A novel stop-flow two-dimensional liquid chromatography–mass spectrometry method for lipid analysis

Wang, Shuangyuan; Li, Jia; Shi, Xianzhe; Qiao, Lizhen; Lü, Xin; Xu, Guowang

doi:10.1016/j.chroma.2013.10.069

Cited by 57 publications

(34 citation statements)

References 33 publications

(35 reference statements)

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“…Considering that, typically, current ESI-MS systems offer only 3–4 orders of magnitude linear dynamic range, it is obvious that, for quantitative methods covering a broad range of lipid classes/ species and concentrations in biological samples, a compromise has to be made with respect to number of detected lipids and the linear dynamic range of the method, unavoidably leading to a lower number of detected and identified lipids compared to qualitative methods where, usually, more concentrated extracts are injected. Specifically, those few studies where the number of annotated/ identified lipids exceeded 350 species were focused mainly on in-depth characterization of lipid extracts [32,38,49,57–60], while only 50–300 annotated lipid species were reported when quantification was mentioned as major aim in studies. A deeper examination of particular lipid classes showed that LC-MS-based lipidomics methods most frequently covered phosphatidylcho-lines, followed by other phospholipids (phosphatidylethanolamines, phosphatidylinositols, phosphatidylserines, phosphatidylglycerols), sphingomyelins, di- and tri-acylglycerols, and ceramides (Fig.…”

Section: Lipid Identification and Automated Annotationmentioning

confidence: 99%

Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry

Čajka

Fiehn

2014

TrAC Trends in Analytical Chemistry

519

439

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Liquid chromatography-mass spectrometry (LC-MS)-based lipidomics has been a subject of dramatic developments over the past decade. This review focuses on state of the art in LC-MS-based lipidomics, covering all the steps of global lipidomic profiling. On the basis of review of 185 original papers and application notes, we can conclude that typical LC-MS-based lipidomics methods involve: (1) extraction using chloroform/MeOH or MTBE/MeOH protocols, both with addition of internal standards covering each lipid class; (2) separation of lipids using short microbore columns with sub-2-μm or 2.6–2.8-μm (fused-core) particle size with C18 or C8 sorbent with analysis time <30 min; (3) electrospray ionization in positive- and negative-ion modes with full spectra acquisition using high-resolution MS with capability to MS/MS. Phospholipids (phosphatidylcholines, phosphatidylethanolamines, phosphatidylinositols, phosphatidylserines, phosphatidylglycerols) followed by sphingomyelins, di- and tri-acylglycerols, and ceramides were the most frequently targeted lipid species.

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Section: Lipid Identification and Automated Annotationmentioning

confidence: 99%

Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry

Čajka

Fiehn

2014

TrAC Trends in Analytical Chemistry

519

439

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“…The peak capacity of this stop-flow 2D LC method was calculated using a previous reported method [19]. Generally speaking, the total peak capacity (n c,t ) equals the sum of the peak capacity of each fraction in the second dimension.…”

Section: Peak Capacity and Orthogonality Of The Stop-flow 2d Lc Methodsmentioning

confidence: 99%

“…Procedure for on-line stop-flow 2D LC analysis An on-line stop-flow 2D LC approach (as described in our previous work [19]) was employed to analyze triterpenoid saponins. The specific scheme is presented in Fig.…”

Section: Instrumentation and Conditionsmentioning

confidence: 99%

On-line stop-flow two-dimensional liquid chromatography–mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract

et al. 2014

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A method based on stop-flow two-dimensional liquid chromatography coupled with electrospray ionization mass spectrometry (2D LC-ESI MS) was established and applied to analyze triterpenoid saponins from the main root of ginseng. Due to the special structure of triterpenoid saponins (they contain polar sugar side chains and nonpolar aglycones), hydrophilic interaction chromatography (HILIC) and reversed-phase liquid chromatography (RPLC) were used for the two dimensions, respectively. A trap column was used to connect the two dimensions. The dilution effect, which is one of the main shortcomings of traditional comprehensive 2D LC methods, was largely avoided. The peak capacity of this system was 747 and the orthogonality was 56.6 %. Compared with one-dimensional HILIC or RP LC MS analysis, 257 and 185 % more mass spectral peaks (ions with intensities that were higher than 1,000) were obtained from the ginseng main root extracts, and 94 triterpenoid saponins were identified based on MS(n) information and summarized aglycone structures. Given its good linearity and repeatability, the established method was successfully applied to classify ginsengs of different ages (i.e., years of growth), and 19 triterpenoid saponins were found through statistical analysis to vary in concentration depending on the age of the ginseng.

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“…Although the stop-flow mode seems to be convenient to increase 2 TG [39][40][41], it is time consuming [40] even with UHPLC conditions in the 2 D [41,42], and, in addition, it requires additional hardware. Moreover, axial dispersion may be a critical issue, particularly for the most retained compounds, thereby leading to significant peak band broadening [8].…”

Section: The Quest For Large Separation Power In On-line Lc X Lc Applmentioning

confidence: 99%

Theoretical and practical interest in UHPLC technology for 2D-LC

Sarrut

Crétier

Heinisch

2014

TrAC Trends in Analytical Chemistry

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A novel stop-flow two-dimensional liquid chromatography–mass spectrometry method for lipid analysis

Cited by 57 publications

References 33 publications

Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry

Comprehensive analysis of lipids in biological systems by liquid chromatography-mass spectrometry

On-line stop-flow two-dimensional liquid chromatography–mass spectrometry method for the separation and identification of triterpenoid saponins from ginseng extract

Theoretical and practical interest in UHPLC technology for 2D-LC

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