• Proceedings of the KIEE Conference
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• 2007.07a
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• pp.1534-1535
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• 2007

This paper describes a novel microfluidic device with a microfabricated electrospray source for a sheathless electrospray ionization interface to a mass spectrometer. This electrospray ionization-mass spectrometry (ESI-MS) device consists of a triangular-shaped metal emitter, allowing the generation of an efficient electrospray for peptide detection, and microfluidic channels monolithically in a glass microchip. The performance of the proposed interface was evaluated by opimizing its experimental condition and spraying standard peptides. The spraying has high signal strength and stability, with a relative standard deviation of 2.9% and singly-charged and doubly-charged peaks of the peptides were successfully detected. The metal emitter source showed a good performance to be comparable to commercially available emitters in signal strength and stability.

• Bulletin of the Korean Chemical Society
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• v.27 no.6
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• pp.947-950
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• 2006

• Bulletin of the Korean Chemical Society
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• v.30 no.8
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• pp.1864-1866
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• 2009

• Bulletin of the Korean Chemical Society
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• v.25 no.6
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• pp.878-880
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• 2004

Revered-phase LC-electrospray ionization mass spectrometry was used to selectively determine enalapril from plasma with minimal sample preparation. Detection limit of the method was 1 ng/mL. Precision (within day and between days) and accuracy of the method at various concentrations were acceptable. The analytical technique was used for pharmacokinetic studies after administration of enalapril to human test subjects.

• Mass Spectrometry Letters
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• v.6 no.2
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• pp.43-47
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• 2015

Detection of mefenamic acid (M, non-steroidal anti-inflammatory drug, NSAIDs) and its metallodrug was investigated using electrospray ionization mass spectrometry (ESI-MS) and fluorescence spectroscopy. ESI-MS data (500 µL, 1×10-3 M) revealed high detection sensitivity for the drug and metallodrug. ESI-MS spectra revealed peaks at 242, 580, and 777 Da corresponding to [M+H]+, [63Cu(M-H)2(H2O)2+H]+, and [56Fe(M-H)3+H]+, respectively. The metal:mefenamic ratios of ESIMS spectra are in complete agreement with the fluorescence spectroscopy results (1:2 for Cu(II) and 1:3 for Fe(III)). ESI is a soft ionization technique that can be used on labile metallo-mefenamic acids and is promising for the detection of these species in environmental samples and biological fluids.

• Proceedings of the KIEE Conference
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• 2004.07c
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• pp.2102-2104
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• 2004

In this study, sheathless electrospray from PDMS/glass microchips with conducting metal emitter tip is described. A chip-based capillary electrophoresis/mass spectrometry (CE/MS) system has advantages of the CE separation and on-line electrospray detection of peptide solution. We have fabricated a new electrospray ionization(ESI) device composed of the metal emitter tip and CE separation channel monolithically in a glass microchip. The separation channel and metal emitter tip are fabricated using a glass wet etching and gold electro plating process, respectively. The fabricated micro electrospray chip was tested by spraying peptide sample for mass spectrometric analysis. Singlely-charged peak and doublely-charged peak of peptide were detected and further MS/MS fragmentation was performed in each peak. Direct comparisons with conventional glass or fused silica emitters showed very similar performance with respect to signal strength and stability.

• Bulletin of the Korean Chemical Society
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• v.24 no.9
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• pp.1319-1323
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• 2003

This paper presents a successful demonstration of the on-line coupling of MEKC (micellar electrokinetic chromatography) to ESIMS (electrospray ionization mass spectrometry) for the quantitative analysis of seven s-triazine herbicides. The on-line MEKC-ESIMS was used to determine the structure of CE-separated peaks of seven triazine herbicides. The mixture of triazine herbicides was separated in a 20 mM sodium borate buffer (pH 8.5) containing 15 mM sodium dodecylsulfate (SDS) by using a bare fused-silica capillary. Electrospray ionization mass spectrometer was operated in the positive-ion mode when the mass spectra of seven triazine herbicides were observed from each peak, and the solution of water-methanol-formic acid (50/49/1 v/v/v) was used as a sheath liquid. The effects of SDS concentration, the run buffer pH, and the electric field on the separation of seven s-triazine herbicides were investigated. The MEKC-ESIMS detection showed 5 to 10 times higher sensitivity compared to the MEKC-UV detection. In addition, it did not need any pretreatment step.

• Bulletin of the Korean Chemical Society
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• v.26 no.8
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• pp.1235-1240
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• 2005

A combination of electrospray ionization and tandem mass spectrometry was used to characterize the scavenging reactions of acrylamide (AA) in the presence of glutathione (GSH) in vitro. In the presence of GSH, AA was deactivated effectively and scavenged by reactions consuming small amount of GSH. Reaction products and structural information were identified using collision-induced dissociation (CID) in an ion trap mass spectrometer. In the mixture of GSH and AA, significant increase in abundance of fragment ion peak was observed at m/z 233, which was identified as $[Cys-Glu]^+$, formed by the elimination of glycine moiety of GSH. GSH also contributes to the AA scavenging reaction by conjugating with AA through the sulfhydryl group in cysteine moiety. The probable scavenging reaction pathway of AA in the presence of GSH has been proposed based on the CID experimental data.

• Mass Spectrometry Letters
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• v.9 no.4
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• pp.91-94
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• 2018

Bilin tetrapyrroles are metabolic products of the breakdown of porphyrins within a species. In the case of mammals, these bilins are formed by the catabolism of heme and can be utilized as either biomarkers in disease or as an indicator of human waste contamination. Although a small subset of bilin tandem mass spectrometry reports exist, limited data is available in online databases for their fragmentation. The use of fragmentation data is important for metabolomics analyses to determine the identity of compounds detected within a sample. Therefore, in this study, the fragmentation of bilins generated by positive ion mode electrospray ionization is examined by collision-induced dissociation (CID) as a function of collision energy on an FT-ICR MS. The use of the FT-ICR MS allows for high mass accuracy measurements, and thus the formulas of resultant product ions can be ascertained. Based on our observations, fragmentation behavior for hemin, biliverdin and its dimethyl ester, phycocyanobilin, bilirubin, bilirubin conjugate, mesobilirubin, urobilin, and stercobilin are discussed in the context of the molecular structure and collision energy. This report provides insight into the identification of structures within this class of molecules for untargeted analyses.

• 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.