Small molecule matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry using a polymer matrix

Soltzberg, Leonard J.; Patel, Pina

doi:10.1002/rcm.1505

Cited by 46 publications

(36 citation statements)

References 12 publications

(13 reference statements)

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“…T he special advantages of matrix assisted laser desorption ionization time of flight (MALDI-TOF) mass spectrometry have been applied principally to large molecules, such as synthetic polymers, proteins, and nucleic acids. However, there have been some notable applications of this mass spectrometric method to small molecule analytes [1,2]. Simplicity of sample preparation, rapid spectrum acquisition, high sensitivity, and relative tolerance to impurities make MALDI-TOF attractive here.…”

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MALDI-TOF mass spectrometric identification of dyes and pigments

Soltzberg

Hagar

Kridaratikorn

et al. 2007

J. Am. Soc. Mass Spectrom.

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We have used MALDI-TOF mass spectrometry to characterize a selection of dyes from the Schweppe dye collection and pigments from the Tate Gallery collection. MALDI-TOF mass spectra of such samples are easily obtained and, through observation of both positive and negative ion spectra, provide a convenient, versatile method for dye characterization and identification. Such pairs of positive and negative ion spectra immediately distinguish between acidic and basic dyes and provide the characteristic mass of either the molecular ion or a simply related fragment ion. This approach is especially useful in situations where very small amounts of analyte are available, as in museum research and forensic analysis. In the case of textile dyes, we have carried out identification on material from single fibers and, with insoluble pigments, have begun to identify components of historically important pastel sticks from submicrogram samples. T he special advantages of matrix assisted laser desorption ionization time of flight (MALDI-TOF) mass spectrometry have been applied principally to large molecules, such as synthetic polymers, proteins, and nucleic acids. However, there have been some notable applications of this mass spectrometric method to small molecule analytes [1,2]. Simplicity of sample preparation, rapid spectrum acquisition, high sensitivity, and relative tolerance to impurities make MALDI-TOF attractive here. Direct laser desorption ionization (LDI) mass spectrometry, with no matrix, has also been explored for the investigation of inks and dyes [3,4].We assess here the utility of MALDI-TOF mass spectrometry for the identification of dyes and pigments from standard collections; the molecular masses of these substances are in the 200 to 1100 Da range. Application of the new solvent-free vortex grinding method for sample preparation [5,6] is well suited for the small sample sizes available in this work and is also assessed. Experimental Sample PreparationWe have utilized both a traditional overlay method and the new solvent-free vortex grinding method. In the overlay method, 4 L of a saturated methanol solution of 9-aminoacridine (9AA) matrix (Aldrich S517216) was deposited on the stainless steel target and allowed to air dry. One L of methanolic dye solution from the Schweppe collection [7] was then applied near the edge of the matrix spot.For the solvent-free method of Hanton and Parees [5], the sample and matrix were intimately ground in a 4 mL glass vial containing two 4.5 mm diameter zinc-plated steel balls using a vortex mixer. For dyes, we applied 1 L of the dye solution to about 15 mg of dry 9AA matrix in the vial, evaporated the methanol under vacuum, scraped the vial walls with a spatula to free the solid deposit, and proceeded with the vortex grinding. For insoluble pigments, about 15 mg of 9AA matrix was added to a microcentrifuge tube containing a barely visible amount of pigment dust (ϳ0.5 g) and mixed with a spatula; this mixture was then transferred to the 4 mL glass vial with the metal balls for vorte...

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“…However, there have been some notable applications of this mass spectrometric method to small molecule analytes [1,2]. Simplicity of sample preparation, rapid spectrum acquisition, high sensitivity, and relative tolerance to impurities make MALDI-TOF attractive here.…”

mentioning

confidence: 99%

MALDI-TOF mass spectrometric identification of dyes and pigments

Soltzberg

Hagar

Kridaratikorn

et al. 2007

J. Am. Soc. Mass Spectrom.

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“…Several neutral organometallic ferrocene-type complexes as well as charged organic acids were also characterized using this method at the 50-pmol range [22]. Soltzberg and coworkers used similar, but larger, alkyl-substituted thiophene polymers for SALDI-MS of small aromatic complexes [23]. The sensitivity of this technique was limited to approximately 10 nmols, compared with attomole/femtomole sensitivity using typical MALDI matrices.…”

Section: Polymeric Materialsmentioning

confidence: 99%

Surface-assisted laser desorption/ionization mass spectrometry

Dattelbaum

Iyer

2006

Expert Review of Proteomics

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Laser desorption/ionization mass spectrometry (MS) is rapidly growing in popularity as an analytical characterization method in several fields. The technique shot to prominence using matrix-assisted desorption/ionization for large biomolecules (>700 Da), such as proteins, peptides and nucleic acids. However, because the matrix, which consists of small organic molecules, is also ionized, the technique is of limited use in the low-molecular-mass range (<700 Da). Recent advances in surface science have facilitated the development of matrix-free laser desorption/ionization MS approaches, which are referred to here as surface-assisted laser desorption/ionization (SALDI) MS. In contrast to traditional matrix-assisted techniques, the materials used for SALDI-MS are not ionized, which expands the usefulness of this technique to small-molecule analyses. This review discusses the current status of SALDI-MS as a standard analytical technique, with an emphasis on potential applications in proteomics.

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“…Therefore, the use of MALDI-TOF-MS has been limited to the analysis of low-mass analytes. As a consequence, many analysts and experts of MALDI-TOF-MS have made considerable efforts and approaches to overcome this problem [1][2][3][4][5].Cyclodextrins are cyclic oligosaccharides that have ␣-d-glucose units that are connected through (1¡4) linkages. The most common forms of cyclodextrin are ␣-, ␤-, and ␥-cyclodextrin (cyclomaltohexa-, hepta-, and octaoses), which contain six, seven, and eight glucose units, respectively.…”

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Using molecular recognition of β-cyclodextrin to determine molecular weights of low-molecular-weight explosives by MALDI-TOF mass spectrometry

Zhang

Shi

Bai

et al. 2006

J. Am. Soc. Mass Spectrom.

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This study presents a novel method for determining the molecular weights of low molecular weight (MW) energetic compounds through their complexes of ␤-cyclodextrin (␤-CD) and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) in a mass range of 500 to 1700 Da, avoiding matrix interference. The MWs of one composite explosive composed of 2,6-DNT, TNT, and RDX, one propellant with unknown components, and 14 single-compound explosives (RDX, HMX, 3,4-DNT, 2,6-DNT, 2,5-DNT, 2,4,6-TNT, TNAZ, DNI, BTTN, NG, TO, NTO, NP, and 662) were measured. The molecular recognition and inclusion behavior of ␤-CD to energetic materials (EMs) were investigated. The results show that (1) the established method is sensitive, simple, accurate, and suitable for determining the MWs of low-MW single-compound explosives and energetic components in composite explosives and propellants; and (2) ␤-CD has good inclusion and modular recognition abilities to the above EMs. has become a powerful instrument for analyzing large synthetic polymers and biomacromolecules. However, for low-mass analytes-especially compounds that have a mass-to-charge of less than 500 Da-it has been a challenge. Because most of the molecular weights (MWs) of the currently used matrixes are less than 500 Da and because, during laser irradiation, they also act as their own matrixes, a variety of matrix-related ions are produced. Therefore, the use of MALDI-TOF-MS has been limited to the analysis of low-mass analytes. As a consequence, many analysts and experts of MALDI-TOF-MS have made considerable efforts and approaches to overcome this problem [1][2][3][4][5].Cyclodextrins are cyclic oligosaccharides that have ␣-d-glucose units that are connected through (1¡4) linkages. The most common forms of cyclodextrin are ␣-, ␤-, and ␥-cyclodextrin (cyclomaltohexa-, hepta-, and octaoses), which contain six, seven, and eight glucose units, respectively. The structures of these molecules are toroidal, containing an apolar cavity with primary hydroxyl groups lying on the outside and the secondary hydroxyl groups being located inside [6,7]. The guest molecules that have a suitable size and shape can be incorporated into the cyclodextrin cavity to form inclusion complexes. The formation of these complexes has been attributed to weak interactions, including van der Waals interactions, hydrophobic effects, and hydrogen bonding. The ability of cyclodextrins to form inclusion complexes with a variety of guest molecules has attracted widespread interest in academic research and industrial applications. Cyclodextrin complexes have been studied by using different physical methods and spectroscopic methods. However, the analysis of low-mass analytes by MALDI-TOF-MS, especially those in the mass range below 500 Da, has been a major challenge [8 -15].In this paper, a novel method of using the molecular recognition of ␤-cyclodextrin (␤-CD) to determine the mass of low-MW explosives by MALDI-TOF-MS is established.

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Small molecule matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry using a polymer matrix

Cited by 46 publications

References 12 publications

MALDI-TOF mass spectrometric identification of dyes and pigments

MALDI-TOF mass spectrometric identification of dyes and pigments

Surface-assisted laser desorption/ionization mass spectrometry

Using molecular recognition of β-cyclodextrin to determine molecular weights of low-molecular-weight explosives by MALDI-TOF mass spectrometry

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