Browsing by Subject "mass spectrometry"

Now showing 1 - 7 of 7

Open Access
Electrospinning of functional poly(methyl methacrylate) nanofibers containing cyclodextrin-menthol inclusion complexes
(Institute of Physics Publishing, 2009) Uyar, Tamer; Nur, Y.; Hacaloglu, J.; Besenbacher, F.
Electrospinning of nanofibers with cyclodextrin inclusion complexes (CD-ICs) is particularly attractive since distinct properties can be obtained by combining the nanofibers with specific functions of the CD-ICs. Here we report on the electrospinning of poly(methyl methacrylate) (PMMA) nanofibers containing cyclodextrin-menthol inclusion complexes (CD-menthol-ICs). These CD-menthol-IC functionalized nanofibers were developed with the purpose of producing functional nanofibers that contain fragrances/flavors with high temperature stability, and menthol was used as a model fragrance/flavor material. The PMMA nanofibers were electrospun with CD-menthol-ICs using three type of CD: α-CD, β-CD, and γ-CD. Direct pyrolysis mass spectrometry (DP-MS) studies showed that the thermal evaporation of menthol occurred over a very high and a broad temperature range (100-355 °C) for PMMA/CDmenthol-IC nanowebs, demonstrating the complexation of menthol with the CD cavity and its high temperature stability. Furthermore, as the size of CD cavity increased in the order α-CD<β-CD<γ-CD, the thermal evolution of menthol shifted to higher temperatures, suggesting that the strength of interaction between menthol and the CD cavity is in the order γ-CD>β-CD>α-CD. © 2009 IOP Publishing Ltd.
Open Access
The formation and characterization of cyclodextrin functionalized polystyrene nanofibers produced by electrospinning
(2009) Uyar, Tamer; Havelund, R.; Hacaloglu J.; Zhou X.; Besenbacher F.; Kingshott P.
Polystyrene (PS) nanofibers containing the inclusion complex forming beta-cyclodextrin (β-CD) were successfully produced by electrospinning aimed at developing functional fibrous nanowebs. By optimization of the electrospinning parameters, which included varying the relative concentration of PS and β-CD in the solutions, bead-free fibers were produced. Homogeneous solutions of β-CD and PS in dimethylformamide (DMF) were used with concentrations of PS varying from 10% to 25% (w/v, with respect to DMF), and β-CD concentrations of 1% to 50% (w/w, with respect to PS). The presence of β-CD facilitated the production of bead-free PS fibers even from lower polymer concentrations as a result of the higher conductivity of the PS/CD solutions. The morphology and the production of bead-free PS/CD fibers were highly dependent on the β-CD contents. Transmission electron microscope (TEM) and atomic force microscope (AFM) images showed that incorporation of β-CD yielded PS fibers with rougher surfaces. Thermogravimetric analysis (TGA) and direct insertion probe pyrolysis mass spectroscopy (DP-MS) results confirmed the presence of β-CD in the PS fibers. X-ray diffraction (XRD) spectra of the fibers indicated that the β-CD molecules are distributed within the PS matrix without any phase separated crystalline aggregates up to 40% (w/w) β-CD loading. Furthermore, chemical analyses by Fourier transform infrared (FTIR) spectroscopy studies confirm that β-CD molecules are located within the PS fiber matrix. Finally, preliminary investigations using x-ray photoelectron spectroscopy (XPS) and time-of-flight static secondary ion mass spectrometry (ToF-static-SIMS) show the presence of the cyclodextrin molecules in the outer molecular layers of the fiber surfaces. The XPS and ToF-SIMS findings indicate that cyclodextrin functionalized PS webs would have the potential to be used as molecular filters and/or nanofilters for the purposes of filtration/purification/separation owing to surface associated β-CD molecules which have inclusion complexation capability. © 2009 IOP Publishing Ltd.
Open Access
Neutral particle mass spectrometry with nanomechanical systems
(Nature Publishing Group, 2015) Sage, E.; Brenac, A.; Alava, T.; Morel, R.; Dupré, C.; Hanay, M.S.; Roukes, M.L.; Duraffourg L.; Masselon, C.; Hentz, S.
Current approaches to mass spectrometry (MS) require ionization of the analytes of interest. For high-mass species, the resulting charge state distribution can be complex and difficult to interpret correctly. Here, using a setup comprising both conventional time-of-flight MS (TOF-MS) and nano-electromechanical systems-based MS (NEMS-MS) in situ, we show directly that NEMS-MS analysis is insensitive to charge state: the spectrum consists of a single peak whatever the speciesa' charge state, making it significantly clearer than existing MS analysis. In subsequent tests, all the charged particles are electrostatically removed from the beam, and unlike TOF-MS, NEMS-MS can still measure masses. This demonstrates the possibility to measure mass spectra for neutral particles. Thus, it is possible to envisage MS-based studies of analytes that are incompatible with current ionization techniques and the way is now open for the development of cutting-edge system architectures with unique analytical capability. © 2015 Macmillan Publishers Limited.
Open Access
Parametric power spectral density analysis of noise from instrumentation in MALDI TOF mass spectrometry
(2007) Shin H.; Mutlu, M.; Koomen J.M.; Markey, M.K.
Noise in mass spectrometry can interfere with identification of the biochemical substances in the sample. For example, the electric motors and circuits inside the mass spectrometer or in nearby equipment generate random noise that may distort the true shape of mass spectra. This paper presents a stochastic signal processing approach to analyzing noise from electrical noise sources (i.e., noise from instrumentation) in MALDI TOF mass spectrometry. Noise from instrumentation was hypothesized to be a mixture of thermal noise, 1/f noise, and electric or magnetic interference in the instrument. Parametric power spectral density estimation was conducted to derive the power distribution of noise from instrumentation with respect to frequencies. As expected, the experimental results show that noise from instrumentation contains 1/f noise and prominent periodic components in addition to thermal noise. These periodic components imply that the mass spectrometers used in this study may not be completely shielded from the internal or external electrical noise sources. However, according to a simulation study of human plasma mass spectra, noise from instrumentation does not seem to affect mass spectra significantly. In conclusion, analysis of noise from instrumentation using stochastic signal processing here provides an intuitive perspective on how to quantify noise in mass spectrometry through spectral modeling.
Open Access
Self-assembled template-directed synthesis of one-dimensional silica and titania nanostructures
(2011) Acar H.; Garifullin, R.; Güler, Mustafa O.
Mineralized biological materials such as shells, skeleton, and teeth experience biomineralization. Biomimetic materials exploit the biomineralization process to form functional organic-inorganic hybrid nanostructures. In this work, we mimicked the biomineralization process by the de novo design of an amyloid-like peptide that self-assembles into nanofibers. Chemically active groups enhancing the affinity for metal ions were used to accumulate silicon and titanium precursors on the organic template. The self-assembly process and template effect were characterized by CD, FT-IR, UV-vis, fluorescence, rheology, TGA, SEM, and TEM. The self-assembled organic nanostructures were exploited as a template to form high-aspect-ratio 1-D silica and titania nanostructures by the addition of appropriate precursors. Herein, a new bottom-up approach was demonstrated to form silica and titania nanostructures that can yield wide opportunities to produce high-aspect-ratio inorganic nanostructures with high surface areas. The materials developed in this work have vast potential in the fields of catalysis and electronic materials. © 2011 American Chemical Society.
Open Access
Synthesis of 3-aroyl-4-aryl-1-isopropylamino-4-piperidinols and evaluation of the cytotoxicities of the compounds against human hepatoma and breast cancer cell lines
(Taylor and Francis Ltd, 2015) Kucukoglu, K.; Mete, E.; Cetin-Atalay, R.; Gul H.I.
Some 4-piperidinol derivatives were synthesized and their cytotoxicity was tested against human hepatoma (Huh7) and breast cancer (T47D) cells. Aryl part was changed as phenyl in 2a, 4-methylphenyl in 2b, 4-methoxyphenyl in 2c, 4-chlorophenyl in 2d, 4-fluorophenyl in 2e, 4-bromophenyl in 2f, 4-nitrophenyl in 2g and 2-thienyl in 3. Compounds were synthesized and reported for the first time by this study except 2a and 2d. Chemical structures were confirmed by 1H NMR, 13C NMR, IR, MS and elemental analyses. Compounds 2a (3.1 times), 2c (3.8 times), 2f (4.6 times), 2g (1.3 times) and 3 (3.2 times) had 1.3-4.6 times higher cytotoxic potency than the reference compound 5-FU against Huh7 cell line while all the compounds synthesized had shown lower activities against T47D cell line than 5-FU. In the light of these results, compounds 2a, 2c, 2f, 2g and 3 may serve as model compounds for further studies. © 2014 Informa UK Ltd.
Open Access
Tissue distribution and correlation profiles of heavy-metal accumulation in the freshwater crayfish astacus leptodactylus
(2013) Tunca, E.; Ucuncu, E.; Ozkan, A.D.; Ulger, Z.E.; Tekinay, T.
The present work details the analysis of heavy-metal and metalloid concentrations in exoskeleton, gill, hepatopancreas, and abdominal muscle tissues of 60 crayfish (Astacus leptodactylus) specimens collected from Lake HirfanlI, a dam lake located in KIrşehir (Turkey) with a low metal-contamination profile. Concentrations of 11 metals (aluminum [Al], chromium [Cd], manganese [Mn], cobalt [Co], nickel [Ni], copper [Cu], molybdenum [Mo], silver [Ag], cadmium [Cd], mercury [Hg], and lead [Pb]) and a metalloid (arsenic [As]) were measured by inductively coupled plasma-mass spectrometry, and the relative frequencies of the most abundant isotopes of Cr, Cu, Ag, Cd, Hg, and Pb were evaluated. Three correlation trends were evaluated between the following: (1) different elements in the each individual tissue, (2) individual elements in different tissues, and (3) different elements in different tissues. In addition, correlation rates of growth parameters (weight, cephalothorax length, and total length) with heavy-metal and metalloid concentrations in each tissue were investigated. Our results suggest that substantial differences in metal and metalloid-accumulation levels exist between male and female specimens, with stronger correlations between the heavy-metal concentrations observed in the male cohort. It is notable that correlation trends of Co, Cu, 52As, Cr, and Ni in exoskeleton of the male specimens display strong similarities. Likewise, a very strong correlation is present in Ni-Cd and Ni-Pb accumulations in abdominal muscle of the male specimens; a similar trend is present between Cd and Pb concentrations in the same tissue of female specimens. For correlation rates of different heavy metals and metalloid in different tissues, the strongest positive association observed was between 63Cu in gill and As in hepatopancreas, whereas the strongest negative correlation was between accumulated Ni in abdominal muscle and As in exoskeleton. Strong correlations between metals and metalloid accumulations were observed between exoskeleton and gill. In many cases, metal and metalloid accumulation was negatively correlated with growth parameters. Preferential accumulation of Cr and Cu isotopes was observed in different tissues, suggesting that significant amounts of isotope fractionation occur during heavy-metal accumulation. Relatively low correlation rates were observed between 52Cr/ 53Cr and 63Cu/65Cu concentrations in several tissue types in both male and female cohorts, whereas no such trend was observed between Cd and Pb isotopes. © 2013 Springer Science+Business Media New York.