Enhanced chromatographic NMR with polyethyleneglycol. A novel resolving agent for diffusion ordered spectroscopy

Kavakka, Jari; Parviainen, Viktor; Wähälä, Kristiina; Kilpeläinen, Ilkka; Heikkinen, Sami

doi:10.1002/mrc.2660

Cited by 44 publications

(30 citation statements)

References 26 publications

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“…In this experiment a pseudo two dimensional spectrum is obtained correlating chemical shift with observed diffusion coefficient [3] and thereby allowing the spectral separation of complex mixtures [3][4][5]. More recently, techniques have been developed which seek to enhance the observed separation in the diffusion dimension via modification of the solvent system using polymer additives [6,7] and surfactant micelles [8,9]. The principle behind these approaches is that the various species comprising the mixture will have differing interactions with these additives, and hence the observed separation in the diffusion dimension will be influenced by the strength of these interactions.…”

Section: Introductionmentioning

confidence: 99%

Chromatographic NMR with size exclusion chromatography stationary phases

Joyce

Day

2012

Journal of Magnetic Resonance

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Section: Introductionmentioning

confidence: 99%

Chromatographic NMR with size exclusion chromatography stationary phases

Joyce

Day

2012

Journal of Magnetic Resonance

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“…(Rodrigues, da Silva, Denise Brentan, de Oliveira, Dionéia Camilo Rodrigues, & da Silva, Gil Valdo José, 2009) Recently, various additives, like polyethylenglycol (PEG) or sodium dodecyl sulfate (SDS) have been used to improve resolution in these DOSY measurements of flavonoid containing mixtures. (Kavakka, Parviainen, Wähälä, Kilpeläinen, & Heikkinen, 2010) Compared to direct HPLC-NMR hyphenation off-line techniques usually provide higher quality of NMR spectra and allow by multiple trapping an increase in analyte amounts. Despite the significant gain of instrumental and experimental sensitivity NMR based approaches still rely on time-consuming NMR resonance assignments in case of flavonoid identifications.…”

Section: Introductionmentioning

confidence: 99%

Efficient identification of flavones, flavanones and their glycosides in routine analysis via off-line combination of sensitive NMR and HPLC experiments

et al. 2017

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We present a standardized, straightforward and efficient approach applicable in routine analysis of flavonoids combining sensitive NMR and HPLC experiments. The determination of the relative configuration of sugar moieties usually requires the acquisition of C NMR shift values. We use a combination of HPLC and sensitive NMR experiments (1D-proton, 2D-HSQC) for the unique identification of known flavones, flavanones, flavonols and their glycosides. Owing to their broad range of polarity, we developed HPLC and UHPLC methods (HO/MeOH/MeCN/HCOOH) which we applied and validated by analyzing 46 common flavones and flavanones and exemplified for four plant extracts. A searchable data base is provided with full data comprising complete proton and carbon resonance assignments, expansions of HSQC-spectra, HPLC parameters (retention time, relative retention factor), UV/Vis and mass spectral data of all compounds, which enables a rapid identification and routine analysis of flavones and flavanones from plant extracts and other products in nutrition and food chemistry.

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“…10 Polymers like polyvinylpyrrolidone (PVP) 11 and polyethylene glycol (PEG) 12 have also been used as efficient matrices in MAD. b-Cyclodextrin 13,14 has been used as a chiral matrix, allowing the resolution of a mixture of two native epimers of naringin.…”

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confidence: 99%

Natural product mixture analysis by matrix-assisted DOSY using Brij surfactants in mixed solvents

et al. 2014

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The assignment of NMR signals to specific components in a mixture is a challenging task. Diffusion-Ordered Spectroscopy (DOSY) has provided important progress in this area, allowing the signals originating from individual components of different molecular sizes to be distinguished. However, when the sizes of the compounds are similar and/or the spectra are overlapped, signal assignment can easily become intractable. The use of a co-solute in a matrix-assisted DOSY (MAD) experiment can be a useful solution, improving diffusional (and sometimes spectral) resolution by exploiting selective binding to the matrix.MAD has generated promising results in the study of several types of mixtures, including those of functional and structural isomers. The challenge is to apply MAD to molecules with high structural similarity, for example in natural product mixtures. Various surfactants, including SDS, AOT and CTAB have previously been shown to be effective in MAD analysis. Here we present an important addition, the Brij family of nonionic surfactants. We demonstrate the use of Brij micelles in mixed solvents with a variety of mixtures relevant to natural products.

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Enhanced chromatographic NMR with polyethyleneglycol. A novel resolving agent for diffusion ordered spectroscopy

Cited by 44 publications

References 26 publications

Chromatographic NMR with size exclusion chromatography stationary phases

Chromatographic NMR with size exclusion chromatography stationary phases

Efficient identification of flavones, flavanones and their glycosides in routine analysis via off-line combination of sensitive NMR and HPLC experiments

Natural product mixture analysis by matrix-assisted DOSY using Brij surfactants in mixed solvents

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