Thin-layer chromatography–matrix-assisted laser desorption ionisation–time-of-flight mass spectrometry using particle suspension matrices

Crecelius, Anna C.; Clench, Malcolm R.; Richards, Donald St. P.; Parr, Vic

doi:10.1016/s0021-9673(02)00391-6

Cited by 66 publications

(55 citation statements)

References 25 publications

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“…The direct coupling described previously has been implemented on axial MALDI-TOF mass spectrometers, [30][31][32][33], showing the feasibility of this method. However, axial MALDI-TOF instruments require a flat surface for sample desorption to achieve optimum resolving power and mass accuracy results.…”

mentioning

confidence: 98%

Ganglioside analysis by thin-layer chromatography matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry

Ivleva

Sapp

O’Connor

et al. 2005

J. Am. Soc. Mass Spectrom.

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Metastable decomposition of ions generated in matrix-assisted laser desorption/ionization (MALDI) mass spectrometers complicates analysis of biological samples that have labile bonds. Recently, several academic laboratories and manufacturers of commercial instruments have designed instruments that introduce a cooling gas into the ion source during the MALDI event and have shown that the resulting vibrational cooling stabilizes these labile bonds. In this study, we compared stabilization and detection of desorbed gangliosides on a commercial orthogonal time-of-flight (oTOF) instrument with results we reported previously that had been obtained on a home-built Fourier transform mass spectrometer. Decoupling of the desorption/ ionization from the detection steps resulted in an opportunity for desorbing thin-layer chromatography (TLC)-separated gangliosides directly from a TLC plate without compromising mass spectral accuracy and resolution of the ganglioside analysis, thus coupling TLC and oTOF mass spectrometry. The application of a declustering potential allowed control of the matrix cluster and matrix adduct formation, and, thus, enhanced the detection of the gangliosides. during matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) analyses of molecules having labile bonds. Although this phenomenon can be used for obtaining analyte structural information for small peptides, oligosaccharides, and some glycolipids [1-5] for larger or more fragile molecules, it can limit the mass accuracy and resolution and complicate interpretation of the spectra of heterogeneous samples. Thus, it is important to develop methods that allow control of the extent of metastable decay. In addition to the pressure of the background gas and extraction field strength in the MALDI technique, the major factors affecting metastable fragmentation are laser wavelength/pulse width and the choice of the MALDI matrix [6,7]. In addition, the presence of electrons may play a role in analyte fragmentation and may cause suppression of multiply charged ions in a spectrum [8,9].Control of the metastable fragmentation in MALDI by increasing the pressure in the ionization source and reduction of the ions internal energy was first introduced by Loboda et al. on orthogonal time-of-flight (oTOF) instruments [10] and later extended to Fourier transform mass spectrometry (FTMS) [11] and to the operation at atmospheric pressure on various types of instruments [12]. These methods have since been used for stabilization of glycolipids [13,14] and peptides and proteins [11,15]. The term vibrational cooling (VC) MALDI recently has been introduced to describe desorption in the pressure range where cooling of the excess bond energy is achieved [12]. Stabilization of the labile bonds under these conditions allows for control of the extent of fragmentation, which is particularly

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confidence: 98%

Ganglioside analysis by thin-layer chromatography matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry

Ivleva

Sapp

O’Connor

et al. 2005

J. Am. Soc. Mass Spectrom.

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“…More recently, the use of ionic liquid matrices has become widespread 9 and the conditions required for the effective use of the matrix suppression effect (MSE) have been investigated. 10 The use of graphite as a matrix [11][12][13] and the utilisation of graphite target plates, without the addition of a standard crystalline matrix, 14 was discussed in our earlier publication, 15 where graphite powder and graphite rod were investigated as possible matrices for the analysis of actinides. Difficulties in handling and deposition of the graphite were highlighted and a simplified method utilising pencil lead (PL) as a new MALDI matrix was developed in this laboratory to address these problems.…”

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confidence: 99%

2B or not 2B, that is the question: further investigations into the use of pencil as a matrix for matrix‐assisted laser desorption/ionisation

Langley

Herniman

Townell

2006

Rapid Comm Mass Spectrometry

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The effective use of pencil as a matrix for matrix-assisted laser desorption/ionisation (MALDI) for the study of actinides has previously been demonstrated (Black et al., Rapid Commun. Mass Spectrom. 2006; 20: 1053). Here, the scope of the types of molecules amenable to analysis by this method has been extended, establishing that $90% of a library containing 50 diverse small molecules can be successfully analysed by this technique. Further, the role played by the bulk materials present in the different pencil leads has been investigated and a simple one-step deposition of matrix and calibration materials has been achieved through the fabrication of different calibration pencils (Cali-Pens).

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“…It is possible that the esters spread out as a result of adding the 2,6-DHB matrix solution because lateral spreading of analytes, caused by using a liquid matrix, has been observed. 10,17,31 However, no ester signal was observed at the edges of the sample spots unless coincident with the pencil line. This suggested that the pencil lead was in fact a more suitable matrix than 2,6-DHB.…”

Section: Resultsmentioning

confidence: 97%

“…Recently, TLC-MALDI has been used in analyses of peptides, 13 lipids, 14,15 oligosaccharides, 16 and medicines. 17 Additionally, matrix-free TLC-laser desorption/ionization (LDI) has been used in the analysis of alkaloids. 10 Among the various matrices available for MALDI analyses, 2,5-dihydroxybenzoic acid (2,5-DHB) is one of the most common for analyzing proteins, peptides, and polyethylene glycol derivatives.…”

Section: Introductionmentioning

confidence: 99%

“…Graphite particles have been used as a matrix material in TLC-MALDI analyses of tetracyclines. 17 Because powdered graphite is not easy to handle, pencil lead has recently been used as a new matrix material. 26,27 Pencil lead has also been used in the TLC separation and MALDI analysis of porphines, where a line was pre-drawn with a pencil on the TLC plate where the sample was separated, followed by laser irradiation on the pencil line to obtain mass spectra.…”

Section: Introductionmentioning

confidence: 99%

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Detection of Long Alkyl Esters of Succinic and Maleic Acid Using TLC-MALDI-MS

Kim¹,

Han²,

Kim³

et al. 2011

Bulletin of the Korean Chemical Society

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Four esters of succinic and maleic acid were synthesized, separated by thin-layer chromatography (TLC), and identified using matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS). A comparison of matrix materials showed that 2,6-dihydroxybenzoic acid (2,6-DHB) yielded a greater ionization efficiency than 2,5-DHB prior to TLC separation. The location of each ester sample on the TLC plate was estimated by comparing the developed plate with a duplicate plate that had been visualized by immersion in a KMnO4 solution. Generally, mass spectra obtained from the KMnO4-visualized plate were relatively poor. Reproducible mass spectra with high peak abundance were difficult to obtain using the 2,6-DHB matrix from crude synthetic esters extracted from the TLC plates. Significant improvements in both reproducibility and sensitivity were realized by using pencil lead as the MALDI matrix. The current methodology will be beneficial to organic chemists since it can provide a guideline for simple and rapid characterization of small organic compounds.

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Thin-layer chromatography–matrix-assisted laser desorption ionisation–time-of-flight mass spectrometry using particle suspension matrices

Cited by 66 publications

References 25 publications

Ganglioside analysis by thin-layer chromatography matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry

Ganglioside analysis by thin-layer chromatography matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry

2B or not 2B, that is the question: further investigations into the use of pencil as a matrix for matrix‐assisted laser desorption/ionisation

Detection of Long Alkyl Esters of Succinic and Maleic Acid Using TLC-MALDI-MS

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