Liquid Sampling-Atmospheric Pressure Glow Discharge Ionization as a Technique for the Characterization of Salt-Containing Organic Samples.

Typical ionization techniques used for mass spectrometry (MS) analysis face challenges when trying to analyze organic species in a high-salt environment. Here, we present results using a recently developed ionization source, liquid sampling-atmospheric pressure glow discharge (LS-APGD), for marine-relevant salt-containing organic samples. Using two representative sample types, a triglyceride mixture and dissolved organic matter, this method is compared to traditional electrospray ionization (ESI) under saline and neat conditions.

Matrix-assisted ionization Fourier transform mass spectrometry for the analysis of lipids.

Rationale: Assessing the utility of vacuum matrix-assisted ionization (MAI) for the direct and rapid analysis of lipids in complex samples with emphasis on bacterial taxonomy.

Methods: Matrix-assisted ionization Fourier transform mass spectrometry (MAI-FTMS) was used to characterize polar and non-polar lipids in mixtures.

Results: For non-polar lipid triacylglycerols (TAGs), MAI-FTMS produced lipid-specific ions for eight different edible oils and allowed these oils to be identified based on their MAI-FTMS profiles.

Matrix-assisted ionization vacuum for high-resolution Fourier transform ion cyclotron resonance mass spectrometers.

Matrix-assisted ionization vacuum (MAIV) produces charge states similar to electrospray ionization (ESI) from the solid state without requiring high voltage or added heat. MAIV differs from matrix-assisted laser desorption/ionization (MALDI) in that no laser is needed and abundant multiply charged ions are produced from molecules having multiple basic sites such as proteins. Here we introduce simple modifications to the commercial vacuum MALDI and ESI sources of a 9.

New structural insights into mechanically interlocked polymers revealed by ion mobility mass spectrometry.

Mechanically interlocked polymers can possess significant additional physical properties, in comparison to those associated with their constituent parts. Their unique properties make them attractive for a range of potential applications, such as as biomaterials and molecular machines. Their efficient and reproducible synthesis is therefore of much interest.

Growth mechanisms involved in the synthesis of smooth and microtextured films by acetylene magnetron discharges.

The growth of hydrogenated amorphous carbons (a-C:H) produced by continuous or pulsed discharges of acetylene (C(2)H(2)) in an unbalanced magnetron setup was investigated. At 5 × 10(-3) Torr, only smooth films are obtained, whereas at 5 × 10(-1) Torr using a pulsed discharge some microtextured films are formed if the duty cycle is low. The morphology of these microtextured films consists of nanoparticles, filamentary particles, and particular agglomerates ("microflowers").

Laser desorption/ionization Fourier transform mass spectrometry of thin films deposited on silicon by plasma polymerization of acetylene.

Thin films deposited on silicon substrate by three different methods of plasma polymerization of acetylene were analyzed by direct laser desorption/ionization Fourier transform mass spectrometry. High-resolution mass spectra showed the presence of carbon clusters and hydrocarbon oligomers in different relative abundances. During unipolar and continuous discharge polymerization of acetylene-hydrogen gas mixtures, quadrupole mass spectra of the plasma constituents showed the presence of molecular species with m/z lower than 100--mainly peaks of C(4)H(2) and C(6)H(2).

Lipid and phospholipid profiling of biological samples using MALDI Fourier transform mass spectrometry.

Here we describe a study of the feasibility of lipid and phospholipid (PL) profiling using matrix assisted laser desorption/ionization (MALDI) Fourier transform mass spectrometry (FTMS) for two different applications. In this work PL profiles of different mammalian tissues as well as those of whole cell organisms were examined. In particular, comparative analysis of lipid and PL profiles of tissues from mice fed different diets was done and, in another application, MALDI FTMS was used to analyze PL profiles of genetically modified Saccharomyces cerevisiae.

Wide mass range trapping using a 7-T internal source matrix-assisted laser desorption/ionization Fourier transform mass spectrometer.

A wide mass range trapping experiment using internal source matrix-assisted laser desorption-Fourier transform mass spectrometry (MALDI-FTMS) was evaluated. In this method, the front trap plate potential is ramped up and the rear trap plate potential is simultaneously decreased using a cubic cell to trap ions over a wide range of mass-to-charge ratios. To apply this to MS/MS experiments, a second ion ejection procedure would remove unwanted ions, with the selected remaining ions then fragmented by collision-induced dissociation.

Characterizing the phospholipid profiles in mammalian tissues by MALDI FTMS.

Discussed here is an analytical method for profiling lipids and phospholipids directly from mammalian tissues excised from Mus musculus (house mouse). Biochemical analysis was accomplished through the use of matrix-assisted laser desorption/ionization (MALDI) Fourier transform mass spectrometry, where whole tissue sections of mouse brain, heart, and liver were investigated. Lipid and phospholipid ions create complex MALDI mass spectra containing multiple ions with different m/z values corresponding to the same fundamental chemical species.

Real-time monitoring of recombinant bacterial proteins by mass spectrometry.

Genetically altered bacteria manipulated to express green fluorescent protein (GFP) were used in an investigation of real-time monitoring for recombinant protein expression in cell by matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS). A significant advantage to whole cell MALDI MS is its ability to analyze bacterial cultures without pretreatment other than concentration. This paper describes the simultaneous analysis of overexpressed GFP recombinant Escherichia coli JM101 by MALDI-TOF MS and standard fluorescence measurements.

Hydrocarbon polymer analysis by external MALDI fourier transform and reflectron time of flight mass spectrometry.

The traditional solvent-based matrix-assisted laser desorption ionization (MALDI) preparation method has been used to analyze nonpolar polymers of various molecular weights. High resolution silver cationized oligomers with masses of up to 12 KDa were measured using 9.4 tesla Fourier transform mass spectrometry (FTMS) with an external ionization source.

Ionic liquid matrix-induced metastable decay of peptides and oligonucleotides and stabilization of phospholipids in MALDI FTMS analyses.

Room-temperature ionic liquid matrices (ILMs) have recently been investigated for use in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) and proven to be advantageous. Literature accounts of ILM performance for biological samples document increased sensitivity and ionization efficiency. These claims have been investigated here, and are supported for MALDI TOF applications to peptides, oligonucleotides, and phospholipids.

Trapping of wide range mass-to-charge ions and dependence on matrix amount in internal source MALDI-FTMS.

Internal ionization source MALDI-FTMS shows clear variation of number average molecular weight (M(n)) for an equimolar mixture of four PEG polymers (PEG 2000, PEG 4000, PEG 6000, PEG 8000) when the 2,5-dihydroxy benzoic acid (DHB) matrix to PEG ratio is varied or the laser power is changed. As the matrix to analyte ratio is increased, the analyte signal of higher molecular mass ions increases and the signal of lower mass ions decreases. Laser power dependence studies show a similar trend.

A comprehensive and comparative analysis for MALDI FTMS lipid and phospholipid profiles from biological samples.

Described here is a computationally automated method for translating complex accurate mass spectra into biologically relevant and meaningful data. Rapid profiling of detailed high resolution mass spectra resulting from direct analysis of whole cells and tissues by matrix-assisted laser desorption/ionization (MALDI) Fourier transform mass spectrometry (FTMS) is discussed. Lipid and phospholipid ions create complex spectra containing multiple m/z values corresponding to the same fundamental chemical species.

Strategies and data analysis techniques for lipid and phospholipid chemistry elucidation by intact cell MALDI-FTMS.

Ions attributed to lipids and phospholipids are directly observed by desorption from whole bacteria using intact cell (IC) matrix-assisted laser desorption-ionization (MALDI) Fourier transform mass spectrometry (FTMS). Saccharomyces cerevisiae are grown in rich media broth, concentrated, and applied directly to the MALDI surface without lysis or chemical treatment. FTMS of MALDI ions gives excellent signal to noise ratios with typical resolving powers of 90,000 and mass precision better than 0.

Use of double-depleted 13C and 15N culture media for analysis of whole cell bacteria by MALDI time-of-flight and Fourier transform mass spectrometry.

In the present paper, results demonstrating the significant advantages of matrix-assisted laser desorption/ionization (MALDI) analysis of whole cell samples of bacteria grown on double isotopically-depleted (13C and 15N) media are presented. It is shown that several advantages accrue for MALDI with a 9.4 T Fourier transform mass spectrometer (FTMS).

Investigation of MALDI-TOF and FT-MS techniques for analysis of Escherichia coli whole cells.

Recently, it has been demonstrated that bacteria can be characterized using whole cells and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). However, identification of specific bacterial proteins usually requires analysis of cellular fractions or purified extracts. Here, the first application of Fourier transform mass spectrometry (FTMS) to analysis of bacterial proteins directly from whole cells is reported.

Acetylenic Cyclophanes as Fullerene Precursors: Formation of C H and C by Laser Desorption Mass Spectrometry of C H (CO).

A logical precursor of macrocycle C H , cyclophane C H (CO) (1) represents a building block in a possible total synthesis of C . In Fourier transform ion cyclotron resonance laser desorption mass spectroscopic experiments in the negative-ion mode, 1 fragments to C H (2) under successive loss of CO. Further loss of six H atoms and rearrangement gives C ions with a fullerenic structure.