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Separation of ketoprofen enantiomers at nanomolar concentration levels by micellar electrokinetic chromatography with on-line electrokinetic preconcentration

100%

Petr J., Ginterová P., Znaleziona J., Knob R., Lošťáková M., Maier V., Ševčík J.

Open Chemistry

2013

vol. 11

issue 3

335-340

Abstract Separation of enantiomers represents an extremely important task in the field of analytical chemistry. This paper contributes to the field of the on-line preconcentration of enantiomers by developing a novel setup based on the electrokinetic accumulation of ketoprofen enantiomers on the pH boundary followed by enantioselective mobilization by a mixture of SDS, sulfated-β-cyclodextrin (S-β-CD), and trimethyl-β-cyclodextrin (TM-β-CD). Under the best conditions, where the injection electrolyte was composed of 50 mmol L−1 borate/NaOH pH 9.5 with 60% (v/v) methanol, the background electrolyte contained 50 mmol L−1 phosphate/NaOH pH 2.5, and the mobilization electrolyte consisted of 50 mmol L−1 phosphate/NaOH pH 2.5 with 4.0% (w/v) S-β-CD, 0.5% (w/v) TM-β-CD, and 20 mmol L−1 SDS, the determination of nanomolar concentration levels of ketoprofen enantiomers was successful by using micellar electrokinetic chromatography with a common UV detection. LODs were 2.5 nmol L−1 and 3.4 nmol L−1, which represent enhancement factors of 9921 and 8529, respectively. The method was also applied to the determination of ketoprofen enantiomers in waste water samples by using simple filtration as a clean-up step. Here, the recovery of ketoprofen enantiomers was 91% at the concentration level of 5×10−9 mol L−1. Graphical abstract [...]

Binuclear copper complexes with non-steroidal anti-inflammatory drugs as studied by electrospray ionization mass spectrometry

88%

Kowcun K., Frańska M., Frański R.

Open Chemistry

2012

vol. 10

issue 2

320-326

The solutions containing one of the copper salts (CuCl2, Cu(ClO4)2, Cu(NO3)2, and CuSO4) and one of the non-steroidal anti-inflammatory drugs (NSAIDs, ibuprofen, ketoprofen or naproxen) were analyzed by electrospray ionization mass spectrometry. Three of the salts, namely CuCl2, Cu(ClO4)2 and Cu(NO3)2, yielded binuclear complexes of drug:metal stoichiometry 1:2. Existence of the complexes of such stoichiometry has not been earlier observed. For copper(II) chloride the complexes (ions of the type [M-HCOOH+Cu2Cl]+ and [M+Cu2Cl]+, M stands for the drug molecule) were formed in the gas phase. When copper(II) perchlorate or copper(II) nitrate was used, the observed binuclear copper complexes (ions of the type [M-H+Cu2(ClO4)2+CH3OH]+, [M-H+Cu2(ClO4)2]+ and [M-H+Cu2(NO3)2+CH3OH]+, [M-H+Cu2(NO3)2]+) were observed at low cone voltage, thus these complexes must have already existed in the solution analysed. Therefore, such complexes may also exist under physiological conditions. [...]

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2 Open Chemistry

1 2013

1 2012

1 Frańska M.

1 Frański R.

1 Ginterová P.

1 Knob R.

1 Kowcun K.

1 Lošťáková M.

1 Maier V.

1 Petr J.

1 Znaleziona J.

1 Ševčík J.

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Separation of ketoprofen enantiomers at nanomolar concentration levels by micellar electrokinetic chromatography with on-line electrokinetic preconcentration

Binuclear copper complexes with non-steroidal anti-inflammatory drugs as studied by electrospray ionization mass spectrometry