• Mass Spectrometry Letters
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• 제10권4호
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• pp.108-111
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• 2019

The hydrolysis of penicillin G, carbenicillin and ampicillin in pure water at room temperature was studied by high pressure liquid chromatography electrospray ionization mass spectrometry. Hydrolysis of ampicillin did not occur under these conditions; however, penicillin G and carbenicillin were completely hydrolyzed after seven days. A short interpretation of this difference is proposed. The mass spectrometric behaviour, namely ESI response and fragmentation pathway, of hydrolyzed penicillin G and hydrolyzed carbenicillin have been also discussed.

• Mass Spectrometry Letters
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• 제2권1호
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• pp.16-19
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• 2011

Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

• Bulletin of the Korean Chemical Society
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• 제25권6호
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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.

• Bulletin of the Korean Chemical Society
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• 제32권4호
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• pp.1221-1227
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• 2011

Ethyl pyruvate (EP) is known as a scavenger of reactive oxygen species (ROS) in the body through its role in the donation of diketone groups to metals to form an EP-metal complex. In order to develop a method for the quantification of EP in biological media, a sensitive and specific, high-performance liquid chromatographyelectrospray ionization-mass spectrometry (HPLC-ESI/MS) method is used to determine the EP-alkali metal ion binding species. The analyte was separated on a ZORBOX SB-C8 ($3.5{\mu}m$, $30mm{\times}2.1mm$ I.D.) column and analyzed in selected ion monitoring (SIM) mode with a positive ESI interface using the m/z 255 $[2M + Na]^+$ ion. The method was validated over the concentration range of $0.5-60.0\;{\mu}g$/mL under 1/9 (v/v) of acetonitrile/methanol solvent system with flow rate 0.05 mL/min. The limit of quantification (LOQ) was $0.5{\mu}g$/mL.

• Bulletin of the Korean Chemical Society
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• 제24권8호
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• pp.1163-1168
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• 2003

The structures of molecular species of galactolipids, such as monogalactosyl diacylglycerol (MGDG) and digalactosyl diacylglycerol (DGDG), isolated from wheat flour have been investigated using negative-ion electrospray ionization (ESI) mass spectrometry interfaced with high performance liquid chromatography (HPLC). According to the result of HPLC analysis, MGDG and DGDG were found to consist of mixtures of five and four molecular species, respectively. The galactolipids have been also analyzed to determine their fatty acid compositions, using HPLC/ESI-MS combined with in-source (or cone voltage) fragmentation. HPLC/ ESI-MS is very useful for one-step analysis of mixtures of galactolipids with a small sample quantity. Especially, the carboxylate anions produced in in-source fragmentations of the negative-ion of each component separated by HPLC provide valuable information on the composition of its fatty acyl chains.

• Mass Spectrometry Letters
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• 제5권1호
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• pp.1-11
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• 2014

Lipids play important roles in biological systems; they store energy, play a structural role in the cell membrane, and are involved in cell growth, signal transduction, and apoptosis. Phospholipids (PLs) in particular have received attention in the medical and lipidomics research fields because of their involvement in human diseases such as diabetes, obesity, atherosclerosis, and many cancers associated with lipid metabolic disorders. Here I review experimental strategies for PL analysis based on nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MSn). In particular, discussed are lipid extraction methods, nanoflow LC separation of PLs, effect of ionization modifiers on the ESI of PLs, influence of chain lengths and unsaturation degree of acyl chains of PLs on MS intensity, structural determination of the molecular structure of PLs and their oxidized products, and quantitative profiling of PLs from biological samples such as tissue, urine, and plasma in relation to cancer and coronary artery disease.

• Bulletin of the Korean Chemical Society
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• 제34권5호
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• pp.1571-1574
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• 2013

• Mass Spectrometry Letters
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• 제2권3호
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• pp.65-68
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• 2011

The effects of column length and particle size on the efficiency of separation and characterization of phospholipids (PLs) are investigated using nanoflow liquid chromatography-electrospray ionization-tandem mass spectrometry (nLC-ESI-MS-MS). Since PLs are associated with cell proliferation, apoptosis, and signal transduction, it is of increasing interests in lipidomics to establish reliable analytical methods for the qualitative and quantitative profiling of PLs related to biomarker development in adult diseases. Due to the complexity of PLs, the preliminary separation of PLs is necessary prior to MS analysis. In this study, length of capillary column and the particle size of reversed phase ($C_{18}$) packing materials are varied to find a reliable condition for the high speed and high resolution separation using 8 PL standard mixtures. From experiments, it was found that a capillary column of nLC-ESI-MS-MS analysis for PL mixtures can be minimized to a 5 cm long pulled tip column packed with 3 ${\mu}m$ $C_{18}$ particles without losing resolution.

• Bulletin of the Korean Chemical Society
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• 제24권9호
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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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• 제26권4호
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• pp.575-578
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• 2005

Electrospray ionization mass spectrometry (ESI MS) was used, along with gas chromatography-mass spectrometry (GC-MS), to monitor Paal-Knorr synthesis of 2,5-dimethyl-1-phenylpyrrole by condensation of aniline with 2,5-hexanedione. In addition to 2,5-dimethyl-1-phenylpyrrole observed as a single spot by TLC, unexpected dimer size compounds were observed by GC-MS. Dimers and trimers were observed by ESI MS. ESI tandem mass spectrometry was used to select plausible structures for the dimer. ESI MS with or without liquid chromatographic separation is useful for observing oligomeric byproducts with low volatility produced in organic reactions.