• Bulletin of the Korean Chemical Society
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• v.34 no.12
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• pp.3659-3664
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• 2013

Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either $[M-H]^-$ for TNT and DNT or $[M]^{{\cdot}-}$ for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i.e., $[M+HCOO]^-$. These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available.

• Analytical Science and Technology
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• v.16 no.6
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• pp.488-498
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• 2003

By LC/MS/MS, the analytical method of sildenafil and its analogues (homosildenafil, vardenafil and tadalafil) used as used medical treatment of impotence was established. electrosprary ionization (ESI) and atmospheric pressure chemical ionization (APCI) as a ionization method were applied. Several parameter were varied and the sensitivity and reproducibility were compared. In LC/ESI-MS method, capillary voltage, cone voltage, extractor, entrance and RF lens to create appropriate productr ions for multiple reaction monitoring (MRM) were variable parameter, but the formation of the other product ions except the precursor ion could not detect. And the value of entrance, collision energy, exit, corona voltage, cone voltage, extractor, RF lens, cone gas, and desolvation gas in APCI mode were varied, only the creation pattern of fragment ions by the change of RF lens value were detected, and the limit of detection was decreased due to the increase of S/N. Ten millimole ammonium formate (pH 4.8):acetonitrile=70:30 by isocratic elution in HPLC system was shown the maximum sensitivity in MS, the detection limit of sildenafil, homosildenafil, vardenafil and tadalafil obtained by ESI-MRM were 0.10, 0.025, 0.025, and $0.25{\mu}g/mL$ at S/N>5, respectively.

• Journal of Microbiology and Biotechnology
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• v.25 no.5
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• pp.704-708
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• 2015

For the analysis of multiple-reaction intermediates for long-chain dicarboxylic acid biotransformation, simple and reproducible methods of extraction and derivatization were developed on the basis of gas chromatography with flame ionization detector (GC-FID) instead of mass spectrometry. In the derivatization step, change of the ratio of pyridine to MSTFA from 1:3 to 9:1 resulted in higher peak intensity (p = 0.021) and reproducibility (0.6%CV) when analyzing 32 g/l ricinoleic acid (RA). Extraction of RA and ω-hydroxyundec-9-enoic acid with water containing 100 mM Tween 80 showed 90.4-99.9% relative extraction efficiency and 2-7%CV compared with those with hydrophobic ethyl acetate. In conclusion, reduction of the pyridine content and change of the extraction solvent to water with Tween 80 provided compatible derivatization and extraction methods to GC-FID-based analysis of longchain carboxylic acids.

• Transactions on Electrical and Electronic Materials
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• v.14 no.6
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• pp.329-333
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• 2013

SiOC films were prepared by capacitively coupled plasma chemical vapor deposition, and the correlation between the binding energy by X-ray photoelectron spectroscopy and Arrhenius equation for ionization energy was studied. The ionization energy decreased with increase of the potential barrier, and then the dielectric constant also decreased. The binding energy decreased with increase of the potential barrier. The dielectric constant and electrical characteristic of SiOC film was obtained by Arrhenius equation. The dielectric constant of SiOC film was decreased by lowering the polarization, which was made from the recombination between opposite polar sites, and the dissociation energy during the deposition. The SiOC film with the lowest dielectric constant had a flat surface, which depended on how carbocations recombined with other broken bonds of precursor molecules, and it became a fine cross-linked structure with low ionization energy, which contributed to decreasing the binding energy by Si 2p, C 1s electron orbital spectra and O 1s electron orbital spectra. The dielectric constant after annealing decreased, owing to the extraction of the $H_2O$ group, and lowering of the polarity.

• Transactions of the Korean Society of Mechanical Engineers B
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• v.29 no.4 s.235
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• pp.453-459
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• 2005

In this paper, we are proposing a robust tool which is capable of measuring the size and elemental composition of submicron particles from twenty to several hundreds nanometers at the same time, i.e., named Single Particle Mass Spectrometer (SPMS). The home-made SPMS employs a laser ablation/multi-photon ionization method to tear a nanoparticle into the constituent elemental ions. One thing different from the conventional Aerosol Time-of-Flight Mass Spectrometer (ATOFMS) is the power of the ionization laser. Much strong laser used in this work makes it possible to generate elemental ions rather than molecular ions from a nanoparticle. Also the use of high power laser may guarantee a complete ionization of a particle, which was confirmed by the existence of multiple charged ions. If a particle is evaporated/ionized completely and detected through electric field-free TOF tube without any loss, we can extract the original particle volume from the measured total ion numbers. Collecting a number of particles mass spectra, we get a database of size and elemental composition of nanoparticles, with which we may take a took into any kinds of chemical reaction occurring at nanoscale. Several issues related to size estimation by SPMS will be discussed.

• Bulletin of the Korean Chemical Society
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• v.31 no.8
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• pp.2293-2298
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• 2010

Focused electrospray (FES) deposition method is presented for matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. FES ion optics consists of two cylindrical focusing electrodes capped with a truncated conical electrode through which an electrospray emitter passes along the cylindrical axis. A spray of charged droplets is focused onto a sample well on a MALDI target plate under atmospheric pressure. The shape and size distributions of matrix crystals are visualized by scanning electron microscope and the mass spectra are obtained by time-of-flight mass spectrometry. Angiotensin II, bradykinin, and substance P are used as test samples, while $\alpha$-cyano-4-hydroxycinnamic acid and dihydroxybenzoic acid are employed as matrices. FES of a sample/matrix mixture produces fine crystal grains on a 1-3 mm spot and reproducibly yields the mass spectra with little shot-to-shot and spot-to-spot variations. Although FES greatly stabilizes the signals, the space charge due to matrix ions limits the detection sensitivity of peptides. To avoid the space charge problem, we adopted a dual FES/FES mode, which separately deposits matrix and sample by FES in sequence. The dual FES/FES mode reaches the detection sensitivity of 0.88 amol, enabling ultrasensitive of peptides by homogeneously depositing matrix and sample under atmospheric pressure.

• Bulletin of the Korean Chemical Society
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• v.30 no.2
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• pp.397-401
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• 2009

The complexes of $C_2-\;and\;C_6$-dihydroceramides with transition metal ions have been investigated by using Electrospray ionization-tandem mass spectrometry (ESI-MS/MS). The formation and fragmentation pathways of several doubly charged cluster ions as well as singly charged cluster ions of $C_2-\;and\;C_6$-dihydroceramides with transition metal ions have studied by ESI-MS/MS in the positive mode. Under ESI conditions, dihydroceramides form singly and doubly charged complexes with transition metal ions $(Mn^{2+},\;Fe^{2+},\;Co^{2+},\;Ni^{2+},\;and\;Zn^{2+}\;except\;Cu^{2+})$ with the compositions of $[DHCer+M+2H^2O-H]^+,\;[2DHCer+M+2H2O-H]^+,\;[3DHCer+M+2H2O-H]^+,\;[2DHCer+M]^{2+},\;[3DHCer+M]^{2+},\;[4DHCer+M]^{2+},\;[5DHCer+M]^{2+},\;and\;[6DHCer+M]^{2+}\;(DHCer\;=\;C_2-\;or\;C_6$-dihydroceramide, M = transition metal ion). The different complexation behavior of copper is responsible for relatively lower affinity of dihydroceramides to copper compared to those of other transition metals. It is also found that in the mass spectrum of the dihydroceramide complexes with copper(II), [2DHCer+Cu-H]$^+$ was observed with considerable intensity as well as [2DHCer+Cu+2$H_2O-H]^+$ due to its different geometry from those of other metals.

• Bulletin of the Korean Chemical Society
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• v.35 no.8
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• pp.2585-2588
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• 2014

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.113-114
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• 2013

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) imaging is a powerful technique for producing chemical images of small biomolecules (ex. metabolites, lipids, peptides) "as received" because of its high molecular specificity, high surface sensitivity, and submicron spatial resolution. In addition, matrix-assisted laser desorption and ionization time-of-flight (MALDI-TOF) imaging is an essential technique for producing chemical images of large biomolecules (ex. genes and proteins). For this talk, we will show that label-free mass imaging technique can be a platform technology for biomedical studies such as early detection/diagnostics, accurate histologic diagnosis, prediction of clinical outcome, stem cell therapy, biosensors, nanomedicine and drug screening [1-7].

• Bulletin of the Korean Chemical Society
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• v.34 no.5
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• pp.1571-1574
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• 2013