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Shin S.,Chungnam National University | Yang H.-J.,Chungnam National University | Kim J.-H.,Dong il Shimadzu Corporation | Kim J.,Chungnam National University | And 3 more authors.
Journal of Mass Spectrometry | Year: 2012

A peptide peak at m/z 1634 in the mass spectrum of tryptically digested cytochrome c has been ambiguously assigned to either a peptide IFVQKCAQCHTVEK or a peptide CAQCHTVEK combined with a heme group (CAQCHTVEK + heme (Fe(III))). A comprehensive investigation was performed to clearly identify the origin of the peak. Tryptic digests of cytochrome c were analyzed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), liquid chromatography-tandem MS (LC-MS/MS), LC-ultraviolet (LC-UV), and MALDI Fourier transform-ion cyclotron resonance (FT-ICR) MS. The use of instruments with extremely high mass accuracy revealed the mass difference between the IFVQKCAQCHTVEK and the (CAQCHTVEK + heme (Fe(III))) ions. Fragmentation of the peptide associated with the unknown peak yielded a heme ion and other fragment ions originating from a (CAQCHTVEK + heme (Fe(III))) ion. Furthermore, an absorption peak at 395 nm confirmed the presence of a heme group in the unknown peptide. High mass accuracy analyses of MS and MS/MS spectra, in addition to three-dimensional UV contour mapping, showed that the peak at m/z 1634 is due to a (CAQCHTVEK + heme (Fe(III))) ion and not from protonated IFVQKCAQCHTVEK. © 2012 John Wiley & Sons, Ltd.

Kim B.,Korea Research Institute of Standards and Science | Park S.,Korea Research Institute of Standards and Science | Park S.,CJ Corporation | Lee I.,Korea Research Institute of Standards and Science | And 4 more authors.
Analytical and Bioanalytical Chemistry | Year: 2010

A certified reference material (CRM), KRISS CRM 108-10-003, has been developed for analysis of acrylamide in potato chips, as a representative of carbohydrate-rich food cooked in high-temperature oil. The material was prepared by grinding commercially available potato chips to a paste which was then homogenized, bottled in 15-g units, and stored at -70 °C. Certification, homogeneity and stability testing, were carried out by liquid chromatography-isotope-dilution mass spectrometry (ID-LC-MS). A single ID-LC-MS measurement was performed for each of 10 selected units for certification and homogeneity assessment. The mean measurement result for the 10 bottles, 0.455∈±∈0.012 mg∈kg-1, was assigned as the certified value of the CRM. The between-bottle homogeneity was 0.8% of the certified value. The within-bottle homogeneity, tested by measuring three replicate sub-samples from each of three randomly selected bottles, was similar to the between-bottle homogeneity. The stability of the CRM under storage conditions (-70 °C) was tested for 21 months and no change in the acrylamide content was observed within the measurement uncertainty. Stability of the CRM at -20 °C (storage at user's site) and room temperature (for regular use and transportation) was also tested. Also presented is the newly designed procedure for evaluating the uncertainty of the certified value for the characterization scheme used in this study. [Figure not available: see fulltext.] © 2010 Springer-Verlag.

Sajjad R.U.,Myongji University | Kim K.J.,Dong il Shimadzu Corporation | Memon S.,Myongji University | Sukhbaatar C.,Myongji University | And 3 more authors.
Water Environment Research | Year: 2015

The monitoring of stormwater runoff from Light Rail Transit (LRT) facilities is insufficient in many regions around the world. In this study, runoff quality and quantity were monitored during operational and non-operational LRT phases during 2010-2013. The event mean concentration (EMC) of pollutants showed little statistical variability during both phases. The antecedent dry day (ADD) showed a strong to moderate positive correlation with most pollutant EMCs during the non-operational phase. The existence and magnitude of the first flush from LRT runoff was found to be similar to those from other transportation land uses. The comparison of LRT runoff data with an adjacent road bridge site showed that the pollutant EMC and unit load were 2 to 9 times higher from the road bridge. It was suggested that LRT automated operation and the elevated track makes this transportation mode a viable option for the management of non-point source pollution.

Park K.M.,Seoul National University | Moon J.H.,Korea Research Institute of Bioscience and Biotechnology | Kim J.H.,Dong il Shimadzu Corporation | Song U.T.,Dong il Shimadzu Corporation | And 3 more authors.
Rapid Communications in Mass Spectrometry | Year: 2016

Rationale In analyte profiling by matrix-assisted laser desorption/ionization (MALDI), drawing a quantitative profile map is an outstanding problem. Recently, we developed a method to quantify an analyte by MALDI, which is needed to solve the problem. Another requirement for quantitative profiling is the quantitative sample-to-matrix analyte transfer, which is investigated in this work. Methods MALDI-time-of-flight (TOF) spectra were acquired for samples produced by two methods. In one, a sample solution containing a matrix and an analyte was loaded with a pipet and dried. In the other, a sample was prepared by a consecutive process, i.e., loading-drying of an analyte solution followed by that of a matrix solution. Two different micro-spotters were used in the second method. Various mixtures of organic solvents with water were used to prepare matrix solutions. Results The organic solvent, matrix, and analyte used in the study did not affect the analyte transfer efficiency, whereas it improved as the water content in the solvent increased. It also improved as the liquid droplet emitted by a micro-spotter got larger. Use of a more polar solvent or a larger droplet increases the contact time between a solution droplet and the sample surface, which seems to be responsible for the improvement in the transfer efficiency. Conclusions Sample-to-matrix analyte transfer occurred efficiently when polar solvents and/or large liquid droplets were used to produce solid samples for MALDI profiling with a micro-spotter. A long contact time between the sample surface and a matrix solution droplet is one of the requirements for quantitative profiling. Copyright © 2015 John Wiley & Sons, Ltd.

Hong Y.,Dong il Shimadzu Corporation | Lee S.,Dong il Shimadzu Corporation | Kim H.-A.,Catholic University of Korea | Hwang Y.-K.,Catholic University of Korea
Journal of Applied Biological Chemistry | Year: 2010

This paper describes a simultaneous method for the determination of two aminoglycosides (neomy-cin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrom-etry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/ MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

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