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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 [...]
A sensitive and specific high performance liquid chromatography coupled with fluorescent detection (HPLC-FL) and tandem mass spectrometry detection (HPLC-MS/MS) methods for separation and determination of carvedilol (CAR) enantiomers and 5′-hydroxyphenyl carvedilol (5′-HCAR) enantiomers has been developed and validated. The analysed compounds were extracted from human urine by solid phase extraction. Good enantioseparation of the studied enantiomers was achieved on CHIRALCEL® OD-RH column using 0.05% trifluoroacetic acid and 0.05% diethylamine in water and acetonitrile in a gradient elution. The mass spectrometric data were acquired using the multiple reaction monitoring mode by positive electrospray ionisation. The method was validated over the concentration range from 25.0 ng mL−1 to 200 ng mL−1 for the analysed compounds. The limit of quantification varied from 14.2 ng mL−1 to 24.2 ng mL−1. Both the repeatability and inter-day precisions were below 10.0%, and the accuracy varied from −13.2% to 3.77%. The extraction recoveries ranged from 79.2% to 108%. The present paper reports the method for the simultaneous determination of CAR enantiomers and their metabolite enantiomers (5′-HCAR) in human urine samples. This newly developed method was successfully used to analyse the aforementioned analytes in human urine samples obtained from patients suffering from cardiovascular disease. [...]
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