• Title/Summary/Keyword: Spectrometric data

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Integracide K: A New Tetracyclic Triterpenoid from Desmodium uncinatum (Jacq.) DC. (Fabaceae)

  • Tsafack, Borice Tapondjou;Ponou, Beaudelaire Kemvoufo;Teponno, Remy Bertrand;Nono, Raymond Ngansop;Jenett-Siems, Kristina;Melzig, Matthias F.;Park, Hee Juhn;Tapondjou, Leon Azefack
    • Natural Product Sciences
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    • v.23 no.2
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    • pp.113-118
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    • 2017
  • A new tetracyclic triterpenoid [4,4,24-trimethylcholesta-${\Delta}^{8,9;14,5;24,28}$-trien-$3{\beta},11{\beta},12{\alpha}$-triol-12-acetate, 3-sulfate] sodium salt (1), together with eight known compounds including ergosterol $5{\alpha},8{\alpha}$-endoperoxide (2), 1,9-dihydroxy-3-methoxy-2-methylpterocarpan (3), 3-O-${\beta}$-D-2-acetyl-amino-2-deoxyglucopyranoxyloleanoic acid (4), hydnocarpin (5), derrone (6), isovitexin (7), erythrinin C (8), and 5,4'-dihydroxy-2"-hydroxyisopropyldihydrofurano [4,5:7,8]-isoflavone (9), were isolated from the EtOAc soluble fraction of the methanol extract of aerial part of Desmodium uncinatum collected in the western highland of Cameroon. The structures of these compounds were established by comprehensive interpretation of their spectral data mainly including 1D- ($^1H$ and $^{13}C$), 2D-NMR($^1H$-$^1H$ COSY, HMQC, HMBC) spectroscopic and ESI-TOF-MS mass spectrometric analysis. The isolation of an integracide-like compound from plant origin is a very unusual finding.

Comparative Proteomic Analysis of Human Amniotic Fluid Supernatants with Down Syndrome Using Mass Spectrometry

  • Park, Ji-Sook;Cha, Dong-Hyun;Jung, Jin-Woo;Kim, Young-Hwan;Lee, Sook-Hwan;Kim, Young-Jun;Kim, Kwang-Pyo
    • Journal of Microbiology and Biotechnology
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    • v.20 no.6
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    • pp.959-967
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    • 2010
  • Down syndrome (DS) is an abnormality of the 21st chromosome that commonly occurs in children born to older women. Thus, amniotic fluid (AF) is usually collected from such women for prenatal diagnosis. This study analyzed human AF supernatants (AFS) using a mass spectrometric (MS) approach to search for candidate biomarkers of a DS pregnancy. The AFS were collected from older pregnant women at weeks 16-18 of their gestation by amniocentesis for cytogenetic analysis. The AFS from the pregnancies carrying DS (n=4) or chromosomally normal (n=6) fetuses, as revealed by the cytogenetic analysis, were then subjected to global protein profiling based on liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS). Affinity chromatography was also applied prior to the LC-ESI-MS/MS to minimize the masking effect of highly abundant albumin and immunoglobulin and thereby increase the diversity of the identified proteins. As a result, at least 30 new AFS proteins were identified and 44 AFS proteins were found to be differentially expressed between the DS and normal cases, where 6 of the proteins were unique to the DS cases and 11 were unique to the chromosomally normal cases. In addition, in the DS cases, 19 AFS proteins were downregulated and 8 were upregulated to varying degrees. A Western blot analysis confirmed the LC-ESI-MS/MS data, indicating that the combined detection of apolipoprotein A-II (apoA-II) and alpha-fetoprotein (AFP) could be a potential tool for diagnosing DS cases.

Systematic Studies of 12S Seed Storage Protein Accumulation and Degradation Patterns during Arabidopsis Seed Maturation and Early Seedling Germination Stages

  • Li, Qing;Wang, Bai-Chen;Xu, Yu;Zhu, Yu-Xian
    • BMB Reports
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    • v.40 no.3
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    • pp.373-381
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    • 2007
  • Seed storage proteins (SSPs) are important for seed germination and early seedling growth. We studied the accumulation and degradation profiles of four major Arabidopsis 12S SSPs using a 2-DE scheme combined with mass spectrometric methods. On the 2-DE map of 23 dpa (days post anthesis) siliques, 48 protein spots were identified as putative full-length or partial $\alpha$, $\delta$ subunits. Only 9 of them were found in 12 dpa siliques with none in younger than 8 dpa siliques, indicating that the accumulation of 12S SSPs started after the completion of cell elongation processes both in siliques and in developing seeds. The length and strength of transcription activity for each gene determined the final contents of respective SSP. At the beginning of imbibition, 68 SSP spots were identified while only 2 spots were found at the end of the 4 d germination period, with $\alpha$, subunits degraded more rapidly than the $\alpha$ subunits. The CRC $\delta$ subunit was found to degrade from its C-terminus with conserved sequence motifs. Our data provide an important basis for understanding the nutritional value of developing plant seeds and may serve as a useful platform for other species.

Principles of Re-Os Isotopic System and Dating the Age of the Subcontinental Lithospheric Mantle Beneath Korean Peninsula (Re-Os 동위원소 시스템의 원리와 한반도 하부지각맨틀의 연령)

  • Lee Seung-Ryeol
    • The Journal of the Petrological Society of Korea
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    • v.15 no.2 s.44
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    • pp.106-117
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    • 2006
  • Re-Os isotopic system, based on the long-lived $\beta^-$ transition of $^{187}Os(\lambda=1.67\times10^{-11}year^{-1})$ is being widely used in cosmochemistry and geochemistry. Along with the development of elemental separation and mass-spectrometric technique, the Re-Os isotopic system, like Sm-Nd, Rb-Sr, U-Th-Pb isotopic system, is now conventionally applied as a useful tool for absolute dating and isotoptc tracers. This paper introduces brief principles of Re-Os isotopic system and presents the general methodology fur dating the formation age of the subcontinental lithospheric mantle, based on the Re-Os isotopic data of the mantle xeonliths from South Korea.

Simultaneous Determination of Asperosaponins and Iridoid Glycosides from Dipsaci Radix by Using LC-ESI-MS Spectrometry (속단(Dipsaci Radix) 중 Asperosaponins 및 Iridoid glycosides의 LC-ESI-MS에 의한 동시분석)

  • Cho, Hwang-Eui;Son, In-Seop;Kim, Sun-Cheun;Son, Kun-Ho;Woo, Mi-Hee;Moon, Dong-Cheul
    • Korean Journal of Pharmacognosy
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    • v.43 no.2
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    • pp.137-146
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    • 2012
  • Dipsaci Radix (Dipsacaceae) has been used as a tonic, an analgesic, anti-inflammatory and anti-complement agents in traditional herbal medicine for the therapy of low back pain, knee pain, rheumatic arthritis, traumatic hematoma, and bone fractures. A high-performance liquid chromatography-electrospray ionization-mass spectrometric method (HPLC-ESI-MS) was developed for the simultaneous quantitation method of the five compounds from the herbal drug: asperosaponin VI and asperosaponin XII (terpene glycosides), sweroside, loganin and dipsacus A(iridoid glycosides). HPLC separation of the analytes was achieved on a C18 column ($150{\times}2.0$ mm i.d., 5 ${\mu}m$) using the aqueous methanol containing 5 mM ammonium acetate with gradient flow of the mobile phase. Detection of the analytes was performed by positive ion electrospray ionization, and selected ion monitoring was used for data acquisition using m/z corresponding molecular adduct ion, $[M+NH_4]^+$ and $[M+H]^+$. Calibration graphs showed good linearity ($r^2$=0.9997) over the wide range of the analytes; intra- and inter-day precisions (RSD, %) were within 9.1% and the accuracy between 94.0-111.0%. Recoveries of the analytes through the assay procedure were in the range of 93.7-110.8%. Analytical results of the herbal drugs of Dipsaci Radix (17 samples) show wide distribution of the five marker compounds and clear difference of the species from Phlomidis Radix (4 samples). The developed method would provide a practical guide for the quality control of the herbal drug.

Mass spectrometric studies of competitive binding of C60 and C70 to mesosubstituted porphyrins

  • Jung, Sung-Han;Shin, Seung-Koo
    • Mass Spectrometry Letters
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    • v.2 no.2
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    • pp.49-52
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    • 2011
  • Competitive binding of $C_{60}$ and $C_{70}$ to meso-substituted porphyrins was studied by mass spectrometry (MS). Electrospray ionization MS was employed to acquire the mass spectra of 1 : 1 porphyrin-fullerene complexes formed in a mixture of mesosubstituted porphyrin and fullerite to determine the ratio of complexes between $C_{60}$ and $C_{70}$. Matrix-free laser desorption ionization MS was used to obtain the mass spectra of fullerite to measure the mole fraction of $C_{60}$ and $C_{70}$. The binding constant ratio ($K_{70}$/$K_{60}$) was determined from the mass spectral data. The difference in standard Gibbs free energy change, ${\Delta}({\Delta}G^o)_{70-60}$, for the competitive binding of $C_{60}$ and $C_{70}$ was calculated from $K_{70}$/$K_{60}$. Of the five porphyrins, tetraphenyl, tetra(4-pyridyl), tetra(4-carboxyphenyl), tetra(3,5-di-tert-butylphenyl), and tetra(pentafluorophenyl) porphyrins, the first three non-bulky porphyrins yield negative values of ${\Delta}({\Delta}G^o)_{70-60}$, whereas the other two bulky porphyrins result in positive values of ${\Delta}({\Delta}G^o)_{70-60}$. This result indicates that $C_{70}$ binding to porphyrin is thermodynamically favored over $C_{60}$ binding in non-bulky porphyrins, but disfavored in bulky ones. It also suggests that the binding mode of $C_{70}$is different between non-bulky and bulky porphyrins, which is in line with previous experimental findings of the "side-on" binding to non-bulky porphyrins and the $C_{60}$-like "end-on" binding to bulky porphyrins.

Electrospray Tandem Mass Spectrometry for the Quantification and Bioavailability Test of Gliquidone in Human Plasma (Electrospray Tandem Mass를 이용한 혈중 글리퀴돈의 정량법 개발 및 생체이용률시험)

  • Moon Chul-Jin;Lee Eun-Hee;Yang Song-Hyun;Moon Hae-Ran
    • YAKHAK HOEJI
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    • v.49 no.3
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    • pp.212-216
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    • 2005
  • A rapid, sensitive and selective electrospray tandem mass spectrometric (ESI-LC/MS/MS) method for the quantitation of gliquidone in human plasma was developed. A bioavailability study of gliquidone tablet (30 mg gliquidone, Boehringer Ingelheim Korea Co.) was performed using the validated ESI-LC/MS/MS method. The dose of 30 mg of gliquidone (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 5, 7, 9, 12, 24, and 33 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $10\~1000 ng/ml$. The coefficient of variation for intra- and inter-day assay were $8.30\~18.86$, and $2.19\~12.92\%$, respectively. The lower limit of quantification for gliquidone was 10 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 3861.17$\pm$1328.61 ng-hr/ml, $C_{max}$ was 831.02$\pm$227.99 ng/ml, $T_{max}$ was $2.94{\pm}0.77 hr,\;K_e$, was 0.19$\pm$0.06 1/hr, and $t_{l/2}$ was 4.47$\pm$3.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of gliquidone dosage forms was prepared successfully and could be used for the bioequivalence test of gliquidone preparation.

Tandem Mass Spectrometry for the Quantification and Bioavailability Test of Nicorandil in Human Plasma (Tandem Mass를 이용한 혈중 니코란딜의 정량법 개발 및 생체이용률시험)

  • Moon Chul-Jin;Lee Eun-Hee;Yang Song-Hyun;Moon Hae-Ran
    • YAKHAK HOEJI
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    • v.49 no.3
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    • pp.225-229
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    • 2005
  • A rapid, sensitive and selective tandem mass spectrometric method (LC-MS/MS) for the quantitation of nicorandil in human plasma was developed. A bioavailability study of Sigmat tablet (5 mg nicorandil, Choongwae Co.) was per-formed using the validated LC-MS/MS method. The dose of 5 fig of nicorandil (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.25, 0.5, 1, 2, 3, 4, 5, 6, 9, 12, and 24 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $0.5\~200.0 ng/ml$. The coefficient of variation for intra- and inter-day assay were $3.55\~7.44$, and $2.17\~9.102\%$, respectively. The lower limit of quantification for nicorandil was 0.5 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 145.9$\pm$83.0 ng-hr/ml, Cmax was 83.8$\pm$32.2 ng/ml, $C_{max}$ was 0.42$\pm$0.13 hr, $K_e$ was 0.56$\pm$0.23 l/hr, and $t_{l/2}$ was 1.42$\pm$0.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of nicorandil dos-age forms was prepared successfully and could be used for the bioequivalence test of nicorandil preparation.

Human Multi-route Exposure Assessment of Lead and Cadmium for Korean Volunteers (일부 자원자를 통한 납, 카드뮴의 다경로 인체 노출평가)

  • Oh, Eun-Ha;Lim, Ho-Sub;Jang, Jae-Yeon;Lee, Eun-Il
    • Journal of Preventive Medicine and Public Health
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    • v.39 no.1
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    • pp.53-58
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    • 2006
  • Objectives: We wanted to evaluate the main route of exposure to lead and cadmium for the general population in Korea by using multi-route and multi-media exposure assessment Methods: Samples of air at the homes, samples of the food and water and peripheral blood samples were collected from thirty volunteers living in Seoul (the metropolitan area), Yong-in (the suburban area) and Ansan (the industrial area) in 2001. Graphite furnace atomic absorption spectrometric methods were used for the determination of the Pb and Cd levels in the air, food, water and blood samples. Results: The average intake of lead through the air, drinking water and food were $5.06{\mu}g/day\;(26.3%)\;0.002{\mu}g/day\;(0.1%),\;and\;16.4{\mu}g/day\;(73.6%)$, respectively. The average intake of cadmium through the air, drinking water and food were $0.082{\mu}g/day\;(0.9%),\;0.001{\mu}g/day\;(0.007%),\;and\;12.61 {\mu}g/day\;(99.0%)$, respectively. The blood lead level was statistically higher in the male subjects than in the female subjects (3.39 and $2.22{\mu}g/dl$, respectively), and only gender was a significant variable on the multiple regression analysis for blood lead. Conclusions: This study showed that the intake of lead and cadmium through food was the major route of exposure. A policy to reduce the pollutants according to the exposure routes should be established. However, more studies will be needed to support these data for the general population.

THE GEOMETRIC ALBEDO OF (4179) TOUTATIS ESTIMATED FROM KMTNET DEEP-SOUTH OBSERVATIONS

  • Bach, Yoonsoo P.;Ishiguro, Masateru;Jin, Sunho;Yang, Hongu;Moon, Hong-Kyu;Choi, Young-Jun;JeongAhn, Youngmin;Kim, Myung-Jin;Kwak, SungWon
    • Journal of The Korean Astronomical Society
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    • v.52 no.3
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    • pp.71-82
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    • 2019
  • We derive the geometric albedo of a near-Earth asteroid, (4179) Toutatis, to investigate its surface physical conditions. The asteroid has been studied rigorously not only via ground-based photometric, spectrometric, polarimetric, and radar observations but also via in situ observation by the Chinese Chang'e-2 space probe; however, its geometric albedo is not well understood. We conducted V-band photometric observations when the asteroid was at opposition in April 2018 using the three telescopes in the southern hemisphere that compose the Korea Microlensing Telescope Network (KMTNet). The observed time-variable cross section was corrected using the radar shape model. We find that Toutatis has a geometric albedo $p_V=0.185^{+0.045}_{-0.039}$, which is typical of S-type asteroids. We compare the geometric albedo with archival polarimetric data and further find that the polarimetric slope-albedo law provides a reliable estimate for the albedo of this S-type asteroid. The thermal infrared observation also produced similar results if the size of the asteroid is updated to match the results from Chang'e-2. We conjecture that the surface of Toutatis is covered with grains smaller than that of the near-Sun asteroids including (1566) Icarus and (3200) Phaethon.