Enrichment procedure based on graphitized carbon black and liquid chromatography-high resolution mass spectrometry for elucidating sulfolipids composition of microalgae

Antonelli, Michela; Benedetti, Bárbara; Cavaliere, Chiara; Cerrato, Andrea; Barbera, Giorgia La; Montone, Carmela Maria; Piovesana, Susy; Laganà, Aldo

doi:10.1016/j.talanta.2019.120162

Cited by 15 publications

(13 citation statements)

References 30 publications

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“…83%, C. vulgaris 95.8%, basil 89.5%, spinach 88%). So far there is only one publication on a semi-quantitative determination of single SQDGs in Arthrospira sp., described by Antonelli et al [24]. They achieved a comparatively better LOQ (0.41 μg/ mL), but almost similar recovery rates (89-110%), and presented a similar range for linearity of the external calibration (0.75-12.5 μg/mL).…”

Section: Methods Validationmentioning

confidence: 65%

“…Chloroform and methanol in different compositions are still the traditional solvent systems, which are used to extract lipids from different tissues [32,33]. More actual methods often rely on these older extraction methods [24,26]. Therefore, the result that chloroform/methanol is (still) the best system to extract different lipid classes in high amounts is not surprising.…”

Section: Sample Preparationmentioning

confidence: 99%

“…It was further determined by CID-MS/MS that the fragment resulting from the fragmentation of the sn1 fatty acid shows a higher intensity, and thus, the regiochemistry of the glycerol backbone of the SQDG can be inferred [21]. Recent studies have focused on the identification of new SQMGs and SQDGs using lipodomic approaches [24][25][26]. Nonetheless, there is actually no method for quantifying multiple intact SQMGs and SQDGs for evaluating phytochemical or food chemical questions.…”

Section: Introductionmentioning

confidence: 99%

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Development of a targeted HPLC-ESI-QqQ-MS/MS method for the quantification of sulfolipids from a cyanobacterium, selected leafy vegetables, and a microalgae species

Fischer¹,

Treblin²,

Sitz³

et al. 2021

Anal Bioanal Chem

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The use of macro- and microalgae, as well as cyanobacteria, becomes increasingly important for human nutrition, even in Western diets. Health effects, positive as well as negative, are believed to result mainly from minor components in the food. In macro- and microalgae as well as in certain cyanobacteria, one class of such minor compounds is sulfolipids, more precisely sulfoquinovosylmonoacylglycerol (SQMG) and sulfoquinovosyldiacylglycerol (SQDG) derivatives. SQMGs and SQDGs consist of a diacylglycerol esterified with varying fatty acid combinations and a sulfoquinovose moiety. Sulfoquinovose is a sulfonated hexose analogous to d-glucose, but featuring a stable carbon-sulfur bond. With regard to their chemical structure, SQDGs can be distinguished according to their sn1- and sn2-bound fatty acids. Although there is great interest in SQDGs, because of their controversially discussed bioactivities, only a negligible number of comprehensive methods for identification and quantification has been published, so far. Within this work, a sample preparation including a quantitative isolation of SQDGs from selected raw materials, a clean-up with solid-phase extraction (SPE), and a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for simultaneous identification and quantitation of different, intact SQMGs and SQDGs were developed and validated. The applicability of the method was further demonstrated by comparing a prominent cyanobacterium (Arthrospira sp.) with a microalgae preparation (Chlorella vulgaris), and selected leafy vegetables (spinach, basil).

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Section: Methods Validationmentioning

confidence: 65%

Section: Sample Preparationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Development of a targeted HPLC-ESI-QqQ-MS/MS method for the quantification of sulfolipids from a cyanobacterium, selected leafy vegetables, and a microalgae species

Fischer¹,

Treblin²,

Sitz³

et al. 2021

Anal Bioanal Chem

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“…Accurate m/z ratios extracted from averaged HILIC-ESI-FTMS spectra in the range between 750 and 850 m/z Online Lipid Calculator were used as input values on the freely available (http://www.mslipidomics.info/lipid-calc/) using a tolerance of ±0.005 m/z and only those values matching with supposed identities, reporting a mass accuracy lower than 5 ppm, were accepted. Since major glycolipids and phospholipids were discussed earlier [1,[5][6][7]16,27,28] relevant attention was given to IPC of spirulina lipid extracts. A snapshot about the composition of IPC class was obtained looking at the MS spectrum ( Fig.…”

Section: Characterization Of Ipc In Sample Extracts Of Spirulina Micrmentioning

confidence: 99%

“…Among high levels of vitamins (A, B, and E), spirulina microalgae contain significant quantity of lipids including monogalactosyldiacyl-glycerols (MGDG), digalactosyldiacylglycerols (DGDG), sulfoquinovosyldiacylglycerols (SQDG), and phospholipids as phosphatidylglycerols (PG) [1]. More recent investigations of the lipid portion of this cyanobacterium focused on the profile of fatty acids being linolenic acid (18:3) the most prevailing [2][3][4] and confirmed the presence of SQDG [5,6], DGDG, and PG as for similar cyanobacteria [7]. Once deemed obscure minor components of biological membranes, inositolphosphoceramides (IPC) are now known to be involved in important cellular processes including differentiation, growth, and apoptosis [8], yet weakly described in cyanobacteria including spirulina microalgae.…”

Section: Introductionmentioning

confidence: 99%

The occurrence of inositolphosphoceramides in spirulina microalgae

et al. 2020

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Spirulina microalga (Arthrospira platensis) is an interesting phototrophic organism because of its high content of nutrients including proteins, lipids, essential amino acids, antioxidants, vitamins, polysaccharides, and minerals. Hydrophilic interaction liquid chromatography (HILIC) coupled to linear ion trap (LIT) and Orbitrap Fourier transform mass spectrometry (FTMS) via ESI was employed for the separation and characterization of lipid species in A. platensis. Inositolphosphoceramides (IPC) are minor but important constituents of spirulina; their investigation was accomplished by HILIC-ESI-MS including collision-induced dissociation (MS 2 , MS 3) of deprotonated molecules in the LIT analyzer and a schematic fragmentation pattern is described. All four commercial spirulina samples revealed the occurrence of the same IPC species at m/z 796.6 (d18:0/16:0;1), 810.6 (d18:0/17:0;1), 824.6 (d18:0/18:0;1), and 826.6 (d18:0/17:0;2) but in diverse relative abundance. This study sets the stage for future investigations on IPC in other algae and microalgae.

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Single‐filament imaging mass spectrometry lipidomics in Arthrospira platensis

Lesco

Rowland

Williams

et al. 2023

Rapid Comm Mass Spectrometry

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Rationale: Elucidating intra-organismal biochemical and lipid organization in photosynthetic biological cell factories of filamentous cyanobacteria, such as Arthrospira platensis (Spirulina), is important for tracking physiological response mechanisms during growth. Little is known about the filaments' biochemical organization and cellular structure and no label-free imaging techniques exist that provide molecular mapping.Methods: We applied ultrahigh-resolution mass spectrometry (MS) with matrixassisted laser desorption ionization (MALDI) imaging to immobilized Spirulina filaments to investigate the localization of lipids across distinct physiological regions.We optimized matrix selection and deposition methods with the goal of facilitating high spatial, and intra-filament, resolution using untargeted multivariate statistical spectral deconvolution across MS pixels.Results: Our results demonstrate an improved two-step matrix application with an optimized procedure for intra-organismal lipid profiling to improve analyte sensitivity and achieve higher spatial resolution. We evaluate several conventional matrices, namely 2,5-dihydroxybenzoic acid (DHB), superDHB (sDHB), 1,5-diaminonaphthalene (DAN), and a 50:50 mix of DHB and sDHB, and compare delineation and pixel-based elucidation of intra-filament lipidomics. We identified a total of 1626 features that could be putatively assigned a lipid-like formula based on database query and 46 unique features, with associated lipid assignments that were significantly distinct in their intra-filament location.Conclusions: MALDI imaging MS with untargeted statistical spectral deconvolution was used to visualize intra-filament lipidomics organization in Spirulina filaments.Improvements in matrix deposition, including sequential sublimation and pneumatic spraying, increased signal abundance at high spatial resolution and allowed for identification of distinct lipid composition regions. This work outlines a methodology that may be used for micro-ecological untargeted molecular phenotyping.

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Enrichment procedure based on graphitized carbon black and liquid chromatography-high resolution mass spectrometry for elucidating sulfolipids composition of microalgae

Cited by 15 publications

References 30 publications

Development of a targeted HPLC-ESI-QqQ-MS/MS method for the quantification of sulfolipids from a cyanobacterium, selected leafy vegetables, and a microalgae species

Development of a targeted HPLC-ESI-QqQ-MS/MS method for the quantification of sulfolipids from a cyanobacterium, selected leafy vegetables, and a microalgae species

The occurrence of inositolphosphoceramides in spirulina microalgae

Single‐filament imaging mass spectrometry lipidomics in Arthrospira platensis

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