• Title/Summary/Keyword: Alpha Spectrometry

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Di- and Triorganotin(IV) Complexes of Sulfur-containing Ylidenemalonates

  • Jung, Ok-Sang;Lee, Young-A;Hong, Jong-Ki;Jeong, Jong-Hwa;Sohn, Youn-Soo
    • Bulletin of the Korean Chemical Society
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    • v.14 no.6
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    • pp.722-726
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    • 1993
  • Organotin(IV) complexes of ylidenemalonates $(R_xSn)_{x-1}(O_2C)_2C=C(SR')_2\;(R=n-C_4H_9,\;C_6H_5,\;cyclo-C_6H_{11},\;CH_3OOCCH_2CH_2;\;x=2,3;\;R'=CH_3,\;R_2'=-CHCH-,\;-CH_2CH_{2^-})$ have been synthesized and characterized by means of various spectroscopic methods. The X-ray crystal structure of $(Ph_3Sn)_2(O_2C)_2C=C(SCH_3)_2$ has been determined (Pi; a= 9.704(2) ${\AA}$, b= 14.412(1) ${\AA}$, c= 14.760(3) ${\AA}$, ${alpha}$=74.26(1)$^{\circ}$, ${beta}$=99.38(l)$^{\circ}$, ${\gamma}$=79.09(1)$^{\circ}$, $V= 1950.7(7){\AA}^3$) and refined to R= 0.045. The crystal structure discloses a discrete molecule with bidentate-like carboxylate ligand. For diorganotin analogues, the structures are discussed in terms of IR, $^1H-NMR,\;^{13}C-NMR$, and FAB mass spectrometry. The mass spectrum indicates that the diorganotin complexes of ylidenemalonates are dimeric.

Proteomic Analysis on Exosomes Derived from Patients, Sera Infected with Echinococcus granulosus

  • Wang, Wen;Zhou, Xiaojing;Cui, Fang;Shi, Chunli;Wang, Yulan;Men, Yanfei;Zhao, Wei;Zhao, Jiaqing
    • Parasites, Hosts and Diseases
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    • v.57 no.5
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    • pp.489-497
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    • 2019
  • Cystic echinococcosis (CE), a zoonotic disease caused by Echinococcus granulosus at the larval stage, predominantly develops in the liver and lungs of intermediate hosts and eventually results in organ malfunction or even death. The interaction between E. granulosus and human body is incompletely understood. Exosomes are nanosized particles ubiquitously present in human body fluids. Exosomes carry biomolecules that facilitate communication between cells. To the best of our knowledge, the role of exosomes in patients with CE is not reported. Here, we isolated exosomes from the sera of patients with CE (CE-exo) and healthy donors and subjected them to liquid chromatography-tandem mass spectrometry analysis. Proteomic analysis identified 49 proteins specifically expressed in CE-exo, including 4 proteins of parasitic origin. The most valuable parasitic proteins included tubulin alpha-1C chain and histone H4. And 8 proteins were differentially regulated in CE-exo (fold change>1.5), as analyzed with bioinformatic methods such as annotation and functional enrichment analyses. These findings may improve our understanding about the interaction between E. granulosus and human body, and may contribute to the diagnosis and prevention of CE.

A MALDI-MS-based Glucan Hydrolase Assay Method for Whole-cell Biocatalysis

  • Ahn, Da-Hee;Park, Han-Gyu;Song, Won-Suk;Kim, Seong-Min;Jo, Sung-Hyun;Yang, Yung-Hun;Kim, Yun-Gon
    • Microbiology and Biotechnology Letters
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    • v.47 no.1
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    • pp.69-77
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    • 2019
  • Screening microorganisms that can produce glucan hydrolases for industrial, environmental, and biomedical applications is important. Herein, we describe a novel approach to perform glucan hydrolase screening-based on analysis of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) spectra-which involves degradation of the oligo- and polysaccharides. As a proof-of-concept study, glucan hydrolases that could break down glucans made of several glucose units were used to demonstrate the MALDI-MS-based enzyme assay. First, the enzyme activities of ${\alpha}$-amylase and cellulase on a mixture of glucan oligosaccharides were successfully discriminated, where changes of the MALDI-MS profiles directly reflected the glucan hydrolase activities. Next, we validated that this MALDI-MS-based enzyme assay could be applied to glucan polysaccharides (i.e., pullulan, lichenan, and schizophyllan). Finally, the bacterial glucan hydrolase activities were screened on 96-well plate-based platforms, using cell lysates or samples of secreted enzyme. Our results demonstrated that the MALDI-MS-based enzyme assay system would be useful for investigating bacterial glucoside hydrolases in a high-throughput manner.

Determination of Heterocyclic Amines in Roasted Fish and Shellfish by Liquid Chromatography-Electrospray Ionization/Mass Spectrometry (Liquid chromatography-mass spectrometry를 이용한 가열 조리된 어패류에서의 heterocyclic amines 함량 분석)

  • Lee, Jae-Hwan;Back, Yoo-Mi;Lee, Kwang-Geun;Shin, Han-Seung
    • Korean Journal of Food Science and Technology
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    • v.41 no.3
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    • pp.326-333
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    • 2009
  • Heterocyclic aromatic amines (HCAs) are mutagenic and carcinogenic substances that are formed during the heating of protein-rich foods. HCAs are generally found at low amounts in a complex matrix, which requires sophisticated analysis. In this study, HCAs were extracted from lyophilized fish and shellfish samples using solid-phase extraction (SPE) and determined by liquid chromatography-electrospray ionization/mass spectrometry (LC-ESI-MS). The HCA recoveries in the fish and shellfish ranged from 15.7 to 74.7% with standard deviations from 0.2 to 7.63%. And HCA concentrations ranged from 0.8 to 1,117.7 $ng/g^{-1}$ in cooked food samples. 1-methyl-9H-pyrido[3,4-b]indole (Harman), 9H-pyrido[3,4-b]indole (Norharman), and 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) were the most abundant HCAs formed in the muscle of fried mackerel, at levels of 1,117.7, 926.6, and 133.7 ng/g, respectively. 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2), 2-aminodipiryrido[1,2-a:3,2-d]imidazole(Glu-P-2), 2-amino-9H-pyrido[2,3-b]indole(A${\alpha}$C), 2-amino-3methyl-9H-pyrido [1,2-a:3,2-d]imidazole(MeA${\alpha}$C), 2-amino-3,4,7,8-tetramethylimidazo[4,5-f]quinoxaline (TriMeIQx), 2-amino-3,7,8-trimethylimidazo [4,5-f]quinoxaline(7,8-DiMeIQx), and 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx) were only detected by small quantities ranged from 1.5 to 98.6 ng/g. Overall, this study provides useful information on HCA levels in fish and shellfish products consumed in Korea.

Preparation of Liquefied Cellulose and Analysis of Its Components by GC-MS Spectrometry (액화셀룰로오스의 제조 및 GC-MS에 의한 그 성분 분석)

  • 조국란;황병호;공영토;도금현
    • Journal of Korea Foresty Energy
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    • v.19 no.2
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    • pp.86-92
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    • 2000
  • The liquefactions of $\alpha$-cellulose(Sigma Chemical, C-8002, 47H0383) was prepared in the presence of phenol using sulfuric acid as a catalyst under $N_2$ gas protection at $180^{\circ}C$ for 60minutes to examine its components. The ratio of $\alpha$-cellulose to phenol was 1: 6.2(w/w), and that to sulfuric acid was 1: 0.05(g/$m\ell$). The yields of liquefaction were calculated after the liquefied mixtures were passed through 1G4 glass filter. The luquefied product of $\alpha$-cellulose was analyzed using GC-MS Spectormeter. The 12 compounds identified by GC-MS Spectrometer, of which peak area covers 54% as 2,4-dimethyl phenol, p-isopropyl phenol, 1-ethyl-3,5-dimethyl benzene, o-isopropyl phenol, (E)-2,4\` dihydroxy-stilbene, 2,2\`-methylene-bisphenol, 4,4\`-methylenebisphenol, 3-methyl-2-hydroxyphenyl-(E)-2-hydroxyl-4\`-methoxy-stilbene, 1-phyenyl-1-(4\`hydroxyphenyl)methanol phenol derivatives. From this results, the reaction pathways of the liquefaction of cellulose were proposed through electrophilic substitution reaction. Phenol as a solvent might react with the reaction intermediates as well in the cellulose liquefaction.

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A Study of $^{222}Rn\;and\;^{226}Ra$ Analysis in the Groundwater by LSC (액체섬광계수기에 의한 지하수중의 $^{222}Rn$$^{226}Ra$ 분석법 연구)

  • Woo, Hyung-Joo;Yoon, Yoon-Yeol;Cho, Soo-Young;Chun, Sang-Ki
    • Journal of Radiation Protection and Research
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    • v.20 no.4
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    • pp.275-283
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    • 1995
  • PERALS(Photon Electron Rejecting Alpha Liquid Scintillation) spectrometry coupled with solvent extraction method has been set up for the analysis of $^{222}Rn\;and\;^{226}Ra$ in the groundwater. This analytical method offers low background, better energy resolution and lower quenching problem than the other techniques. By the analysis of NIST SRM 4966 $^{226}Ra$ standard, the analytical accuracy and precision were found to be 3% and 1%, respectively, and the relative standard deviation of the recovery of Rn extraction between pH2 and pH10 was 7%. Detection limits of $^{222}Rn$ and $^{226}Ra$ for 10 hours counting were counted to be $0.42 pCi/{\iota}\;and\;0.016 pCi/{\iota}$, respectively. For the test analysis of $^{222}Rn\;and\;^{226}Ra$ in the graundwater, hot spring water samples of 17 regions were analyzed. The concentration of $^{222}Rn$ were in the range of $90{\sim}5200pCi/{\iota}$ and average value was $1470pCi/{\iota}\;^{226}Ra$ concentration showed a peak value of $97.9pCi/{\iota}$ in a Kangwon region, but the average value was $1.14pCi/{\iota}$ except that region.

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Comparison of Volatile Compounds Identified in Different Parts of Peucedanum japonicum Thunberg by Harvest Time (방풍나물의 수확시기에 따른 부위별 향기성분 비교 분석)

  • Jung, Bok-Mi;Shin, Tai-Sun;Heo, Young-Ran
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.12
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    • pp.1871-1880
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    • 2014
  • Headspace volatile compounds of leaf, stem, and root of Peucedanum japonicum Thunberg (PJT) harvested in March and July were isolated, separated, and identified by using a combined system of solid phase microextraction and gas chromatography/mass spectrometry. Identified numbers of volatile compounds were 72, 75, and 63 in March PJT as well as 78, 73, and 69 in July, respectively. Total compounds identified from PJT consisted of alcohols (1~7), aldehydes (7~15), esters (1~4), hydrocarbons (5~9), ketones (1~2), monoterpenes (13~16), monoterpene alcohols (1~5), monoterpene aldehydes (2~4), monoterpene esters (1~4), monoterpene ketones (1~2), sesquiterpenes (16~24), and miscellaneous compounds (2~3). Major volatile compounds of PJT were monoterpenes at all harvest times and in all parts of PJT. The amounts of ${\beta}$-pinene in leaf and stem harvested in March were highest in monoterpenes, followed by ${\alpha}$-pinene and ${\beta}$-myrcene. However, amounts of volatile compounds of monoterpenes in leaf and stem from July PJT were in the decreasing order of ${\beta}$-pinene, ${\beta}$-phellandrene, and ${\beta}$-myrcene. Of the 39 sesquiterpenes identified in PJT, (E)-caryophyllene in March leaf was the most abundant volatile compound, followed by acoradiene in March leaf, ${\beta}$-elemene, and ${\alpha}$-copaene in July stem.

Method Development for the Profiling Analysis of Urine Globotriaosylceramide (Gb3) for the Screening of Fabry Disease by Tandem Mass Spectrometry (ESI-MS/MS를 이용한 소변 중 Globotriaosylceramide(Gb3)의 정량 및 임상 응용; 패브리병(Fabry) 진단)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Kang, Seung-Woo;Kwon, Young-Joo;Jeong, Choon-Sik;Lee, Yong-Soo
    • YAKHAK HOEJI
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    • v.51 no.2
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    • pp.96-102
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    • 2007
  • Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

Volatile Components of Flower and Seed of Safflower (홍화꽃 및 홍화씨의 휘발성성분)

  • Choi, Sung-Hee;Im, Sung-Im;Jang, Eun-Young;Cho, Young-Su
    • Korean Journal of Food Science and Technology
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    • v.36 no.2
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    • pp.196-201
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    • 2004
  • Volatile components in flower and seed of safflower were identified. Volatile flavor compounds of safflower (Carthamus tinctorius L.) was extracted by simultaneous steam distillation and extraction method using Likens and Nickerson's extraction apparatus. Concentrated extract was analyzed and identified by gas chromatography and GC-mass spectrometry. Main volatile components in flower were terpene compounds, including p-cymene, limonene, ${\alpha}-phellandrene$, ${\gamma}-terpinene$, camphor, 4-terpineol, selinene, ${\beta}-caryophyllene$, torreyol, ${\beta}-eudesmol$, and 10 acids including 3-methylbutanoic acid, 2-methylbutanoic acid, and acids of $C_{2},\;C_{5}-C_{11}$. Main volatile components in seed and safflower were 20 aldehydes including hexanal (7.17%), (E)-2-heptenal (1.10%), (E,Z)-2,4-decadienal and (E,E)-2,4-decadienal.

Studies on Biological Activity of Wood Extractives(II) - Antimicrobial and antioxidative compound isolated from heartwood of Zelkova serrata - (수목추출물의 생리활성에 관한 연구(II) -느티나무 심재의 항균 및 항산화물질-)

  • Lee, Sung-Suk;Choi, Don-Ha;Lee, Hak-Ju;Kang, Ha-Young
    • Journal of the Korean Wood Science and Technology
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    • v.28 no.2
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    • pp.32-41
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    • 2000
  • Antimicrobial and antioxidative activities on heartwood extractives from Zelkova serrata were investigated to develop a natural fungicide or preservative. The ethanol extract from Z. serrata was fractionated in the order of petroleum ether, diethylether and ethylacetate to determine antimicrobial activity. The highest antimicrobial activity against the tested microorganisms was found in the petroleum ether soluble fraction. An active antimicrobial compound was isolated from petroleum ether soluble fraction, and identified as 7-hydroxy-3-methoxycadalene by $^1H$-, $^{13}C$-NMR and EI-MS spectrometry. This compound showed higher antifungal activity, but lower antibacterial activity than hinokitiol(${\beta}$-thujaplicin), strong antimicrobial compound isolated from Thujopsis dolabrata. Antioxidative activity was also higher than ${\alpha}$-tocopherol and similar to BHT(butylated hydroxytoluene), one of the strongest synthetic antioxidant. As a result, it was concluded that 7-hydroxy-3-methoxycadalene isolated from Z. serrata had strong antifungal and antioxidative activities.

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