Evaporative light scattering detection for in-line monitoring of stopped-flow liquid chromatography-nuclear magnetic resonance analysis of compounds with weak or no chromophore groups

Pétritis, Konstantinos; Gillaizeau, Isabelle; Elfakir, Claire; Dreux, M.; Petit, Alain; Bongibault, Nelly; Luijten, W.

doi:10.1002/1615-9314(20020601)25:9<593::aid-jssc593>3.0.co;2-f

Cited by 13 publications

(4 citation statements)

References 41 publications

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“…This extended hyphenation is useful not only by making MS or MS/MS data available simultaneously with the NMR data, but also because trapping of non-UV-absorbing constituents can be triggered by signals provided by MS (total ion or single ion monitoring). Furthermore, it can be mentioned that evaporative light scattering detection (ELS), already used in connection with stopped-flow HPLC-NMR [53], could be used to trigger trapping in a putative HPLC-ELS-SPE-NMR experiment.…”

Section: Hyphenation Of Other Techniques With Hplc-spe-nmrmentioning

confidence: 99%

Hyphenated NMR Methods in Natural Products Research, Part 2: HPLC-SPE-NMR and Other New Trends in NMR Hyphenation

2005

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IntroductionIn the first part of this review [1], the use of direct NMR hyphenation in natural products research has been discussed. The direct HPLC-NMR methods were defined as methods in which the NMR data acquisition is performed on the HPLC column eluate [1]. This implies either a direct connection between the NMR spectrometer and the HPLC apparatus, or use of storage capillaries in which the HPLC eluate is temporarily stored prior to acquisition of NMR data.Many useful results related to natural products have been obtained using direct HPLC-NMR methods [1] [30]. However, the direct combination of state-of-the-art separation technology with the most powerful and versatile tool for structure elucidation of organic molecules in solution suffers from various practical problems. In short, these practical limitations are due to somewhat contradictory requirements of HPLC and NMR with respect to solvents and time-scale of the experiment, and thus compromises are necessary in order to hyphenate these two techniques. For example, 1 H-NMR spectra are preferably acquired in deuterated solvents, but use of deuterated solvents for HPLC is expensive and the selection is limited. Some useful HPLC eluents, such as buffers with high ionic strengths, are directly undesirable in direct HPLC-NMR hyphenation. Gradient elution of HPLC columns, required in most separations, implies constantly changing magnetic susceptibility and field homogeneity in the NMR flowprobe, not to mention variations of analyte chemical shifts with solvent composition. Hyphenated NMR Methods in Natural Products AbstractThis review describes the principles and performance of a novel and highly promising hyphenated technique, HPLC-SPE-NMR, which is based on post-column analyte trapping by solid-phase extraction. The analytes are subsequently eluted from the SPE cartridges using deuterated solvents. This indirect HPLC-NMR hyphenation offers numerous advantages compared to direct HPLC-NMR methods. Multiple trapping leads to a dramatic increase of analyte amounts available for NMR, enabling acquisition of high-quality 2D NMR data within a short time. Other new developments, including combination of solenoidal coil capillary flow-probes with microflow HPLC, are also discussed. Fast extract dereplication using these techniques enables focusing of isolation efforts on truly novel and promising natural products, based on precise structural data obtained with crude extracts or fractions.

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Section: Hyphenation Of Other Techniques With Hplc-spe-nmrmentioning

confidence: 99%

Hyphenated NMR Methods in Natural Products Research, Part 2: HPLC-SPE-NMR and Other New Trends in NMR Hyphenation

2005

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“…In addition, detection methods such as conductometry [21][22][23][24][25][26][27][28][29], electrospray ionizationtandem mass spectrometry (ESI-MS/MS) [30] or nuclear magnetic resonance spectroscopy (NMR) [31][32] can be used. Recently Petritis et al [30,33,34] reported the evaluation of an enantioselective method for the analysis of 20 un-derivatised amino acids by liquid chromatography ion spray tandem mass spectrometry using a teicoplanin-based chiral stationary phase to separate the enantiomers of the amino acids.…”

Section: Introductionmentioning

confidence: 99%

Quantitative determination of un-derivatised amino acids in artistic mural paintings using high-performance liquid chromatography/electrospray ionization triple quadrupole mass spectrometry

Zangrando¹,

Piazza²,

Cairns³

et al. 2010

Analytica Chimica Acta

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“…These methods include direct detection by UV absorbance at low wavelengths when high sensitivity is not necessary [1 -5], conductivity detection [2, 6 -8] electrospray MS methods, in simple and tandem MS mode [2, 9 -11], detection via native fluorescence (FL) [12], and some other detection techniques, e.g., evaporative light scattering (ELS) [2,13,14], refractive index (RI) [2], chemiluminescent nitrogen (CLN) [2] or NMR detection [2] as well as a combination of two different methods of detection such as NMR-ELS [15] or UV-ELS detection [16]. The detector, however, that has been investigated the most for underivatized amino acid analysis is the electrochemical (EC) detector [4, 17 -28].…”

Section: Introductionmentioning

confidence: 99%

Direct RP‐HPLC determination of underivatized amino acids with online dual UV absorbance, fluorescence, and multiple electrochemical detection

Agrafiotou

Sotiropoulos

Pappa-Louisi

2009

J of Separation Science

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Original PaperDirect RP-HPLC determination of underivatized amino acids with online dual UV absorbance, fluorescence, and multiple electrochemical detectionThe combined use of a dual-UV detector, a fluorimetric one and of a multiple electrochemical (EC) detector equipped with a dual electrode, consisting of a conventional size 3 mm diameter glassy carbon electrode (GCE) and of a pair of 30 lm thick carbon microfibers, is proposed for the determination of 15 amino acids, two dipeptides and creatinine. This online coupling of the above detection modes could partially replace amino acid analysis by derivatization methods, since it solves problems concerning the direct detection of selected underivatized amino acids. Additionally, it was proved that the use of multiple-detection allows positive peak identification in a single chromatographic run, yields more information for free amino acids and solves in some cases the problem of chromatographic resolution. In order to optimize the detection conditions of the underivatized amino acids and related compounds by different detectors, their detection characteristics were determined by adequate preliminary experiments. The electro-oxidation characteristics of the underivatized compounds of interest were determined by hydrodynamic voltammetry using a flow cell with a macrodisc GCE and by ex-situ voltammetry using both a GCE of conventional size and a carbon fiber disk microelectrode. Important practical advantages of microfiber and microdisk electrodes with respect to macroelectrodes were demonstrated.Keywords: Dual electrode / Microdisc electrode / Multiple UV-fluorescence-electrochemical detection / Reversed phase liquid chromatography (RPLC) / Underivatized amino acids and related compounds /

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Evaporative light scattering detection for in-line monitoring of stopped-flow liquid chromatography-nuclear magnetic resonance analysis of compounds with weak or no chromophore groups

Cited by 13 publications

References 41 publications

Hyphenated NMR Methods in Natural Products Research, Part 2: HPLC-SPE-NMR and Other New Trends in NMR Hyphenation

Hyphenated NMR Methods in Natural Products Research, Part 2: HPLC-SPE-NMR and Other New Trends in NMR Hyphenation

Quantitative determination of un-derivatised amino acids in artistic mural paintings using high-performance liquid chromatography/electrospray ionization triple quadrupole mass spectrometry

Direct RP‐HPLC determination of underivatized amino acids with online dual UV absorbance, fluorescence, and multiple electrochemical detection

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