Development of chiral methodologies by capillary electrophoresis with ultraviolet and mass spectrometry detection for duloxetine analysis in pharmaceutical formulations

Sánchez-López, Elena; Montealegre, Cristina; Marina, Marı́a Luisa; Crego, Antonio L.

doi:10.1016/j.chroma.2014.07.038

Cited by 31 publications

(21 citation statements)

References 18 publications

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“…A work reported by our research group described the use of PFT in an EKC‐MS 2 (IT) system aimed to develop a chiral methodology to evaluate the enantiomeric purity of the drug duloxetine . Although just a 0.5% w/v of chiral selector ((2‐hydroxypropyl)‐β‐CD) was employed, PFT had to be applied to avoid the loss of sensitivity caused by ion suppression.…”

Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

“…CE conditions: BGE, 150 mM phosphate buffer (pH 3.0) + 0.5% w/v (2‐hydroxypropyl)‐β‐CD in (A), and 150 mM ammonium formate (pH 3.0) with a PFT step consisting on injecting 0.5% w/v (2‐hydroxypropyl)‐β‐CD in BGE at 1 bar during 1 min in (B); voltage, 30 kV; temperature, 20ºC in (A) and 15ºC in (B); hydrodynamic injection, 50 mbar for 20 s in (A) and 50 mbar for 5 s in (B). Reprinted and modified from with permission from Elsevier.…”

Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

“…Since EKC has been the only CE mode reported in the last years (see Table ), these strategies had to be employed. Thereby, PFT has been used in four CE‐MS methodologies whereas that CMT, jointly with PFT, has been employed in just a work . Moreover, the analyzer most employed in CE‐MS has been IT either using MS or MS 2 experiments , although a work employing a TOF using MS experiments has been reported too .…”

Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

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Improving the sensitivity in chiral capillary electrophoresis

2015

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CE is known for being one of the most powerful analytical techniques when performing enantioseparations due to its numerous advantages such as excellent separation efficiency and extremely low solvents and reagents consumption, all of them derived from the capillary small dimensions. Moreover, it is worth highlighting that unlike in chromatographic techniques, in CE the chiral selector is generally within the separation medium instead of being attached to the separation column which makes the method optimization a more versatile task. Despite its numerous advantages, when using UV-Vis detection, CE lacks of sensitivity detection due to its short optical path length derived from the narrow separation capillary. This issue can be overcome by means of different approaches, either by sample treatment procedures or by in-capillary preconcentration techniques or even by employing detection systems more sensitive than UV-Vis, such as LIF or MS. The present review assembles the latest contributions regarding improvements of sensitivity in chiral CE published from June 2013 until May 2015, which follows the works included in a previous review reported by Sánchez-Hernández et al. [Electrophoresis 2014, 35, 12-27].

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Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

Section: Strategies To Enhance the Detection Sensitivitymentioning

confidence: 99%

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Improving the sensitivity in chiral capillary electrophoresis

2015

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“…Several CE‐MS/MS methodologies were developed for drug quality and composition control: simultaneous determination of 12 pharmaceutical components in dietary supplements for weight loss ; simultaneous determination of vitamins B, namely thiamine, riboflavin, nicotinamide, nicotinic acid, pantothenic acid, pyridoxine, biotin, folic acid, and cyanocobalamine in pharmaceuticals and dietary supplements ; two chiral CE‐UV and CE‐MS methodologies were developed to ensure the quality control of the drug duloxetine, while the LOD of 0.02% of duloxetine enantiomeric impurity is the lowest value ever reported for this drug . Two CE‐MS sensitive methods of drugs analyses in body fluids and tissues were developed: for simultaneous determination of psychoactive drugs: 1‐benzylpiperazine, 7‐aminoclonazepam, alprazolam, clonazepam, diazepam, estazolam, lorazepam, and tetrazepam in human serum and hair samples and for the isolation and enrichment of modified nucleosides and nucleobases in urine .…”

Section: Analytical Applicationsmentioning

confidence: 99%

Recent advances in CE‐MS coupling: Instrumentation, methodology, and applications

2016

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This review focuses on the latest development of microseparation electromigration methods in capillaries and microfluidic devices coupled with MS for detection and identification of important analytes. It is a continuation of the review article on the same topic by Kleparnik (Electrophoresis 2015, 36, 159-178). A wide selection of 161 relevant articles covers the literature published from June 2014 till May 2016. New improvements in the instrumentation and methodology of MS interfaced with capillary or microfluidic versions of zone electrophoresis, isotachophoresis, and isoelectric focusing are described in detail. The most frequently implemented MS ionization methods include electrospray ionization, matrix-assisted desorption/ionization and inductively coupled plasma ionization. Although the main attention is paid to the development of instrumentation and methodology, representative examples illustrate also applications in the proteomics, glycomics, metabolomics, biomarker research, forensics, pharmacology, food analysis, and single-cell analysis. The combinations of MS with capillary versions of electrochromatography, and micellar electrokinetic chromatography are not included.

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“…CE in its different modes such as CZE and EKC has been widely used as a powerful tool for enantioseparation in pharmaceutical analysis given to its high efficiency and resolution, low solvent consumption, and short analysis time, becoming an alternative to the conventional HPLC method . Among all chiral selectors in CE, CDs are considered the most important mainly to their usefulness in the development of analytical separation methods and also for the study and characterization of supramolecular complex formation.…”

Section: Introductionmentioning

confidence: 99%

Development of an enantioselective capillary electrophoretic method for the simultaneous determination of montelukast enantiomeric and diastereoisomeric forms and its main degradation product

et al. 2016

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A stereoselective CD-MEKC system has been developed for the quality control of Montelukast (MK), commercialized as a pure enantiomer. The proposed method is the first one that allows the simultaneous determination of MK, its enantiomeric form, diasteroisomers and its main degradation compound (MK sulphoxide). CD-MEKC system is composed of 10 mM SDS, 10 mM sulfobutylether-␤-CD, 10 mM TM-␤-CD, and 20 mM borate buffer at pH 9.0. Combination of these two CDs allows high baseline enantioresolution between MK and its enantiomeric impurity, but also, between the diasteroisomeric forms. Moreover, a multivariate design was applied to optimize operational parameters. The method was designed to meet with requirements of the official pharmacopoeias and fully validated according to international guidelines. Linearity of MK was demonstrated in the range from 10.0 to 100.0 g/mL (r 2 = 0.9908) with a LOD and LOQ of 0.30 and 0.90 g/mL, respectively. Intra and interday precision were evaluated and RSD values were below 2%, and also, accuracy expressed as percentage of recovery was in a range from 99.0 to 101.9 for the three assayed levels. The method allows determining 0.02% w/w of the enantiomeric and diasteroisomeric impurities, and 0.01% w/w of MK sulphoxide. Robustness was evaluated by a Plackett and Burman design. Finally, the CD-MEKC system was successfully applied to the determination of related substances in MK bulk drug and its quantification in two pediatric pharmaceutical dosage forms.

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Development of chiral methodologies by capillary electrophoresis with ultraviolet and mass spectrometry detection for duloxetine analysis in pharmaceutical formulations

Cited by 31 publications

References 18 publications

Improving the sensitivity in chiral capillary electrophoresis

Improving the sensitivity in chiral capillary electrophoresis

Recent advances in CE‐MS coupling: Instrumentation, methodology, and applications

Development of an enantioselective capillary electrophoretic method for the simultaneous determination of montelukast enantiomeric and diastereoisomeric forms and its main degradation product

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