Using 1.5 mm internal diameter columns for optimal compatibility with current liquid chromatographic systems

Fekete, Szabolcs; Murisier, Amarande; Losacco, Gioacchino Luca; Lawhorn, Jason; Godinho, Justin M.; Ritchie, Harry; Boyes, Barry E.; Guillarme, Davy

doi:10.1016/j.chroma.2021.462258

Cited by 11 publications

(5 citation statements)

References 12 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…columns will be explored as lower flow rates may make use of deuterated solvents affordable. 18 These steps will help improve the platform introduced here for merging NMR into LC−MS based lipidomics workflows.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…As for whether to use an aprotic solvent for the LC run so the eluent is directly compatible with NMR analysis, the benefits of using 1.5 mm i.d. columns will be explored as lower flow rates may make use of deuterated solvents affordable . These steps will help improve the platform introduced here for merging NMR into LC–MS based lipidomics workflows.…”

Section: Discussionmentioning

confidence: 99%

See 1 more Smart Citation

Segmented Flow Strategies for Integrating Liquid Chromatography–Mass Spectrometry with Nuclear Magnetic Resonance for Lipidomics

et al. 2023

View full text Add to dashboard Cite

Building an accurate lipid inventory relies on coordinated information from orthogonal analytical capabilities. Integrating the familiar workflow of liquid chromatography (LC), high-resolution mass spectrometry (HRMS), and tandem mass spectrometry (MS/MS) with proton nuclear magnetic resonance spectroscopy (1H NMR) would be ideal for building that inventory. For absolute lipid structural elucidation, LC–HRMS/MS can provide lower-level structural information with superior sensitivity, while 1H NMR can provide invaluable higher-order structural information for the disambiguation of isomers with absolute chemical specificity. Digitization of the LC eluent followed by splitting the microfractions into two flow paths in a defined ratio for HRMS/MS and NMR would be the ideal strategy to permit correlation of the MS and NMR data as a function of chromatographic retention time. Here, we report an active segmentation platform to transform analytical flow rate LC eluent into parallel microliter segmented flow queues for high confidence correlation of the MS, MS/MS, and NMR data. The practical details in implementing this strategy to achieve an integrated LC–MS–NMR platform are presented, including the development of an active segmentation technology using a four-port two-way valve to transform the LC eluent into parallel segmented flows for online MS analysis followed by offline segment-specific 1H NMR and optimization of the detector response toward segmented flow. To demonstrate the practicality of this novel platform, it was tested using lipid mixture samples.

show abstract

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Segmented Flow Strategies for Integrating Liquid Chromatography–Mass Spectrometry with Nuclear Magnetic Resonance for Lipidomics

et al. 2023

View full text Add to dashboard Cite

show abstract

“…columns packed with sub-2 μm particles have enhanced the detection of compounds in a complex sample while reducing both the time involved and solvent consumption without any loss in efficiency. 16,18,104,115 Even obtaining a metabolic profile of a complex crude extract, which often requires runs of 60 min or more and 150 mm-long columns, can be achieved while reducing the consumption of solvents, when compared to conventional HPLC analysis. 19,116 Unfortunately, the daily contact with toxic solvents by analysts and others, such as undergraduate students who may not be fully aware of the risks involved, has continued.…”

Section: ■ a Survey On The Most Accessed Solvents In Phytochemistry O...mentioning

confidence: 99%

“…It is estimated that 26,000,000–52,000,000 L of chemical waste, mostly containing organic solvents, is produced every year by HPLC procedures . The reduction and replacement of these organic solvents should be the focus in LC method development. ,,− A reduction in the consumption of solvents in analytical chromatography has been adopted due to miniaturization of extraction and separation/identification systems. , For example, high-field NMR spectroscopy equipped with cryoprobes has been developed to allow complete 2D measurements from sub-milligram quantities of the metabolite under identification. High-resolution MS analyzers, such as time-of-flight or Q-orbitrap, also became available and can detect a picogram or a femtogram of a compound, respectively, depending on their ionization efficiency in the ionization source.…”

Section: Other Current Approaches To the Use Of Green Chemistry Princ...mentioning

confidence: 99%

“…Furthermore, powerful UHPLC instruments and small i.d. columns packed with sub-2 μm particles have enhanced the detection of compounds in a complex sample while reducing both the time involved and solvent consumption without any loss in efficiency. ,,, Even obtaining a metabolic profile of a complex crude extract, which often requires runs of 60 min or more and 150 mm-long columns, can be achieved while reducing the consumption of solvents, when compared to conventional HPLC analysis. , …”

Section: Other Current Approaches To the Use Of Green Chemistry Princ...mentioning

confidence: 99%

See 1 more Smart Citation

Reaction of the Phytochemistry Community to Green Chemistry: Insights Obtained Since 1990

et al. 2023

View full text Add to dashboard Cite

This review article aims to study how phytochemists have reacted to green chemistry insights since 1990, the year when the U.S. Environmental Protection Agency launched the “Pollution Prevention Act”. For each year in the period 1990 to 2019, three highly cited phytochemistry papers that provided enough information about the experimental procedures utilized were sampled. The “greenness” of these procedures was assessed, particularly for the use of solvents. The highly hazardous diethyl ether, benzene, and carbon tetrachloride did not appear in the papers sampled after 2010. Advances in terms of sustainability were observed mainly in the extraction stage. Similar progress was not observed in purification procedures, where chloroform, dichloromethane, and hexane regularly have been employed. Since replacing such solvents in purification procedures should be a major goal, potential alternative approaches are discussed. Moreover, some current initiatives toward a more sustainable phytochemical research considering aspects other than only solvents are highlighted. Although some advances have been achieved, it is believed that natural products chemists can play a major role in developing a novel ecological paradigm in chemistry. To contribute to this objective, six principles for performing natural products chemistry consistent with the guidelines of green chemistry are proposed.

show abstract

Influence of the Column Inner Diameter on Chromatographic Efficiency in Miniaturized and Conventional Ultra-High-Performance Liquid Chromatography

2023

View full text Add to dashboard Cite

Using 1.5 mm internal diameter columns for optimal compatibility with current liquid chromatographic systems

Cited by 11 publications

References 12 publications

Segmented Flow Strategies for Integrating Liquid Chromatography–Mass Spectrometry with Nuclear Magnetic Resonance for Lipidomics

Segmented Flow Strategies for Integrating Liquid Chromatography–Mass Spectrometry with Nuclear Magnetic Resonance for Lipidomics

Reaction of the Phytochemistry Community to Green Chemistry: Insights Obtained Since 1990

Influence of the Column Inner Diameter on Chromatographic Efficiency in Miniaturized and Conventional Ultra-High-Performance Liquid Chromatography

Contact Info

Product

Resources

About