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Ultra performance liquid chromatography-tandem mass spectrometry for the determination of 5-nitroimidazoles and their metabolites in egg

100%
Tamošiūnas V., Padarauskas A.
Open Chemistry
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2009
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vol. 7
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issue 3
267-273
EN
An ultra performance liquid chromatography (UPLC) coupled to tandem mass spectrometry (MS/MS) procedure was developed for the determination of five 5-nitroimidazoles (dimetridazole, ipronidazole, metronidazole, ronidazole and ternidazole) and three of their metabolites (1-methyl-2-hydroxymethyl-5-nitroimidazole, 1-(2-hydroxyethyl)-2-hydroxymethyl-5-nitroimidazole and 1-methyl-2-(2′-hydroxyisopropyl)-5-nitroimidazole) in egg matrices. Conditions for UPLC separation and electrospray ionization MS/MS in the positive ion mode were optimized. Samples were prepared by liquid-liquid extraction with buffered aqueous 2.5% trichloroacetic acid followed by solid-phase extraction on a Strata-X-C cartridge with reversed-phase and cation-exchange functionalities. The method’s performance was evaluated in accordance with Commission Decision 2002/657/EC, applying the alternative matrix-comprehensive in-house validation approach using specially designed InterVal software. The method was robust against different sample matrix and SPE cartridges, operator change, and changes in sample extract storage. Acceptable apparent recoveries (76 to 109%) were obtained for all analytes. The decision limits (CCα) and detection capabilities (CCα) were within the ranges of 0.19–2.62 and 0.26–4.29 μg kg−1. For all compounds the calibration curve linearity was good with correlation coefficients greater than 0.99. Fifteen eggs and ten whole egg powder samples obtained commercially in Lithuania were analyzed by UPLC-MS/MS; none were found contaminated by 5-nitroimidazoles or their metabolites.
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Ionic liquids in microextraction techniques

100%
Vičkačkaitė V., Padarauskas A.
Open Chemistry
|
2012
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vol. 10
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issue 3
652-674
EN
The tremendous potential of room temperature ionic liquids as an alternative to environmentally harmful ordinary organic solvents is well recognized. Due to their unique properties, such as low volatility, tunable viscosity and miscibility, and electrolytic conductivity, ionic liquids have attracted extensive attention and gained popularity in many areas of analytical chemistry including modern sample preparation techniques. In this review the advantages and limitations of application of ionic liquids as solvents/sorbents for microextraction are critically discussed. Topics covered include solid-phase microextraction, single drop microextraction, dispersive liquid-liquid microextraction and hollow-fiber liquid-phase microextraction. The compatibility of the ionic liquid-based microextraction with different analytical techniques such as gas chromatography, high-performance liquid chromatography, electrothermal or flame atomic absorption spectrometry and some others is also discussed. Finally, the main practical applications on this topic are summarized. [...]
3
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Ion-pair chromatographic monitoring of photographic effluents

71%
Kesiũnaitė G., Pranaitytė B., Padarauskas A., Dikčius A., Ragauskas R.
Open Chemistry
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2007
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vol. 5
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issue 2
455-465
EN
Ion-pair chromatographic technique was developed for the rapid and simple determination of the main contaminants (bromide, iodide, sulphite, thiosulphate, thiocyanate, iron(III)-EDTA chelate, free EDTA, hydroquinone and phenidone) in spent photographic solutions. Free EDTA was converted into stable Ni(II)-EDTA chelate prior to analysis. The optimal mobile phase conditions were established by varying the concentrations of tetrabutylammonium (TBA) phosphate and acetonitrile, pH and ionic strength. Separation of five inorganic anions, two metal chelates and two neutral compounds was accomplished in about 30 min using a mobile phase containing 7.5 mmol/L TBA-phosphate, 10 mmol/L NaCl (pH 6.5) and 20% (v/v) acetonitrile. The detection limits (UV detection at 210 nm) ranged from 0.4 µmol/L for phenidone to 8 µmol/L for sulphite with a linearity of 2–2.5 orders of magnitude. The method was applied to the rapid monitoring of spent photographic solutions before and after decomposition. The recovery tests established for two samples were within the range 95–103%. [...]
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