Separations coupled with NMR detection

Cardoza, Laurie A.; Almeida, Valentino K.; Carr, Amy; Larive, Cynthia K.; Graham, David W.

doi:10.1016/s0165-9936(03)01012-4

Cited by 35 publications

(21 citation statements)

References 31 publications

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“…Examples for this have been reported in the literature. 15 The second, more serious strategy consists in characterizing environmental samples as comprehensively as possible with respect to their composition. This approach includes elements of both target and non-target analysis and is of particular importance if in situ processes and transformation reactions are investigated at the waste site.…”

Section: Results and Discussion Strategies For The Analysis Of Enviromentioning

confidence: 99%

Analysis of highly polar compounds in groundwater samples from ammunition waste sites. Part I—Characterization of the pollutant spectrum

Preiß

Elend

Gerling

et al. 2005

Magnetic Reson in Chemistry

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Five groundwater samples from the former ammunition production site at Elsnig, Germany, were analyzed for highly polar components by LC-NMR and LC-MS. A variety of unknown pollutants could be identified. Possibilities and limitations of the combined use of LC-NMR and LC-MS techniques for on-line identification are discussed. Further unknown components were identified through isolation by HPLC cuts and off-line NMR and MS investigations. Most of the polar compounds in the investigated samples could also be quantified.

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Section: Results and Discussion Strategies For The Analysis Of Enviromentioning

confidence: 99%

Analysis of highly polar compounds in groundwater samples from ammunition waste sites. Part I—Characterization of the pollutant spectrum

Preiß

Elend

Gerling

et al. 2005

Magnetic Reson in Chemistry

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“…For this investigation, 3 µg of a drug-like molecule, ethyl 8-allyl-5-(3-methylbutoxy)-4-oxo-4H-chromene-2-carboxylate, was dissolved in methanol-d 4 . The minimum volume of solvent required for the specific probe and tube was used in the case of tube probes.…”

Section: Comparison Of Nmr Probes Sensitivitymentioning

confidence: 99%

“…1,2 Since then, improvements in experimental set-up and probe technology have ensured that analytical-scale LC-NMR has become a well-established technique in laboratories across the globe. 3,4 NMR sensitivity has always been an issue in LC-NMR and different groups have favoured different methods of dealing with analytes at low concentration. 5 -11 One approach to improve sensitivity has been miniaturization of the NMR probe.…”

Section: Introductionmentioning

confidence: 99%

A comparison of capillary‐scale LC–NMR with alternative techniques: spectroscopic and practical considerations

Lewis

Bernstein

Duncan

et al. 2005

Magnetic Reson in Chemistry

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Experimental and practical details for the use of capillary LC (CapLC)-NMR are reported. The capillary NMR probe has high sensitivity and excellent flow characteristics and we found CapLC-NMR to be best suited to samples that are truly mass limited. CapLC-NMR relies on good capillary-scale chromatography where highly concentrated peaks with a volume closely matched to the NMR flow cell are achievable. Provided that the loading capacity of the capillary column is not limiting, the combination of high sensitivity and high solvent suppression quality makes CapLC-NMR an excellent choice. For many real samples, however, the loading is limiting and we found the combination of LC-SPE-MS-NMR with a cryoprobe enables more material to be purified for NMR analysis, while retaining sensitivity.

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“…With the introduction of high-field 1 H NMR (500-800 MHz) and cryogenic probe technologies, absolute amounts of small and medium-size compounds can be analyzed in the lower microgram range [10]. Meanwhile, NMR and HPLC-NMR are recognized as important tools in environmental analysis [11,12,13]. Non-target analysis by HPLC-NMR and HPLC-MS has already been applied to groundwater samples from waste sites with specific classes of pollutants such as explosives and related compounds [14] or quinolines [15] and also to organic acids in leachate samples from industrial landfills [16].…”

Section: Introductionmentioning

confidence: 99%

A new analytical approach for the comprehensive characterization of polar xenobiotic organic compounds downgradient of old municipal solid waste (MSW) landfills

et al. 2012

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Groundwater samples collected downgradient from a former municipal solid waste landfill near Berlin, Germany, were analyzed by GC-MS, HPLC-MS, and HPLC-NMR hyphenated techniques to comprehensively characterize the xenobiotic organic compounds (XOCs). The focus thereby was on the detection and identification of the polar XOCs which were analyzed in the extract obtained after separation of the unpolar components by pre-extraction. HPLC-NMR and HPLC-MS runs were used to identify polar XOCs on-line or to obtain preliminary structure information on the other XOCs. These compounds were then isolated by HPLC fractionation and their structures elucidated by off-line NMR and MS investigations. A variety of polar XOCs, products of the dye industry, degradation products of polyethylene glycol, and some heterocyclic compounds could be identified. Furthermore, a semi-quantitative estimation of the identified polar compounds is given.

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Separations coupled with NMR detection

Cited by 35 publications

References 31 publications

Analysis of highly polar compounds in groundwater samples from ammunition waste sites. Part I—Characterization of the pollutant spectrum

Analysis of highly polar compounds in groundwater samples from ammunition waste sites. Part I—Characterization of the pollutant spectrum

A comparison of capillary‐scale LC–NMR with alternative techniques: spectroscopic and practical considerations

A new analytical approach for the comprehensive characterization of polar xenobiotic organic compounds downgradient of old municipal solid waste (MSW) landfills

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