Desorption electrospray ionization (DESI) mass spectrometry and tandem mass spectrometry (MS/MS) of phospholipids and sphingolipids: Ionization, adduct formation, and fragmentation

Manicke, Nicholas E.; Wiseman, Justin M.; Ifa, Demian R.; Cooks, R. Graham

doi:10.1016/j.jasms.2007.12.003

Cited by 162 publications

(143 citation statements)

References 51 publications

(35 reference statements)

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“…Owing to its ability to readily desorb and ionize lipids from a variety of surfaces including glass, poly(methyl methacrylate) and polytetrafluoroethylene (PTFE) [182], tissue sections [20] and silica TLC plates [183,184], lipid analysis has become one of the most popular applications of DESI. Early studies focused on optimization of solvent composition and surface structure to enhance the sensitivity of lipid detection from standards and extracts [182].…”

Section: Desorption Electrospray Ionization (Desi)mentioning

confidence: 99%

Surface analysis of lipids by mass spectrometry: More than just imaging

Ellis

Brown

Panhuis

et al. 2013

Progress in Lipid Research

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Mass spectrometry is now an indispensable tool for lipid analysis and is arguably the driving force in the renaissance of lipid research. In its various forms, mass spectrometry is uniquely capable of resolving the extensive compositional and structural diversity of lipids in biological systems. Furthermore, it provides the ability to accurately quantify molecular-level changes in lipid populations associated with changes in metabolism and environment; bringing lipid science to the "omics" age. The recent explosion of mass spectrometry-based surface analysis techniques is fuelling further expansion of the lipidomics field. This is evidenced by the numerous papers published on the subject of mass spectrometric imaging of lipids in recent years. While imaging mass spectrometry provides new and exciting possibilities, it is but one of the many opportunities direct surface analysis offers the lipid researcher. In this review we describe the current state-ofthe-art in the direct surface analysis of lipids with a focus on tissue sections, intact cells and thin-layer chromatography substrates. The suitability of these different approaches towards analysis of the major lipid classes along with their current and potential applications in the field of lipid analysis are evaluated. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 2 AbstractMass spectrometry is now an indispensable tool for lipid analysis and is arguably the driving force in the renaissance of lipid research. In its various forms, mass spectrometry is uniquely capable of resolving the extensive compositional and structural diversity of lipids in biological systems. Furthermore, it provides the ability to accurately quantify molecular-level changes in lipid populations associated with changes in metabolism and environment;bringing lipid science to the "omics" age. The recent explosion of mass spectrometry-based surface analysis techniques is fuelling further expansion of the lipidomics field. This is evidenced by the numerous papers published on the subject of mass spectrometric imaging of lipids in recent years. While imaging mass spectrometry provides new and exciting possibilities, it is but one of the many opportunities direct surface analysis offers the lipid researcher. In this review we describe the current state-of-the-art in the direct surface analysis of lipids with a focus on tissue sections, intact cells and thin-layer chromatography substrates.The suitability of these different approaches towards analysis of the major lipid classes along with their current and potential applications in the field of lip...

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Section: Desorption Electrospray Ionization (Desi)mentioning

confidence: 99%

Surface analysis of lipids by mass spectrometry: More than just imaging

Ellis

Brown

Panhuis

et al. 2013

Progress in Lipid Research

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“…Sulfatides differ from the lipids discussed thus far in that they do not contain a glycerol-phosphate backbone but instead possess a sphingosine base (Scheme 1). Sulfatide fragmentation described in the literature shows several complex processes [93,102,103] Table 1. These data are consistent with previously reported MS analysis of rat brain sections [45,80,89].…”

Section: Identification Of Compoundsmentioning

confidence: 99%

“…Only the most intense peaks for each class of lipids have been annotated for clarity, but the mass spectrum in Figure 3 is dominated by PC species. MS/MS experiments were also performed on the tissue samples and compared to published fragmentation [93,94,104] to identify the lipids detected in the full scan mass spectra, as well as accurate mass measurements on the DESI-Orbitrap (see Figure S1 in the Supplementary Material). Indeed, based on its fragmentation behavior, the ion detected at m/z 782.8 in the MS spectrum (m/z 782.5704, error: ϩ4.5 ppm on the DESI-Orbitrap) has been identified as [PC (16: Table 2.…”

Section: Identification Of Compoundsmentioning

confidence: 99%

“…Reported MS studies of rat brain tissues have also yielded strong mass peaks associated with PC in positive ion mode [43,44,93,112]. Although glycerophosphocholines (PC) and glycerophosphoethanolamines (PE) have similar concentrations in rat spinal cords [21], the relative abundances of the PE species are weak compared to PC in the positive mass spectra.…”

Section: Identification Of Compoundsmentioning

confidence: 99%

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Desorption electrospray ionization imaging mass spectrometry of lipids in rat spinal cord

Girod

Shi

Cheng

et al. 2010

J. Am. Soc. Mass Spectrom.

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Imaging mass spectrometry allows for the direct investigation of tissue samples to identify specific biological compounds and determine their spatial distributions. Desorption electrospray ionization (DESI) mass spectrometry has been used for the imaging and analysis of rat spinal cord cross sections. Glycerophospholipids and sphingolipids, as well as fatty acids, were detected in both the negative and positive ion modes and identified through tandem mass spectrometry (MS/MS) product ion scans using collision-induced dissociation and accurate mass measurements. Differences in the relative abundances of lipids and free fatty acids were present between white and gray matter areas in both the negative and positive ion modes. DESI-MS images of the corresponding ions allow the determination of their spatial distributions within a cross section of the rat spinal cord, by scanning the DESI probe across the entire sample surface. Glycerophospholipids and sphingolipids were mostly detected in the white matter, while the free fatty acids were present in the gray matter. These results show parallels with reported distributions of lipids in studies of rat brain. This suggests that the spatial intensity distribution reflects relative concentration differences of the lipid and fatty acid compounds in the spinal cord tissue. The "butterfly" shape of the gray matter in the spinal cord cross section was resolved in the corresponding ion images, indicating that a lateral resolution of better than 200 m was achieved. The selected ion images of lipids are directly correlated with anatomic features on the spinal cord corresponding to the white and the gray

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“…To explore this application, we procured custom-made PTFE printed glass slides in a 96-sample format (Figure 1). This PTFE printed glass substrate has been shown to be an effective and versatile surface for DESI that gives strong, stable signal for a wide array of analytes [18,20]. This system offers several advantages.…”

mentioning

confidence: 99%

High-throughput quantitative analysis by desorption electrospray ionization mass spectrometry

Manicke

Kistler

Ifa

et al. 2009

J. Am. Soc. Mass Spectrom.

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A newly developed high-throughput desorption electrospray ionization (DESI) source was characterized in terms of its performance in quantitative analysis. A 96-sample array, containing pharmaceuticals in various matrices, was analyzed in a single run with a total analysis time of 3 min. These solution-phase samples were examined from a hydrophobic PTFE ink printed on glass. The quantitative accuracy, precision, and limit of detection (LOD) were characterized. Chemical background-free samples of propranolol (PRN) with PRN-d 7 as internal standard (IS) and carbamazepine (CBZ) with CBZ-d 10 as IS were examined. So were two other sample sets consisting of PRN/PRN-d 7 at varying concentration in a biological milieu of 10% urine or porcine brain total lipid extract, total lipid concentration 250 ng/ L. The background-free samples, examined in a total analysis time of 1.5 s/sample, showed good quantitative accuracy and precision, with a relative error (RE) and relative standard deviation (RSD) generally less than 3% and 5%, respectively. The samples in urine and the lipid extract required a longer analysis time (2.5 s/sample) and showed RSD values of around 10% for the samples in urine and 4% for the lipid extract samples and RE values of less than 3% for both sets. The LOD for PRN and CBZ when analyzed without chemical background was 10 and 30 fmol, respectively. The LOD of PRN increased to 400 fmol analyzed in 10% urine, and 200 fmol when analyzed in the brain lipid extract. (J Am Soc Mass Spectrom 2009, 20, 321-325) © 2009 Published by Elsevier Inc. on behalf of American Society for Mass Spectrometry Q uantitative analysis of pharmaceutical compounds in biological fluids is typically carried out using liquid chromatography separation combined with a mass spectrometer fitted with an atmospheric pressure ionization (API) ion source, usually electrospray ionization or atmospheric pressure chemical ionization (LC/ESI-MS or LC/APCI-MS). Such a system can analyze one sample for numerous components in a matter of a few minutes [1]. In most applications, the separation device is directly coupled on-line with the MS. In others, however, extensive prior separation is not necessary, and it can be replaced by a simpler extraction step. In these cases, current highthroughput approaches include direct injection of the sample solution into the MS from a 96-well sample plate for analysis by API [2], or the spotting of solid samples with an organic matrix for analysis by matrix-assisted laser desorption/ionization (MALDI) [3].New options for the ionization of samples at atmospheric pressure have emerged recently. The family of ambient ionization methods for mass spectrometry, which originated with desorption electrospray ionization (DESI) [4] and direct analysis in real time (DART) [5], has rapidly expanded to include a number of new members including MALDESI, LAESI, PADI, ASAP, DBDI, and ELDI [6 -11]. In DESI-MS, samples are analyzed by directing a pneumatically-assisted stream of charged microdroplets at the surface in the ambient...

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Desorption electrospray ionization (DESI) mass spectrometry and tandem mass spectrometry (MS/MS) of phospholipids and sphingolipids: Ionization, adduct formation, and fragmentation

Cited by 162 publications

References 51 publications

Surface analysis of lipids by mass spectrometry: More than just imaging

Surface analysis of lipids by mass spectrometry: More than just imaging

Desorption electrospray ionization imaging mass spectrometry of lipids in rat spinal cord

High-throughput quantitative analysis by desorption electrospray ionization mass spectrometry

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