• Title/Summary/Keyword: alpha spectrometry

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Analysis of Branched PEG-Conjugated Interferon Alpha by Capillary Electrophoresis and MALDI- TOF Mass Spectrometry

  • Na, Dong-Hee;Park, Eun-Ji;Lee, Snag-Deuk;Jo, Young-Woo;Lee, Sung-Hee;Kim, Won-Bae;Lee, Kang-Choon
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.406.3-407
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    • 2002
  • Analysis of interferon alpha (IFN) modified with high molecular weight branched PEG was performed by capillary electrophoresis (CE) and MALDI-TOF mass spectrometry (MALDI-TOF MS). IFN was modified by the reaction of amine residues with an active ester of monomethoxy polyethylene glycol at various molar ratios. As a CE method. capilary electrophoresis sodium dodecyl sulfate nongel sieving (CE-SDS NGS) was performed using an uncoated capilary filled with a hydrophilic replaceable polymer network matrix. (omitted)

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Comparative Chemical Composition of Domestic and Imported Chrysanthemum indicum L. Flower Oils

  • Chang, Kyung-Mi;Kim, Gun-Hee
    • Food Science and Biotechnology
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    • v.18 no.5
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    • pp.1288-1292
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    • 2009
  • Volatile flavor compounds were isolated from the flowers of Chrysanthemum indicum L. (gamguk) produced in Korea and China by the hydro distillation, and were analyzed by gas chromatography-mass spectrometry (GC/MS). The yield of oils from Korean and Chinese gamguk were 2.0 and 0.5%(v/w), respectively. Sixty-three volatile compounds of Korean gamguk representing 89.28% of the total peak area were tentatively identified, including 35 hydrocarbons, 12 alcohols, 6 ketones, 3 esters, 5 aldehydes, 1 oxide, and 1 miscellaneous component. Thirty-six volatile components of Chinese gamguk constituted 58.15% of the total volatile composition were tentatively characterized, consisting of 19 hydrocarbons, 7 alcohols, 2 ketones, 2 esters, 4 aldehydes, 1 oxide, and 1 miscellaneous component. The predominant components of Korean oil were ${\alpha}$-pinene, 1,8-cineol, and chrysanthenone. Whereas, camphor, ${\alpha}$-curcumene, and ${\beta}$-sesquiphellandrene were the main aroma compounds of Chinese gamguk.

Sterol Compositions in Some Cucurbitaceae Vegetable Oils (몇가지 박과 식물 종자유중의 Sterol 조성)

  • Tae Myoung Jeong;Min Suk Yang;Taro Matsumoto
    • Journal of the Korean Chemical Society
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    • v.21 no.3
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    • pp.193-203
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    • 1977
  • Three sterol fractions; 4-desmethyl-, 4-monomethyl-, and 4,4-dimethylsterol, separated by thin layer chromatography from the unsaponifiables of five Cucurbitaceae (cucumber, watermelon, sponge cucumber, gourd and snake gourd) seed oils were analyzed by gas liquid chromatography and combined gas liquid chromatography-mass spectrometry. ${\alpha}$-Spinasterol, ${\Delta}^{7,22,25}$-stigmastatrienol and ${\Delta}^{7,25}$-stigmastadienol isolated from the 4-desmethylsterol fraction were identified by IR, NMR and mass spectrometry.

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Screening Analysis of 10 Adrenal Steroids by Matrix-Assisted Laser Desorption Ionization-Tandem Mass Spectrometry

  • Kim, Sun-Ju;Jung, Hyun-Jin;Chung, Bong-Chul;Choi, Man-Ho
    • Mass Spectrometry Letters
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    • v.2 no.3
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    • pp.69-72
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    • 2011
  • Defective synthesis of the steroid hormones by the adrenal cortex has profound effects on human development and homeostasis. Due to the time-consuming chromatography procedure combined with mass spectrometry, the matrix-assisted laser desorption ionization method coupled to the linear ion-trap tandem mass spectrometry (MALDI-LTQ-MS/MS) was developed for quantitative analysis of 10 adrenal steroids in human serum. Although MALDI-MS can be introduced for its applicability as a high-throughput screening method, it has a limitation on reproducibility within and between samples, which renders poor reproducibility for quantification. For quantitative MALDI-MS/MS analysis, the stable-isotope labeled internal standards were used and the conditions of crystallization were tested. The precision and accuracy were 3.1~35.5% and 83.8~138.5%, respectively, when a mixture of 10 mg/mL ${\alpha}$-cyano-4-hydroxycinnamic acid in 0.2% TFA of 70% acetonitrile was used as the MALDI matrix. The limit of quantification ranged from 5 to 340 ng/mL, and the linearity as a correlation coefficient was higher than 0.988 for all analytes in the calibration range. Clinical applications include quantitative analyses of patients with congenital adrenal hyperplasia. The devised MALDI-MS/MS technique could be successfully applied to diagnosis of clinical samples.

Determination of trace actinide (Am, Pu, Th, U) using alpha spectrometry and neutron activation analysis (알파분광법과 중성자방사화분석법에 의한 극미량의 악티늄계원소 (Am, Pu, Th, U)분석연구)

  • Yoon, Yoon Yeol;Lee, Kil Yong;Cho, Soo Young;Kim, Yongjai;Lee, Myong Ho
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.302-307
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    • 2004
  • Determination of actinides in the environmental sample requires separation of each element. This procedure is tedious and time consuming. And also, the detection limits of some nuclides using alpha spectrometry are rather higher. To overcome the lower detection limit and complicated separation procedure, a simple analytical technique for the determination of actinide isotopes in the environmental samples was developed and applied to IAEA and NIST reference sediment samples. For the separation of actinides from matrix, anion exchange resin and TRU-spec extraction chromatography resin were used and chemical yields were obtained using natural uranium, thorium, $^{242}Pu$ and $^{243}Am$ tracers. For overcoming the higher detection limits of U and Th in alpha spectrometry, neutron activation analysis was applied. Using combined method, the detection limit was increased about 10 times. The activity values of each isotope were consistent with the reference values reported by IAEA and NIST.

Development of Gas Chromatography/Mass Spectrometry for the Determination of Essential Fatty Acids in Food Supplemental Oil Products

  • Ahn, Seonghee;Yim, Yoon-Hyung;Kim, Byungjoo
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.75-78
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    • 2013
  • A gas chromatography/mass spectrometric (GC/MS) method was developed as a candidate reference method for the accurate determination of essential fatty acids (linoleic acid, ${\alpha}$- and ${\gamma}$-linolenic acids) in food supplemental oil products. Samples were spiked with three internal standards (stearic acid-$d_{35}$, $^{13}C_{18}$-linoleic acid, and $^{13}C_{18}$-${\alpha}$-linolenic acid). Samples were then subject to saponification, derivatization for methylation, and extraction by organic solvent. For GC/MS measurement, an Agilent HP-88 column, designed for the separation of fatty acid methyl esters, was selected after comparing with other columns as it provided better separation for target analytes. Target analytes and internal standards were detected by selected ion monitoring of molecular ions of their methyl ester forms. The GC/MS method was applied for the measurement of three botanical oils in NIST SRM 3274 (borage oil, evening primrose oil, and flax oil), and measurement results agreed with the certified values. Measurement results for target analytes which have corresponding isotope-labeled analogues as internal standard were calculated based on isotope dilution mass spectrometry (IDMS) approach, and compared with results calculated by using the other two internal standards. Results from the IDMS approach and the typical internal standard approach were in good agreement within their measurement uncertainties. It proves that the developed GC/MS method can provide similar metrological quality with IDMS methods for the measurement of fatty acids in natural oil samples if a proper fatty acid is used as an internal standard.

Electrodeposition of $^{237}Np$ for Alpha Spectrometry and Application to Spent Nuclear Fuel Samples (알파분광분석법에 의한 $^{237}Np$ 정량 및 사용후핵연료 시료에의 적용)

  • Joe Kih-Soo;Kim Jung-Suck;Han Sun-Ho;Park Yeong-Jai;Kim Won-Ho
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.4 no.2
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    • pp.95-102
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    • 2006
  • Alpha spectrometry was studied for the determination of $^{237}Np$ in spent nuclear fuel samples. The optimum condition for the electrodeposition of $^{237}Np$ was obtained as follows : for $1{\sim}1.5$ hour of deposition time, at the current intensity of $1.2{\sim}1.5$ A and at sodium sulfate electrolyte without organic additive. The deposition yield and its reproducibility on $^{237}Np$ was decreased as the amount of $^{237}Np$ decreased from 4.16 Bq down to 0.0264 Bq(1ng). The recovery yield of $^{237}Np$ determined by alpha spectrometry after separation in synthetic solution was $98.8{\pm}5.1%$(n=4). The contents of $^{237}Np$ in spent nuclear fuel samples were determined and the result showed an agreement within 10% of a difference between the measurement and the calculation.

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