Evaluation of on-line solid-phase extraction parameters for hyphenated, high-performance liquid chromatography–solid-phase extraction–nuclear magnetic resonance applications

Clarkson, Cailean; Sibum, Martin; Mensen, Robert; Jaroszewski, Jerzy W.

doi:10.1016/j.chroma.2007.07.016

Cited by 43 publications

(47 citation statements)

References 32 publications

Supporting

Mentioning

Contrasting

Unclassified

Order By: Relevance

“…Consequently, LC-SPE-NMR coupling provides increased sensitivity and substantial gains in the signal-to-noise ratio relative to conventional LC-NMR by multiple trapping of the interest peaks onto the same SPE cartridges through repeated chromatographic injections. 30,31 Moreover, when using LC-SPE-NMR, there is no need to use deuterated water as in LC-NMR methods. Hence, the structural information obtained from NMR analysis combined with the molecular mass and the fragmentation profile obtained from LC-MS n enable an unequivocal structural elucidation of impurities, mainly for isomeric mixtures.…”

Section: Structure Elucidation Of the Unknown Impurities By Lc-ms N Amentioning

confidence: 99%

Preparative Separation and Structural Identification of Impurities of a New α2‑Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR

Cardoso

Thomasi

Venâncio

et al. 2016

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

Identifying impurities in drug substances has become one of the most important issues in pharmaceutical analysis since it can have a significant impact on the efficacy of new pharmaceutical products. Due to the purity requirements, in this paper a new synthetic α 2 -adrenoceptor agonist, called LPSF-PT-31, was purified and its impurities were characterized by liquid chromatographymultistage mass spectrometry (LC-MS n ) and liquid chromatography-solid phase extraction-nuclear magnetic resonance (LC-SPE-NMR). The purification step was conducted using a semi-preparative liquid chromatography and stacked injections as a new approach to drug purification. As a result, a total yield of 75% of the pure LPSF-PT-31 and 2.9 L day -1 in solvent reduction was obtained. The combination of semi-preparative stacking injection, LC-MS n , and LC-SPE-NMR, demonstrated to be efficient to purify active drugs and unambiguously identify its impurities. In addition, isolation and identification of drug impurities in the early stages of development can improve the synthetic pathway, preventing the formation of impurities or minimizing this formation to minimum levels.

show abstract

Section: Structure Elucidation Of the Unknown Impurities By Lc-ms N Amentioning

confidence: 99%

Preparative Separation and Structural Identification of Impurities of a New α2‑Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR

Cardoso

Thomasi

Venâncio

et al. 2016

J. Braz. Chem. Soc.

View full text Add to dashboard Cite

show abstract

“…This involves performing NMR detection at-line after the HPLC separation by either trapping the LC-peaks on SPE (LC-SPE-NMR) [13,68,69] or by HPLC microfractionation, drying and reinjection of the concentrated LC-peak in deuterated solvent in a microflow capillary LC-NMR probe (CapNMR) [14,63,70].…”

Section: Spe-nmr Microflow Nmr and Nmr With Cryogenized Probesmentioning

confidence: 99%

“…This technique presents the advantage that the separation can be performed with normal protonated solvent and, moreover, multiple trapping of the same analyte from repeated LC injection circumvents problems of low concentration. The operation can be fully automated on state-of-the-art systems, but a good optimization of the trapping conditions is required for optimum performances [69,71]. The use of either semipreparative or analytical columns with and without multiple trapping parameters has been investigated [72].…”

Section: Spe-nmr Microflow Nmr and Nmr With Cryogenized Probesmentioning

confidence: 99%

Modern Approaches in the Search for New Active Compounds from Crude Extracts of Natural Sources

Queiroz

Hostettmann

Wolfender

2012

Plant Bioactives and Drug Discovery

View full text Add to dashboard Cite

“…The system was applied to biological samples, detecting a number of modified nucleosides. Clarkson et al [47] described HPLC -SPE -NMR hyphenation for structural elucidation of some natural products. Lambert et al [48] described the identification of natural products by using SPE -HPLC coupling with Cap-NMR.…”

Section: Hyphenation In Liquid Chromatographymentioning

confidence: 99%

Hyphenation in sample preparation: Advancement from the micro to the nano world

Ali

Gupta

Aboul‐Enein³

et al. 2008

J of Separation Science

121

View full text Add to dashboard Cite

Analysis at trace levels, an ideal area of application for hyphenated techniques, is steadily gaining importance. Many sample pre-concentration and clean-up methods have been hyphenated with core analytical techniques to accomplish the task of low level detection. The present article describes the state of the art of hyphenation of various techniques such as solid phase extraction, micro-solid phase extraction, dialysis, and chromatographic modalities etc. with liquid chromatography, gas chromatography, capillary electrophoresis, and spectroscopic methods. Besides, attempts have been made to address the hyphenation approach in microfluidic devices.

show abstract

Evaluation of on-line solid-phase extraction parameters for hyphenated, high-performance liquid chromatography–solid-phase extraction–nuclear magnetic resonance applications

Cited by 43 publications

References 32 publications

Preparative Separation and Structural Identification of Impurities of a New α2‑Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR

Preparative Separation and Structural Identification of Impurities of a New α2‑Adrenoceptor Agonist Using Stacking Injection, LC-MSn and LC-SPE-NMR

Modern Approaches in the Search for New Active Compounds from Crude Extracts of Natural Sources

Hyphenation in sample preparation: Advancement from the micro to the nano world

Contact Info

Product

Resources

About