Separation and Analysis of Trace Degradants in a Pharmaceutical Formulation Using On-Line Capillary Isotachophoresis-NMR

Eldridge, Stacie L.; Almeida, Valentino K.; Korir, and Albert K.; Larive, Cynthia K.

doi:10.1021/ac7016629

Cited by 29 publications

(17 citation statements)

References 44 publications

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“…In one report, the limitations in sensitivity were partially overcome by online coupling isotachophoresis cITP to microcoil NMR detection (78). After preconcetration by ITP, microcoil NMR was suitable to detect trace impurities of degradation products in acetaminophen samples.…”

Section: Detectionmentioning

confidence: 99%

Capillary Electrophoresis in Bioanalysis

2008

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Science reports ∼4800 hits on capillary electrophoresis (CE) including 410 reviews. Because of the prominence of CE techniques in bioanalysis, we decided make them the focus of this review and selected 200 hundred papers representing advances in this field. The selected papers cover advances in CE theory, instrumentation, and methodologies that are specific to various analytes of biological origin or relevance. The group of analytes includes nucleic acids, proteins and peptides, carbohydrates, lipids, single cells, and bioparticles. In addition, we have included advances in the use of CE to define functional assays or to investigate biomolecular interactions. The use of microfabricated devices for CE analysis was not included because this is already covered in other review. Technique Developments Separation SchemesDetermining the velocity of the electroosmotic flow (EOF) and how it changes during an electrophoretic separation is still an important research topic. A simple method for EOF measurements using so-called thermal marks was reported (1). Here, a tungsten filament caused punctual heating at the capillary wall and caused a perturbation in the electrolyte concentration. A sequence of these "thermal marks" then migrated with the EOF until each mark reached and was detected by a conductivity detector. The feasibility of using thermal marks as internal EOF standards in different separation systems was thereby demonstrated.Isoelectric focusing separates amphoteric analytes such as proteins or peptides by the differences in their isoelectric points. Most of the reports on capillary isoelectric focusing (cIEF) describe an initial focusing phase after which the focused zones are mobilized and detected. A dynamic cIEF method for protein analysis was reported (2). This technique made it possible to control each protein's position and focused width by moving the pH gradient within the capillary through manipulation of the electric fields. An important advantage of this approach is the capability of collecting focused analytes from the central section, suggesting that there may be great potential for introducing selectively focused proteins to a second separation dimension such as LC or CE.Micellar electrokinetic capillary chromatography (MEKC) is typically incompatible with electrospray mass spectrometry (ESI-MS) because the nonvolatile surfactants in the micellar phase result in complicated adduct formation and loss of sensitivity during the electrospray process and because the presence of the organic solvent needed for electrospray may cause instability in the micellar phase. These drawbacks were overcome by using synthetic polymeric surfactants that can work as a pseudostationary phase and provide stable electrospray (3). The polymeric surfactant was made by polymerizing three amino acidderived (L-leucinol, L-isoleucinol, L-valinol) sulfated chiral surfactants. These polymeric

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Section: Detectionmentioning

confidence: 99%

Capillary Electrophoresis in Bioanalysis

2008

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“…1 H NMR spectral signals could be obtained for PAP and other DPs, which were dimeric in nature. The characterization was further confirmed through LC-MS/MS study [257].…”

Section: Ce-nmrmentioning

confidence: 91%

A critical review on the use of modern sophisticated hyphenated tools in the characterization of impurities and degradation products

Singh

Handa

Narayanam

et al. 2012

Journal of Pharmaceutical and Biomedical Analysis

184

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“…This principle was applied for the determination of 4-aminophenol in an acetaminophen sample spiked at the 0.1% level by hyphenating ITP to an NMR spectrometer, overcoming in this way the relatively poor sensitivity of the spectrometric method (in comparison to MS). By this combination, several other trace compounds could be detected after thermal degradation of the parent drug [30].…”

Section: Miscellaneous Drugsmentioning

confidence: 98%

Impurity analysis of pharmaceuticals using capillary electromigration methods

Jouyban

Kenndler

2008

Electrophoresis

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This review deals with the determination of impurities in pharmaceuticals by electromigration methods in the capillary format. These separation methods are either based on the different effective mobility of the charged analytes (as in zone electrophoresis and isotachophoresis) or include hybrid methods such as micellar electrokinetic chromatography, microemulsion electrokinetic chromatography and electrochromatography. The pharmaceutically active compounds under consideration belong to chemotherapeutic agents, central nervous system drugs, histamine receptor drugs, cardiovascular drugs, anticancer drugs, anti-inflammatory drugs and some other drugs. The review discusses about 150 publications from the period between 1980 and 2007 with special emphasis on the recent trends and gives details about the experimental conditions applied for analyses and the obtained analytical performance parameters.

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Separation and Analysis of Trace Degradants in a Pharmaceutical Formulation Using On-Line Capillary Isotachophoresis-NMR

Cited by 29 publications

References 44 publications

Capillary Electrophoresis in Bioanalysis

Capillary Electrophoresis in Bioanalysis

A critical review on the use of modern sophisticated hyphenated tools in the characterization of impurities and degradation products

Impurity analysis of pharmaceuticals using capillary electromigration methods

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