• Mass Spectrometry Letters
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• 제12권4호
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• pp.126-130
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• 2021

The mass spectrometry (MS) provides the mass-to-charge ratios of atoms, molecules, stable/metastable complexes, and their fragments. I have taken a long journey with MS to address outstanding issues and problems by experiments and theory and gain insights into underlying principles in chemistry. By looking through the mass-to-charge ratio, I have studied thermochemical problems in silicon chemistry, the infrared multiphoton dissociation spectroscopy of organometallic intermediates, unimolecular dissociations of halotoluene radical cations, and the kinetics of association/dissociation of alkali halide triple ions with Lewis bases. Various MS platforms have been used to characterize non-covalent interactions between porphyrins and fullerenes and those between the group IIB ions and trioctylchalcogenides, and to examine the binding of the group IA, IIA and porphyrin ions to G-quadruplex DNA. Recently, I have focused on mass-balanced H/D isotope dipeptide tags for MS-based quantitative proteomics, a simple chemical modification method for MS-based lipase assay, and the kinetics and dynamics of energy-variable collision-induced dissociation of chemically modified peptides. Now, I see an important role of MS in global issues in the post-COVID era, as the society demands high standards for indoor air quality to contain the airborne-pathogen transmission as well as in-situ monitoring and tracking of carbon emissions to reduce global warming.

• 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.

• Mass Spectrometry Letters
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• 제10권1호
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• pp.32-37
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• 2019

The ${\pi}-{\pi}$ interactions of the peptide-dimer and peptide-trimer complexes were investigated in the (VQIVYK + LYQLEN) and (VQIVYK + NNQQNY) mixing solutions. The results showed that tyrosine (Y) residues were critical in the formation of hetero peptide-dimers and -trimers during the early oligomerization process. We used collision-induced dissociation (CID) along with electrospray ionization mass spectroscopy (ESI-MS) to obtain the structural information of the hetero-dimers and -trimers. We chose three amyloidogenic peptides-VQIVYK, NNQQNY, and LYQLEN-from tau protein, yeast prion-like protein Sup35, and insulin chain A, respectively. Hetero-dimer, -trimer, -tetramer, and -pentamer complexes were observed in the mass spectra. The tandem mass spectrum of the hetero-dimer and hetero-trimer showed two different fragmentation patterns (covalent and non-covalent bond dissociation). Y-Y interaction structures were also proposed for the hetero-dimer and -trimer complexes.

• Mass Spectrometry Letters
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• 제4권4호
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• pp.91-94
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• 2013

We performed computer simulations to improve transmission efficiencies of a dual ion funnel system implemented on an FT-ICR MS. We found that the low m/z range from 50 to 150 could be significantly improved by operating the two ion funnels at different RF amplitudes. These new operational conditions could be applied to analyze metabolome samples, which require high sensitivity in the m/z range from 50 to 1,000.

• BMB Reports
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• 제43권7호
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• pp.506-511
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• 2010

The levels of salivary cortisol and cortisone in Korean adults were measured for the first time using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The salivary cortisol and cortisone were separated within 10 min. The regression coefficients (r) of the calibration curves were greater than 0.999 for the two steroids. The limits of quantitation (LOQ) were 0.2 ng/ml for cortisol and 1 ng/ml for cortisone. The intra-day precisions of the assay were <3.9% and 8.6% for cortisol and cortisone respectively, and the inter-day precisions were <1.9% and 4.3% for cortisol and cortisone, respectively. The salivary cortisone concentrations were approximately 4-9 times higher than those of salivary cortisol during the daytime. Diurnal rhythms, during which the cortisol and cortisone concentrations were higher in the morning than in the afternoon, were also observed. The present assay may be useful for the diagnosis of several adrenal dysfunctions in clinical biochemistry.

• Mass Spectrometry Letters
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• 제8권1호
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• pp.14-17
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• 2017

The effect of cationization agent concentration on glycan detection via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was investigated using $Na^+$ ions in the form of NaCl as the cationization agent. NaCl solution concentrations ranging from 1 mM to 1 M were investigated. Glycans from ovalbumin were mixed with the cationization agent solution and the 2,5-dihydroxybenzoic acid (2,5-DHB) matrix solution in a volume ratio of 1:1:1. The resulting mixture was loaded onto the MALDI plate. Two MALDI-TOF MS instruments (Voyager DE-STR MALDI-TOF MS and Tinkerbell RT MALDI-TOF MS) were used for detection of glycans. The best detection, in terms of the number of identified glycans, the peak intensity, and the signal-to-noise (S/N) ratio, was obtained with NaCl concentrations of 0.01-0.1 M for both MALDI-TOF MS instruments.

• 대한임상약리학회:학술대회논문집
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• 대한임상약리학회 2007년도 추계학술대회
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• pp.92-93
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• 2007

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• Mass Spectrometry Letters
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• 제3권2호
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• pp.29-38
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• 2012

A new approach of volatile compounds analysis is proposed using a linear ion trap Orbitrap mass spectrometer coupled with gas chromatography through an atmospheric pressure photoionization interface. In the proposed GC-HRMS/MS approach, direct chemical composition analysis is made for the precursor ions in high resolution MS spectra and the structural identifications were made through the database search of high quality MS/MS spectra. Successful analysis of a complex perfume sample was demonstrated and compared with GC-EI-Q and GC-EI-TOF. The current approach is complementary to conventional GC-EI-MS analysis and can identify low abundance co-eluting compounds. Toluene co-sprayed as a dopant through API probe significantly enhanced ionization of certain compounds and reduced oxidation during the ionization.

• BMB Reports
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• 제30권4호
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• pp.253-257
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• 1997

Negative ion fast atom bombardment (FAB) mass spectra were found to allow the determination of the linkage positions in a series of underivatized linkage-isomeric oligosaccharides. A previous work (Laine et al., 1988) reported that ion patterns of linkage-isomeric trisaccharides could be distinguished by a positive ion. Negative ion FAB collison-activated dissociation (CAD) mass spectrometry (MS) spectra of trisaccharides exhibited better sensitivity than the positive ion mode and provided specific fragmentation patterns according to the linkage positions. Especially, the fragmentations, m/z 205 in F6 and m/z 221 in G6, not occuring in 1-3 or 1-4 linkage. were an indication of 1-6 linkage, by changing collision energies from + 10 eV to +60 eV. The survival ratios of molecular ions in each collision energy set gave support to previous results in which the order of bond stability was 1-6>1-4>1-3 linkage.

• Mass Spectrometry Letters
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• 제8권4호
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• pp.90-97
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• 2017

Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry ($LC/MS^n$) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, $5{\alpha}-estrane-3{\beta}$, $17{\alpha}-diol$ exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in $LC-ESI-MS^n$ analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.