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1.
Stowers MA van Wuijckhuijse AL Marijnissen JC Scarlett B van Baar BL Kientz CE 《Rapid communications in mass spectrometry : RCM》2000,14(10):829-833
Matrix-assisted laser desorption/ionization (MALDI) mass spectra were obtained from single biological aerosol particles using an aerosol time-of-flight mass spectrometer (ATOFMS). The inlet to the ATOFMS was coupled with an evaporation/condensation flow cell that allowed the aerosol to be coated with matrix material as the sampled stream entered the spectrometer. Mass spectra were generated from aerosol composed either of gramicidin-S or erythromycin, two small biological molecules, or from aerosolised spores of Bacillus subtilis var niger. Three different matrices were used: 3-nitrobenzyl alcohol, picolinic acid and sinapinic acid. A spectrum of gramicidin-S was generated from approximately 250 attomoles of material using a molar ratio of 3-nitrobenzyl alcohol to analyte of approximately 20:1. A single peak, located at 1224 Da, was obtained from the bacterial spores. The washing liquid and extract solution from the spores were analyzed using electrospray mass spectrometry and subsequent MS/MS product ion experiments. This independent analysis suggests that the measured species represents part of the B. subtilis peptidoglycan. The on-line addition of matrix allows quasi-real-time chemical analysis of individual, aerodynamically sized particles, with an overall system residence time of less than 5 seconds. These results suggest that a MALDI-ATOFMS can provide nearly real-time identification of biological aerosols. Copyright 2000 John Wiley & Sons, Ltd. 相似文献
2.
Jackson SN Mishra S Murray KK 《Rapid communications in mass spectrometry : RCM》2004,18(18):2041-2045
Matrix-assisted laser desorption/ionization (MALDI) was used for the on-line analysis of single particles. An aerosol was generated at atmospheric pressure and particles were introduced into a time-of-flight (TOF) mass spectrometer through a single-stage differentially pumped capillary inlet. Prior to entering the mass spectrometer, a matrix was added to the particles using a heated saturator and condenser. A liquid matrix, 3-nitrobenzyl alcohol (NBA), and a solid matrix, picolinic acid (PA), were used. Particles were ablated with a 351 nm excimer laser and the resulting ions were mass-separated in a two-stage reflectron TOF mass spectrometer. Aerosol particles containing the biomolecules erythromycin and gramicidin S were analyzed with and without the matrix addition step. The addition of NBA to the particles resulted in mass spectra that contained an intact molecular ion mass peak. In contrast, PA-coated particles did not yield molecular ion peaks from matrix-coated particles. 相似文献
3.
Wang Y Schubert M Ingendoh A Franzen J 《Rapid communications in mass spectrometry : RCM》2000,14(1):12-17
Non-covalently-bound subunit complexes of proteins have been measured by an ion trap mass spectrometer equipped with an orthogonal electrospray ionization source. For the analysis of the generated molecular ions with high mass/charge ratios, the mass/charge range of the ion trap was extended by increasing its radio frequency (rf) voltage to 15 kV (V(0-p)) and by resonant ion ejection. Ions of the non-covalent dimer of bovine serum albumin (BSA), as well as of subunit complexes of alcohol dehydrogenase (ADH) from bakers' yeast and from horse liver, have been detected at mass/charge values between 3000-9000 Th. The maximum observed molecular weight was that of a non-covalently-bound subunit-octamer of bakers' yeast ADH (two non-covalently-bound subunit-tetramers) at ca. 290 kDa. 相似文献
4.
Desorption electrospray ionization (DESI) mass spectrometry has been implemented on a commercial ion‐trap mass spectrometer and used to optimize mass spectrometric conditions for DNA nucleobases: adenine, cytosine, thymine, and guanine. Experimental parameters including spray voltage, distance between mass spectrometer inlet and the sampled spot, and nebulizing gas inlet pressure were optimized. Cluster ions including some magic number clusters of nucleobases were observed for the first time using DESI mass spectrometry. The formation of the cluster species was found to vary with the nucleobases, acidification of the spray solvent, and the deposited sample amount. All the experimental results can be explained well using a liquid film model based on the two‐step droplet pick‐up mechanism. It is further suggested that solubility of the analytes in the spray solvent is an important factor to consider for their studies by using DESI. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
5.
Schneider BB Baranov VI Javaheri H Covey TR 《Journal of the American Society for Mass Spectrometry》2003,14(11):1236-1246
An atmosphere to vacuum interface was designed to exploit the different mobility and momentum characteristics of ions, and charged and neutral particles in electrospray ionization-mass spectrometry. The purpose of this device is to transmit with high efficiency the ions created at atmospheric pressure into the mass analyzer and to deflect the large charged and neutral particles prior to entrance into the vacuum system, thereby maintaining system cleanliness and stability. This interface is particularly suitable for low flow rate electrospray ionization-mass spectrometry where the close proximity of the electrospray emitters to the vacuum entrance, and near total consumption of the entire spray, leads to the production of large quantities of non-desolvated droplets and large charged and neutral particles. The improvement involves the application of potential gradients to a particle discriminator space located between the gas restricting ion entrance orifice of the mass spectrometer and the exit of a heated laminar flow chamber to divert large particles from the gas conductance limiting orifice. A counter-current flow of drying gas is used to deflect neutral particles and solvent vapor. Two stages of desolvation are achieved with the combined effects of the curtain gas and heated laminar flow chamber. This enhances the efficiency of desolvation and ion production, and stabilizes the resulting ion current under a wide variety of solvent compositions. In addition, this system eliminates the problems associated with the boiling of solution in nanospray tips when operated in close proximity to a heated mass spectrometer inlet. The particle discriminator interface gives approximately a 2-fold improvement in ion count rates, and a 3-fold improvement in stability (as measured by the signal relative standard deviation). 相似文献
6.
Roger Guevremont Luyi Ding Barbara Ells David A. Barnett Randy W. Purves 《Journal of the American Society for Mass Spectrometry》2001,12(12):47-1330
A tandem FAIMS–FAIMS system for ion trapping at room temperature and atmospheric pressure is described. The first FAIMS device consisted of a side-to-side configuration (sFAIMS) suitable for ion separation, whereas the second FAIMS device was appropriate for ion trapping (tFAIMS). Ions pre-selected by the sFAIMS entered the tFAIMS and were captured by virtual trapping fields at the hemispherical tip of the inner electrode. The use of the sFAIMS, with wider electrode diameters, and consequently better ion separation efficiency than the tFAIMS, lowered the number of background ions captured in the trapping region of tFAIMS, and thus reduced the space charge effects in the trap. This tandem device was coupled to a laboratory built time-of-flight mass spectrometer and was evaluated using the electrospray generated [M + 2H]2+ ion of gramicidin S. The half-time (t1/2) of the exponential decay of the ion cloud in tFAIMS, determined by monitoring the residual intensity of ions extracted from the ion trapping region of tFAIMS after various delay times, was about 2 s. 相似文献
7.
Myung S Cohen H Fenyo D Padovan JC Krutchinsky AN Chait BT 《International journal of mass spectrometry》2011,301(1-3):211-219
A high-capacity ion trap coupled to a time-of-flight (TOF) mass spectrometer has been developed to carry out comprehensive linked scan analysis of all stored ions in the ion trap. The approach involves a novel tapered geometry high-capacity ion trap that can store more than 10(6) ions (range 800-4000 m/z) without degrading its performance. Ions are stored and scanned out from the high-capacity ion trap as a function of m/z, collisionally fragmented and analyzed by TOF. Accurate mass analysis is achieved on both the precursor and fragment ions of all species ejected from the ion trap. We demonstrate the approach for comprehensive linked-scan identification of phosphopeptides in mixtures with their corresponding unphosphorylated peptides. 相似文献
8.
We have used an infrared laser for desorption of material and ionization by interaction with electrosprayed solvent. Infrared laser-assisted desorption electrospray ionization (IR LADESI) mass spectrometry was used for the direct analysis of water-containing samples under ambient conditions. An ion trap mass spectrometer was modified to include a pulsed Er:YAG laser at 2.94 microm wavelength coupled into a germanium oxide optical fiber for desorption at atmospheric pressure and a nanoelectrospray source for ionization. Analytes in aqueous solution were placed on a stainless steel target and irradiated with the pulsed IR laser. Material desorbed and ablated from the target was ionized by a continuous stream of charged droplets from the electrosprayed solvent. Peptide and protein samples analyzed using this method yield mass spectra similar to those obtained by conventional electrospray. Blood and urine were analyzed without sample pretreatment to demonstrate the capability of IR LADESI for direct analysis of biological fluids. Pharmaceutical products were also directly analyzed. Finally, the role of water as a matrix in the IR LADESI process is discussed. 相似文献
9.
R E Kaiser J D Williams S A Lammert R G Cooks D Zakett 《Journal of chromatography. A》1991,562(1-2):3-11
A theromospray ion source using corona discharge ionization was interfaced to a quadrupole ion trap mass spectrometer via a multi-element lens system. Ions were injected into the trap periodically where they were stabilized by collisions with helium bath gas. Mass spectra were recorded on the trapped ions using the mass-selective instability scan mode. Data are shown for a peptide and a nucleoside and the effects of some experimental variables on the spectra are explored. 相似文献
10.
Dixon RB Bereman MS Muddiman DC Hawkridge AM 《Journal of the American Society for Mass Spectrometry》2007,18(10):1844-1847
A commercial air ejector was coupled to an electrospray ionization linear ion trap mass spectrometer (LTQ) to transport remotely generated ions from both electrospray (ESI) and desorption electrospray ionization (DESI) sources. We demonstrate the remote analysis of a series of analyte ions that range from small molecules and polymers to polypeptides using the AE-LTQ interface. The details of the ESI-AE-LTQ and DESI-AE-LTQ experimental configurations are described and preliminary mass spectrometric data are presented. 相似文献
11.
The direct analysis of separated rhodamine dyes on reversed-phase C(8) thin-layer chromatography plates using a surface sampling/electrospray emitter probe coupled with a triple-quadrupole linear ion trap mass spectrometer is presented. This report represents continuing work to advance the performance metrics and utility of this basic surface sampling electrospray mass spectrometry system for the analysis of thin-layer chromatography plates. Experimental results examining the role of sampling probe spray end configuration on liquid aspiration rate and gas-phase ion signal generated are discussed. The detection figures-of-merit afforded by full-scan, automated product ion and selected reaction monitoring modes of operation were examined. The effect of different eluting solvents on mass spectrum signal levels with the reversed-phase C(8) plate was investigated. The combined effect of eluting solvent flow-rate and development lane surface scan rate on preservation of chromatographic resolution was also studied. Analysis of chromatographically separated red pen ink extracts from eight different pens using selected reaction monitoring demonstrated the potential of this surface sampling electrospray mass spectrometry system for targeted compound analysis with real samples. 相似文献
12.
Colas C Garcia P Popot MA Bonnaire Y Bouchonnet S 《Rapid communications in mass spectrometry : RCM》2006,20(22):3257-3266
A method has been developed for the analysis and characterization in equine urine and plasma of iridoid glycosides: harpagide, harpagoside and 8-para-coumaroyl harpagide, which are the main active principles of Harpagophytum, a plant with antiinflammatory properties. The method involves liquid chromatography coupled with positive electrospray ionization mass spectrometry. The addition of sodium or lithium chloride instead of formic acid in the eluting solvent has been studied in order to enhance the signal and to modify the ion's internal energy. Fragmentation pathways and associated patterns are proposed for each analyte. A comparison of three types of mass spectrometer: a 3D ion trap, a triple quadrupole and a linear ion trap, has been conducted. The 3D ion trap was selected for drug screening analysis whereas the linear ion trap was retained for identification and quantitation analysis. 相似文献
13.
Chen H Touboul D Jecklin MC Zheng J Luo M Zenobi R 《European journal of mass spectrometry (Chichester, England)》2007,13(4):273-279
A home-made extractive electrospray ionization source is coupled to an linear quadrupole ion trap mass spectrometer to investigate ion/molecule reactions of biopolymers at ambient pressure. Multiply charged biopolymers such as peptides and proteins generated in an electrospray are easily reduced to a low charge state by the atmospheric pressure ion/molecule reactions occurring between the multiply charged ions and a strong basic reagent sprayed in neutral form into the electrospray plume. The charge state of the biopolymer ions can be manipulated by controlling the amount of the basic reagent. The production of biopolymer ions with low charge states results in a substantial improvement of sensitivity and reduced spectral congestion in ESI-MS. This is of importance for biopolymer mixture analysis and could have promising applications in proteomics. 相似文献
14.
Tsung-Yi Chen Jia-Yi Lin Jen-Yi Chen Yu-Chie Chen 《Journal of the American Society for Mass Spectrometry》2010,21(9):1547-1553
In this paper, we describe a novel technique—ultrasonication-assisted spray ionization (UASI)—for the generation of singly
charged and multiply charged gas-phase ions of biomolecules (e.g., amino acids, peptides, and proteins) from solution; this
method employs a low-frequency ultrasonicator (ca. 40 kHz) in place of the high electric field required for electrospray ionization.
When a capillary inlet is immersed into a sample solution within a vial subjected to ultrasonication, the solution is continually
directed to the capillary outlet as a result of ultrasonication-assisted capillary action; an ultrasonic spray of the sample
solution is emitted at the outlet of the tapered capillary, leading to the ready generation of gas-phase ions. Using an ion
trap mass spectrometer, we found that singly charged amino acid and multiply charged peptides/proteins ions were generated
through this single-step operation, which is both straightforward and extremely simple to perform. The setup is uncomplicated:
only a low-frequency ultrasonicator and a tapered capillary are required to perform UASI. The mass spectra of the multiply
charged peptides and proteins obtained from sample solutions subjected to UASI resemble those observed in ESI mass spectra. 相似文献
15.
Boue SM Stephenson JL Yost RA 《Rapid communications in mass spectrometry : RCM》2000,14(15):1391-1397
Previous infrared multiphoton dissociation (IRMPD) experiments utilizing a quadrupole ion trap mass spectrometer yielded limited photodissociation efficiencies. Helium buffer gas continuously infused into the analyzer region at pressures of typically 1 x 10(-3) Torr to improve ion trap performance can collisionally quench photoexcited ions during the IRMPD process. Photodissociation experiments have indicated that uncorrected pressures below 2 x 10(-5) Torr are necessary to avoid collisional deactivation of photoexcited ions. This paper describes IRMPD in the quadrupole ion trap at reduced pressures utilizing a dual-pulsed introduction of helium buffer gas incorporated into the ion trap scan function. The pulsed introduction of helium buffer gas before ion injection allows the efficient trapping of ions injected from an electrospray source and the removal of helium before laser irradiation. A second pulse of helium directly before ion detection improves the intensity of the ion signal. The use of this dual-pulsed inlet of helium for improved IRMPD is demonstrated with the carbohydrate antibiotics neomycin and erythromycin. Copyright 2000 John Wiley & Sons, Ltd. 相似文献
16.
Upthagrove AL Hackett M Nelson WL 《Rapid communications in mass spectrometry : RCM》1999,13(6):534-541
Propranolol, deuterium- and 18O-labeled propranolol and related compounds were analyzed using an ion trap mass spectrometer equipped with a modified Finnigan API electrospray interface. Sequential product ion (MSn) experiments were used to elucidate fragmentation pathways for these compounds. The observed ions were compared to those observed under electron impact (EI) conditions. The electrospray ionization (ESI) ion trap spectra, as well as the EI spectra, afford useful information to allow assignments of most product ions, many of which retain portions of the aliphatic three-carbon side chain. 相似文献
17.
Gökhan Baykut Oliver von Halem Oliver Raether 《Journal of the American Society for Mass Spectrometry》2009,20(11):2070-2081
A dynamic method is applied to measure the mobility of gas-phase ions in the dual ion funnel interface of the electrospray
source of a quadrupole orthogonal time-of-flight mass spectrometer. In a new operational mode, a potential barrier was formed
in the second ion funnel of the mass spectrometer and then progressively increased. In this region, a flow of gas drags the
ions into the mass spectrometer while the electric force applied by the potential barrier decelerates them. Ions with lower
mobility can be carried by the gas flow more easily than those with high mobility. Thus, electrical forces can block the more
mobile ions more easily. Hence, the electric barrier formed in the ion funnel permits only ions below a certain mobility threshold
to enter the mass spectrometer. When the barrier voltage is increased, this threshold moves from high to low mobilities. Ions
with mobilities above the threshold cannot enter the mass spectrometer, and their signal decreases to zero. Thus, in a barrier
voltage scan, mass spectrometric signals of ions sequentially disappear. Differentiation of these decreasing ion signal curves
produces peaks from which an ion mobility spectrum can be reconstructed. Blocking voltages, i.e., the positions of the peaks
on the barrier voltage scale are directly related to the mobility of these ions. An internal calibration using ions with known
mobility values helps determine the unknown ion mobilities and allows calculation of ionic cross sections. 相似文献
18.
Hiroyuki Inoue Hiroaki Hashimoto Susumu Watanabe Yuko T. Iwata Tatsuyuki Kanamori Hajime Miyaguchi Kenji Tsujikawa Kenji Kuwayama Noriyuki Tachi Naohito Uetake 《Journal of mass spectrometry : JMS》2009,44(9):1300-1307
A novel approach to the analysis of ecstasy tablets by direct mass spectrometry coupled with thermal desorption (TD) and counter‐flow introduction atmospheric pressure chemical ionization (CFI‐APCI) is described. Analytes were thermally desorbed with a metal block heater and introduced to a CFI‐APCI source with ambient air by a diaphragm pump. Water in the air was sufficient to act as the reactive reagent responsible for the generation of ions in the positive corona discharge. TD‐CFI‐APCI required neither a nebulizing gas nor solvent flow and the accompanying laborious optimizations. Ions generated were sent in the direction opposite to the air flow by an electric field and introduced into an ion trap mass spectrometer. The major ions corresponding to the protonated molecules ([M + H]+) were observed with several fragment ions in full scan mass spectrometry (MS) mode. Collision‐induced dissociation of protonated molecules gave characteristic product‐ion mass spectra and provided identification of the analytes within 5 s. The method required neither sample pretreatment nor a chromatographic separation step. The effectiveness of the combination of TD and CFI‐APCI was demonstrated by application to the direct mass spectrometric analysis of ecstasy tablets and legal pharmaceutical products. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
19.
Myles W. Gardner Jennifer S. Brodbelt 《Journal of the American Society for Mass Spectrometry》2009,20(12):2206-2210
Supplemental infrared (IR) activation was applied to reduce background chemical noise and increase analyte ion signal in a
linear ion trap mass spectrometer. Peptides, proteins, and small molecules were all introduced by electrospray ionization,
and when regions of chemical noise were isolated and subjected to IR irradiation, protonated analyte molecules were observed
in the product ion mass spectra. By isolating the entire mass range (e.g., m/z 400–2000) and then irradiating all ions in the trap, supplemental IR activation increased the signal of singly protonated
peptides by almost 70% and by 40%–55% for the lower charge states of cytochrome c. This increase in analyte ion signal was less dramatic for the higher charge states of peptides and proteins. The chemical
noise present in the mass spectra is attributed to incomplete desolvation of the electrospray, as the abundance of the protonated
peptides observed upon supplemental IR activation of the chemical noise decreased with higher inlet capillary temperatures.
Collision activation was not as effective for desolvating the ions present in the chemical noise. 相似文献
20.
The diterpenoids and flavonoids in Isodon rubescens were analyzed simultaneously by high-performance liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS-MS) for the first time. The fragmentation pathway of rubescensin A (oridonin) and rubescensin B (ponicidin) in an electrospray ion trap mass spectrometer was also investigated. A total of 10 compounds, including five diterpenoids and five flavonoids, were identified or preliminarily characterized based on their mass spectra. Six of them were reported from Isodon species for the first time. 相似文献