoobjects. This process depends on the structure of AgNPs surface layer, which is essentially affected by the chosen stabilizer. To assess influence of the nanoparticle stabilizer and the nature of the analyte, possibilities of AgNPs covered with stabilizers of three types (citrate, polyvinylpyrrolidone, and polyhexamethylene guanidinium) for the spectrophotometric determination of hydrogen peroxide and differently substituted organic peroxides were studied. The approach is based on AgNPs oxidation leading to discoloration of the solution monitored spectrophotometrically. Different selectivity of the oxidation depending on the stabilizer was shown. Effects of various factors (time of interaction, pH, concentration of AgNPs) on the oxidation and analytical performance of the procedure were investigated. The method allows for the determination of hydrogen peroxide, peracetic acid, m-chloroperbenzoic acid, and t-butylhydroperoxide in the range of 0.3–1.5, 0.1–0.8, 1.0–7.5, and 1–7 μg mL−1 and with the limits of detection of 0.1, 0.04, 0.3, and 0.3 μg mL−1, respectively. The analysis can be performed using either spectrophotometry or naked-eye detection.
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•Oxidation of AgNPs covered with stabilizers of three types by peroxides were studied.•The type of an AgNPs stabilizer plays an important role in their oxidation.•Hydrogen peroxide and differently substituted organic peroxides are considered.•Best strategies for the determination of peroxides using AgNPs are proposed.
•Current trends in LC-MS/MS determination of NF metabolites in food are considered.•Main approaches to sample preparation of food are discussed.•Multi-class, multi-residue methods for NF metabolites ...determination are considered.•Future trends in food analysis during NF metabolites determination are outlined.
Nitrofurans (NFs) are synthetic broad-spectrum antibacterial and antiparasitic drugs, which recently were extensively used in veterinary practice. In the body of animals, NFs are converted into carcinogenic and mutagenic metabolites that can be accumulated in foods of animal origin having an adverse effect on human health. Therefore, NFs are currently banned in animal husbandry and aquaculture of many countries. However, the data from monitoring the quality of food products indicate that, despite the prohibitions established by the law, they still are used not only in the developing countries but also in the European Union, due to their high antibacterial activity, low cost, and accessibility. Thus, it is of great importance for human health to develop reliable and sensitive analytical methods for monitoring NF metabolites in animal-derived foods. The objective of this review is to summarize the pretreatment strategies and chromatographic methods that have been reported during the last decade for the determination of NF metabolites in food samples, and to outline the future trends with an emphasis on the novel solutions in this area.
