• Title/Summary/Keyword: High-resolution mass spectrometry

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Mass Spectrometry-Based Strategy for Effective Disulfide Bond Identification (질량분석기를 활용한 효과적 이황화결합 분석법 개발)

  • Jin, Jonghwa;Min, Hophil;Kwon, Oh-Seung;Oh, Hyun Jeong;Kim, Jongwon;Park, Chulhwan
    • Korean Chemical Engineering Research
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    • v.55 no.1
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    • pp.27-33
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    • 2017
  • The determination of disulfide bonds is important for comprehensive understanding of the chemical structure of protein. So far, many strategies for the disulfide bond analysis have been suggested in terms of speed and sensitivity. However, most of these strategies have not considered free thiol residues in the target protein in the process of determining the disulfide bond. We suggested the strategy which was composed of four steps for the identification of disulfide bonds; the first step was the prediction of possible disulfide bonds, the second step was the determination of free cysteine residues, the third step was the analysis of disulfide bond using a high-resolution mass spectrometry, and the final step was the determination of disulfide bonds based on the comprehensive verification. In this study, we performed the characterization of disulfide bonds for the recombinant protein (HRPE1), where 1 and 5 inter- and intra-chain disulfide bonds were identified, respectively.

Deposition flux of dioxin-like polychlorinated biphenyls(DLPCBs) in urban environment of Busan (도심 지역의 다이옥신류 폴리염화비페닐류의 침적 플럭스)

  • Mun, Hyo-Bang;Lee, Su-Jeong;Choe, Hui-Gu;Ok, Gon
    • Journal of Environmental Science International
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    • v.13 no.5
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    • pp.469-478
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    • 2004
  • Atmospheric bulk (wet and dry) samples were monthly collected in an urban environment (Daeyeon-dong) of Busan over a year, to assess the deposition flux and seasonality of dioxin-like polychlorinated biphenyls (DLPCBs) using stainless steel pots. Deposition fluxes of DLPCBs in bulk samples were determined using high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Particle deposition fluxes in the urban environment varied from 23 to 98 $mg^2$/year (mean 41 $gm^2$/year). DLPCB deposition fluxes in atmospheric bulk samples ranged from 0.09 to 0.77 ng-$TEQ/m^2$/year (mean 0.35 ng-$TEQ/m^2$/year). Seasonal atmospheric deposition fluxes of DLPCBs were high in winter and low in summer. Atmospheric deposition fluxes of particles and DLPCBs in this study were comparable to or slightly lower values than those of different locations in the world. Monthly DLPCB profiles in deposition bulk samples were similar over a year. Non-ortho PCBs were higher contributions to the total DLPCBs fluxes than mono-ortho PCBs. In particular, PCB 126 had the highest concentrartion (>75%) in all deposition samples, followed by PCB 169 and PCB 156. A highly positive correlation was found among the deposition fluxes of DLPCB species, suggesting the possibility of that the DLPCB contamination originated from one source. The deposition fluxes of DLPCBs were not significantly correlated with temperature and the amount of precipitation even though the summer season with the highest temperature and the largest amount of precipitation showed the lowest DLPCB deposition flux.

Levels of PBDEs in Pig Feed (축산물 사료중의 Polybrominated Diphenyl Ethers(PBDEs) 평가)

  • Shin, Jeoung-Hwa;Ahn, Yun-Gyong
    • The Korean Journal of Community Living Science
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    • v.23 no.3
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    • pp.255-263
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    • 2012
  • Polybrominated diphenyl ethers (PBDEs) are a group of brominated flame retardants (BFRs), which are used in a variety of consumer products. Several of those are produced in large quantities. Their chemical structure similarities to polychlorinated dibenzo-p-dioxins and polychlorinated biphenyls (PCBs), as well as their toxicity, has been studied. PBDEs are persistent and lipophilic, which results in their bioaccumulation in the fatty tissues of organisms and enrichment throughout food chains. In addition, a number of studies also reported high levels of PBDEs in animals and food resulting from the use of contaminated animal feed Public concern about PBDEs levels in animals and food has been raised. Feed contamination by toxic chemicals has been the cause of the contamination of poultry products. The purpose of this study was to evaluate PBDEs in pig feed to search the origin chase of POPs in pigs. Feed samples were obtained wheat from East Europe, corn from South America and America, soybean meal from Korea, America, South America and India and tallow from Korea. The preparation of samples was based on the EPA method 1614. Instrumental analysis was based on the use of high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Quantification was carried out by the isotopic dilution method. The analysis of ${\Sigma}PBDEs$ involved 22 PBDE congeners, including BDE-17, 28, 47, 49, 66, 71, 77, 85, 99, 100, 119, 126, 138, 153, 154, 156, 183, 184, 190, 191, 196 and 197.

Evaluation for Concentration of Residual PCDD/Fs in Pig Feed (돼지사료 중의 다이옥신 잔류 평가)

  • Ahn, Yun-Gyong;Shin, Jeoung-Hwa
    • The Korean Journal of Community Living Science
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    • v.23 no.2
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    • pp.129-136
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    • 2012
  • Dioxins are chemical substances that are not properly decomposed degradation under natural photochemical, biological and chemical conditions in the environment, and bio-accumulate through the food chain, so pose a risk of causing adverse effects to human health and the environment. Ninety seven percent of human exposure to dioxins comes through meat, fish, dairy consumption and so on. Pork is the largest proportion meat aspect of daily intake in the Korean food. Pigs are three times more than Cattle in terms of breeding population and production amount in the world, and the amount is increasing every year. Therefore, it is necessary to monitor the exposure level of dioxins in pig's body. Also, it is required to evaluate the presence of these chemical substances in the pig's feed grain such as corn, soybeans, and tallow. The purpose of this study was to evaluate PCDD/Fs in pig's feed to search the origin of PCDD/Fs. Feed samples obtained were wheat from East Europe, corn from South America and America, soybean meal from Korea, America, South America and India and tallow from Korea. The preparation of samples was based on the EPA method 1613. Instrumental analysis was based on the use of high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). The concentrations of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) and 1,2,3,7,8-pentachlorodibenzo-p-dioxin (PCDD), which are the most toxic potent dioxins, were not observed in any of the samples. However OCDD was detected in most of the samples. The TEQs in the feed samples were ranged from 0 pg TEQ/g to 0.09841 pg TEQ/g. Especially, the high level of TEQs was observed in the samples of wheat from East Europe and soybean meal from Korea.

Antibacterial Effect of Fructose Laurate Synthesized by Candida antarctica B Lipase-Mediated Transesterification

  • Lee, Ki Ppeum;Kim, Hyung Kwoun
    • Journal of Microbiology and Biotechnology
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    • v.26 no.9
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    • pp.1579-1585
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    • 2016
  • Sugar esters are valuable compounds composed of various sugars and fatty acids that can be used as antibacterial agents and emulsifiers in toothpaste and canned foods. For example, fructose fatty acid esters suppress growth of Streptococcus mutans, a typical pathogenic bacterium causing dental caries. In this study, fructose laurate ester was chosen as a target material and was synthesized by a transesterification reaction using Candida antarctica lipase B. We performed a solvent screening experiment and found that a t-butanol/dimethyl sulfoxide mixture was the best solvent to dissolve fructose and methyl laurate. Fructose laurate was synthesized by transesterification of fructose (100 mM) with methyl laurate (30 mM) in t-butanol containing 20% dimethyl sulfoxide. The conversion yield was about 90%, which was calculated based on the quantity of methyl laurate using high-performance liquid chromatography. Fructose monolaurate (Mr 361) was detected in the reaction mixture by high-resolution mass spectrometry. The inhibitory effect of fructose laurate on growth of oral or food spoilage microorganisms, including S. mutans, Bacillus coagulans, and Geobacillus stearothermophilus, was evaluated.

Analysis of Micropollutants and Their Metabolites in the Hwapo Wetland through Target, Suspect, and Non-target Screening Using LC-HRMS (LC-HRMS 기반의 표적, 추정 및 비표적 분석기법을 이용한 화포습지 내 미량오염물질 및 대사체 분석)

  • Hwang, Sumin;Jeon, Junho
    • Journal of Environmental Analysis, Health and Toxicology
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    • v.21 no.4
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    • pp.304-315
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    • 2018
  • Located in Gimhae, Hwapo is the biggest riverine wetland in the province of Gyeongsangsam-do, Korea, and is a major habitat for various species. However, it is suspected that various pollutants enter the wetlands from agricultural and industrial areas. This study identifies major organic pollutants in this wetland and their sources using high performance liquid chromatography-high resolution mass spectrometry during one summer season. Forty-five substances were selected for quantitative analysis using target screening, and other non-selected compounds were screened using suspect and non-target screening methods. The results were that 21 and 17 targeted substances were detected in July and August, respectively. Major pollutants in July and August were oxadiazon (July: 17-220 ng/L, August: 66-460 ng/L), carbendazim (July: 10-110 ng/L, August: 64-520 ng/L), caffeine (July: 33-1,100 ng/L, August: 56-580 ng/L), and niflumic acid (July: 23-75 ng/L, August: 42-290 ng/L). Sampling sites S4 in July and S2 in August were the major inflow points. Ten substances (tricyclazole, hexaconazole, diuron, fexofenadine, irbesartan, simetryn, cimetidine, valsartan, tebuconazole, and benzotriazole) and four metabolites (valsartan acid, azoxystrobin acid, TEB_M324c, and 2-aminobenzimidazole) were tentatively identified through suspect and non-target screening, respectively.

Analyzing Co-planar PCBs in Food by HRGC/HRMS with Isotopic Dilution Method (동위원소희석법 HRGC/HRMS에 의한 식품 중 Co-planar PCBs 분석)

  • Choi, Dongmi;Suh, Junghyuck;Kim, Minjung;Hong, Mooki;Kim, Changmin;Song, Insang
    • Analytical Science and Technology
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    • v.16 no.4
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    • pp.325-332
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    • 2003
  • To analyze co-planar PCBs in food, the isotopic dilution method by high resolution gas chromatography/high resolution mass spectrometry was applied. Among 209 PCB congeners, 12 congeners (#77, #81, #126, #169, #105, #114, #118, #123, #156, #157, #167 and #189) were chosen as target compounds that were toxic congeners re-assessed by WHO in 1998. Milk and milk products including cheese and butter were collected as food samples. Samples were homogenized, spiked with the known amount of the standard mixture and extracted. After extraction, extracts were cleaned up by sulfuric acid impregnated silica gel, purified on silica gel and alumina column chromatography and then analyzed by HRGC/HRMS. As results, the overall recoveries were ranged from 83% to 106% and the limit of detection was about 0.1 pg/g at signal/noise>3. Levels of targets in the selected food samples were 0.001~0.107 pgWHO-TEQ/g.

Fast and Accurate Determination of Algal Toxins in Water using Online Preconcentration and UPLC-Orbitrap Mass Spectrometry (온라인 시료주입과 UPLC-Orbitrap 질량분석법을 이용한 수질 조류독소의 고속분석방법 개발 및 환경시료적용)

  • Jang, Je-Heon;Kim, Yun-Seok;Choi, Jae-Won
    • Journal of Korean Society on Water Environment
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    • v.28 no.6
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    • pp.843-850
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    • 2012
  • Due to the fast response to algae bloom issue in drinking water treatment plant, very fast determination methodology for algal toxin is required. In this study, column switching technique based online preconcentration method was combined with high resolution full scan mass spectrometer to save sample preparation time and to obtain fast and accurate result. After parameter optimization of online preconcentration, 1mL filtered sample was directly injected to trap column with switching valve system. Next, target toxins are eluted by 98% acetonitrile and analysed with 150 - 1,100 amu scan range at 50,000 resolving power. Method detection limit (MDL) for microcystin-LR, the most toxic isomer, was 0.1 ng/mL and others such as microcystin-YR, microcystin-RR and nodularin were 0.08, 0.03 and 0.04 ng/mL, respectively. This is the best improved sensitivities with 1mL volume in the literature. Furthermore, due to the use of ultra pressure HPLC (UPLC), the whole method run was completed in 4 min. Real sample applications for 173 sample including 55 surface water and 118 treatment plant samples for raw and treated water could be done within 16 hours. In our calculation, this methodology is roughly 80% faster than the previous manual solid-phase extraction with LC-MS/MS method.

Isolation and Identification of Newly Isolated Antagonistic Streptomyces sp. Strain AP19-2 Producing Chromomycins

  • Wu, Xue-Chang;Chen, Wei-Feng;Qian, Chao-Dong;Li, Ou;Li, Ping;Wen, Yan-Ping
    • Journal of Microbiology
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    • v.45 no.6
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    • pp.499-504
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    • 2007
  • A new antagonistic strain of actinomycete, designated AP19-2, was isolated from the feces of giant pandas inhabiting the Foping National Nature Reserve in China. Cultural characteristic studies strongly suggested that this strain is a member of the genus Streptomyces. The nucleotide sequence of the 16S rRNA gene of strain AP19-2 evidenced profound similarity (97-99 %) with other Streptomyces strains. Two pure active molecules were isolated from a fermentation broth of Streptomyces sp. strain AP19-2 via extraction, concentration, silica gel G column chromatography, and HPLC. The chemical structures of the two related compounds (referred to as chromomycin $A_2$ and chromomycin $A_3$) were established on the basis of their Infrared spectra (IR), High Resolution Electrospray Ionization Mass Spectrometry (HR-ESI-MS), and Nuclear Magnetic Resonance (NMR) data, and by comparison with published data.

Catalytic oxidation kinetics of iron-containing carbon particles generated from diesel-sprayed hydrogen-air diffusion flame (디젤-분무 수소-공기 확산화염에서 생성된 철-함유 탄소입자의 촉매 산화반응 특성)

  • Kim, Yongho;Kim, Yong-Tae;Kim, Soo Hyung;Lee, Donggeun
    • Particle and aerosol research
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    • v.4 no.2
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    • pp.51-67
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    • 2008
  • In this study, we devoted to kinetic measurement of the catalytic oxidation of iron-containing flame soot particles and better understanding the role of catalytic particles on carbon oxidation in particular at low temperature, targeting on autothermal regeneration of diesel particulate filter by diesel exhaust gas. Carbon-based Fe-containing particles generated by spraying ferrocene-doped diesel fuel in an oxy-hydrogen flame are tested and compared with a commercial carbon black powder for thermogravimetric analysis (TGA), secondary ion mass spectrometry (SIMS), Fourier-transform infrared spectroscopy (FTIR), Induced coupled plasma-Atomic emission spectroscopy (ICP-AES), and High-resolution transmission electron microscopy (HR-TEM). As a result, we found that a small amount of the ferrocene addition led to significant reductions in a on-set temperature and an activation energy of the carbon oxidation as well. An oxygenated surface complex forming at the particle surface could be thought as active species that would be readily consumed in particular at low temperature.

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