• Title/Summary/Keyword: Alpha spectrometry

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Determination of oestrone, $17{\alpha}$-and $17{\beta}$-oestradiol in bovine aqueous humor using gas chromatography-negative ion chemical ionization mass spectrometry

  • Zafar-Iqbal;Midgley, John-M;Watson, David-G
    • Archives of Pharmacal Research
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    • v.20 no.3
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    • pp.247-252
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    • 1997
  • Perfluorotolyl (PFT)-ether and perfluorotoly-trimethylsilyl (PFT-TMS) ether derivatives of oestrone, $17{\alpha}$- and $17{\beta}$oestradiol were prepared under phase transfer conditons. The former derivatives under negative ion chemical ionization conditions gave significant ions in the mass spectrometer but $17{\alpha}$- and $17{\beta}$ -oestradiol gave poor resolution. However, the PFT-TMS derivatives of 17.${\alpha}$- and$17{\beta}$-oestradiol showed good resolution. These derivatives were used for the analysis of oestrogens in bovine aqueous humour, vitreous humour and retina. The mean $({\pm}SEM)$ concentrations of oestrone in bovine aqueous humour (n=18), vitreous humour (n=18) and bovine retina (n=4) were $0.47{\pm}0.11$, $0.46{\pm}0.14$ and $1.10{\pm}0.24 ng.ml^{-1}$, respectively. $17{\alpha}$-Oestradiol was detected in 16 out of 18 samples of bovine aqueous humour and vitreous humour and the mean $({\pm}SEM)$ concentrations were $0.30{\pm}0.10$ and $0.08{\pm}0.02 ng.ml^{-1}$, respectively. The mean $({\pm}SEM)$ concentration of 17.betha.-oestradiol in aqueous humour (n=7) and vitreous homour (n=11) $0.83{\pm}0.26 ng ml^{-1}$ and $0.39{\pm}0.09 ng ml^-1$, respectively. In retina the concentrations of both steroids were below the detection limit.

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Bio-assay Guided Isolation and Identification of α-Glucosidase Inhibitors from the Leaves of Diospyros lotus (고욤나무 잎으로부터 활성유도 분획법에 의한 α-Glucosidase 저해물질 분리 및 확인)

  • Kim, Sang Jun;Kim, Ji-Ae;Kim, Da Hye;Kwak, Seol Hwa;Yu, Kang-Yeol;Jang, Seon Il;Kim, Seon-Yeong;Jeong, Seung-Il
    • Korean Journal of Pharmacognosy
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    • v.46 no.2
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    • pp.105-108
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    • 2015
  • To establish the anti-diabetic(α-glucosidase inhibitory) activity of D. lotus leaf extract, isolate and identify the constituents responsible for the activity. The methanolic extract of leaves was partitioned between water, n-butanol and ethyl acetate. Bio-assay guided fractionation, based on inhibition of ;${\alpha}$-glucosidase, allowed isolation and identification of the active components. Liquid chromatography/mass spectrometry(LC/MS), 1 H-NMR and 13 C-NMR spectra analyses demonstrated that the active compound was myricetin-3-O-;${\alpha}$-L-rhamnoside(1). Compound 1 demonstrated a strong inhibition on the α-glucosidase, in vitro and ;${\alpha}$-glucosidase inhibitory value was calculated as 98.08%, when that of a reference drug, acarbose was estimated as 83.03%. The present study indicates compound 1 could be considered as an ;${\alpha}$-glucosidase inhibitor and developed as an important antidiabetes agent for type II diabetes therapy.

Proteomic Profiling of Serum from Stage I Lung Squamous Cell Carcinoma Patients

  • Li, Xin-Ju;Wu, Qi-Fei;He, Da-Lin;Fu, Jun-Ke;Jin, Xin
    • Asian Pacific Journal of Cancer Prevention
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    • v.14 no.4
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    • pp.2273-2276
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    • 2013
  • Objectives: This study employed proteomic profiling to identify specific tumor markers that might improve early diagnosis of lung squamous cell carcinoma. Methods: Serum samples were isolated from 30 patients with stage I lung squamous cell carcinoma and 30 age-and gender-matched healthy controls, and proteomic profiles were obtained by matrix-assisted laser desorption ionization time of flight mass spectrometry. Results: Three highly expressed potential tumor markers were identified in the sera of stage I lung squamous cell carcinoma patients, with molecular weights of 3261.69, 3192.07, and 2556.92 Da. One protein peak with molecular weight 3261.69 Da was chosen as the candidate biomarker and identified as a fibrinogen alpha chain through a search of the IPI, NCBI or SWISS-PROT protein databases. Conclusion: As a potential tumor biomarker, fibrinogen alpha chain may be applicable for the early diagnosis and prognosis of lung squamous cell carcinoma patients.

Yeast Elf1 Factor Is Phosphorylated and Interacts with Protein Kinase CK2

  • Kubinski, Konrad;Zielinski, Rafal;Hellman, Ulf;Mazur, Elzbieta;Szyszka, Ryszard
    • BMB Reports
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    • v.39 no.3
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    • pp.311-318
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    • 2006
  • One of the biggest group of proteins influenced by protein kinase CK2 is formed by factors engaged in gene expression. Here we have reported recently identified yeast transcription elongation factor Elf1 as a new substrate for both monomeric and tetrameric forms of CK2. Elf1 serves as a substrate for both the recombinant CK2$\alpha$' ($K_m$ 0.38 ${\mu}M$) and holoenzyme ($K_m$ $0.13\;{\mu}M$). By MALDI-MS we identified the two serine residues at positions 95 and 117 as the most probable in vitro phosphorylation sites. Co-immunoprecypitation experiments show that Elf1 interacts with catalytic ($\alpha$ and $\alpha$') as well as regulatory ($\beta$ and $\beta$') subunits of CK2. These data may help to elucidate the role of protein kinase CK2 and Elf1 in the regulation of transcription elongation.

Tentative Identification of Ginseng Flavor Components by Capillary Gas Chromatography and Mass Spectrometry (모세관(毛細管) GC/MS에 의한 인삼향기성분(人蓼香氣成分)의 일차적(一次的) 동정(同定))

  • Park, Nae-Joung;Kim, Man-Wook
    • Applied Biological Chemistry
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    • v.27 no.4
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    • pp.259-263
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    • 1984
  • Volatile flavor components of raw ginseng were collected from the manufacturing process of ginseng extract. Flavor components were separated by capillary column chromatography using SE-54 stationary phase and individual components were identified by means of GC/MS. Twenty six compounds including monoterpenes, esters, ethers, and sesquiterpenoids were tentatively identified. Major flavor components characteristic to ginseng appeared to he sesqiterpenoids such as ${\alpha}-gurjunene,\;{\beta}-maaliene,\;{\alpha}-guaiene,\;{\beta}-patchoulene$, (-)aromadendrene, and ${\beta}-elemene$.

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Chemical and Antimicrobial Properties of Essential Oils from Three Coniferous Trees Abies koreana, Cryptomeria japonica, and Torreya nucifera

  • Oh, Hyun-Jeong;Ahn, Hyo-Min;So, Kyoung-Ha;Kim, Sang-Suk;Yun, Pil-Yong;Jeon, Gyeong-Lyong;Riu, Key-Zung
    • Journal of Applied Biological Chemistry
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    • v.50 no.3
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    • pp.164-169
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    • 2007
  • Three coniferous essential oils were extracted from Abies koreana, Cryptomeria japonica, and Torreya nucifera by hydrodistillation. The chemical composition of each oil was analyzed by GCMS, and their antimicrobial activities were tested against two bacteria and one yeast strains. Fortyseven compounds were identified from A. koreana oil, 39 from C. japonica, and 59 from T. nucifera. Main components of the essential oils were limonene (23.5%), bornyl acetate (17.9%), ${\alpha}-pinene$ (11.1%), and camphene (10.2%) in A. koreana, kaurene (26.3%), ${\gamma}-eudesmol$ (19.0%), elemol (6.9%), and sabinene (5.1%) in C. japonica, limonene (13.5%), ${\delta}-cadinene$ (10.5%), ${\alpha}-bisabolol$ (10.2%), and ${\alpha}-copaene$ (7.7%) in T. nucifera. Among the three coniferous trees tested, the essential oils of A. koreana exhibited higher and broader antimicrobial activity against the tested organisms than those of C. japonica and T. nucifera.

Comparison of the Cold-Pressed Peel Oil Composition between ]Korean and Japanese Satsuma Mandarin (Citrus unshiu Marcov. forma Miyagawa-wase) by GC, GC-MS and GC-O

  • Park, Hyang-Sook;Sawamura, Masayoshi
    • Preventive Nutrition and Food Science
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    • v.7 no.1
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    • pp.5-11
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    • 2002
  • The comparison of the volatile flavor components from Korean and Japanese Satsuma mandarin (C. unshiu Marcov. forma Miyagawa-wase) peel oils, isolated by cold-pressing, was performed by gas chromatography, mass-spectrometry and gas chromatography-olfactometry (GC-O). Eighty-five volatile components were identified in each oil by GC and GC-MS. Forty-three components were detected in each oil by GC-O. The total amount of monoterpene hydrocarbons was 95.88% (Korean mandarin) and 95.29% (Japanese mandarin). Limonene, ${\gamma}$-terpinene, myrcene and $\alpha$-pinene were the main components of the cold-pressed oils from the both samples. The volatile composition of the Japanese mandarin was characterized by a higher content of sesquiterpene hydrocarbons, especially bicyclogermacrene, $\alpha$-humullene and valencene. The volatile composition of two samples can easily be distinguished by the percentages of aldehydes, ketones and esters, which were found at higher levels in the Japanese mandarin. The sweet and fruity flavor was stronger in the Korean mandarin oil while herbaceous flavor was stronger in Japanese sample. From GC-O data it is suggested that the sweet and fruity flavor of the Korean mandarin resulted from terpinolene and linalool, and the herbaceous note of the Japanese mandarin from $\alpha$-humullene, nepal, ι-carvone and perill aldehyde.

Frangrance and Chemical Composition of Essential Oil in Cone of Metasequoia (Metasequoia glyptostroboides Hu et Cheng) (메타세콰이아 (Metasequoia glyptostroboides)구과(毬果) 정유의 향취 및 휘발성 화학성분)

  • Yeon, Bo-Ram;Cho, Hae-Me;Jeong, Mi-Soon;Kim, Song-Mun
    • Korean Journal of Weed Science
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    • v.31 no.2
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    • pp.146-151
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    • 2011
  • Essential oil was extracted from cones of metasequoia (Metasequoia glyptostroboides) by steam distillation, fragrance was determined by sensorial analysis and chemical compositions were analyzed by gas chromatography-mass spectrometry with solid-phase microextraction apparatus. Metasequia contained 0.40% of essential oil in the cone. Major impact fragrances of the essential oil were woody, coniferous and herbal, and minor impact fragrances were minty, spicy and oily. There were nine constituents in the essential oil : 8 hydrocarbons and 1 oxide. Constituents were limonene (66.18%), ${\delta}$-3-carene (11.11%), ${\beta}$-caryophyllene (6.66%), ${\beta}$-myrcene (5.92%), ${\beta}$-pinene (4.14%), caryophyllene oxide (2.39%), camphene (2.32%), ${\alpha}$-caryophyllene (0.85%), and tricyclene (0.43%). Herbal and minty frangrances could be due to limonene and ${\delta}$-3-carene, spicy frangrance to caryophyllene, woody and coniferous frangrances to ${\alpha}$-pinene and ${\beta}$-pinene, and oily fragrance to camphene.

Determination of La in $U_3Si/Al$ Spent Nuclear Fuel by Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry (Ion Chromatography-Inductively Coupled Plasma-Mass Spectrometry에 의한 $U_3Si/Al$ 사용후핵연료 중 La의 분리 및 정량)

  • Han, Sun Ho;Choi, Kwang Soon;Kim, Jung Suk;Jeon, Young Shin;Park, Yang Soon;Jee, Kwang Yong;Kim, Won Ho
    • Analytical Science and Technology
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    • v.13 no.5
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    • pp.601-607
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    • 2000
  • Lanthanum has been used as one of the burnup monitor in spent nuclear fuel. $U_3Si/Al$ spent nuclear fuel contains small amount of La in high concentration of U and Al. Therefore, chemical separation of La is required to remove matrix elements. At first, ion chromatography (IC) and inductively coupled plasma systems were installed in radiation shielded glove box to handle the radioactive samples. Retention behavior of uranium, aluminum, lanthanum and some interesting fission products (Sr, Zr, Y, Mo, Ru, Pd, Rh, Cs, Ba, Ce, Pr, Nd, Sm, Eu and Cd) was investigated using the CG10 column and ${\alpha}$-HiBA eluent. As all elements were eluted earlier than lanthanum in 0.2 M ${\alpha}$-HiBA eluent, a portion of U and Al was directly passed to waste using a three way valve between the column and the nebulizer. Thus it was possible to determine the lanthanum in a high concentration of U and Al matrix. Retention time of La was about 12 minutes in this separation condition. Optimum range for the determination of La in $U_3Si/Al$ spent nuclear fuel was $1-10{\mu}g/L$ (ppb) with this system and detection limit was $0.25{\mu}g/L$ in case of $200{\mu}L$ of sample volume.

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Seasonal Variation in Concentration and Composition of Monoterpenes from Artemisia princeps var. orientalis (쑥에 함유된 monoterpenes 의 함량과 조성의 계절적 변이)

  • Kim, Jong-Hee
    • The Korean Journal of Ecology
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    • v.19 no.4
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    • pp.321-328
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    • 1996
  • The profile and concentration of monoterpene metabolites in the leaf and stem of Artemisia princeps var. orientalis were quantified, and seasonal variation in monoterpenes of Artemisia plant was investigated. Samples were taken from five sites at the campus of Kyungnam University during maturing season. Monoterpenes in leaf and stem were analyzed using gas chromatography-mass spectrometry (GC-MS). The major constituents of A. princeps var. orientalis in both the leaf and stem were 21 monoterpenes.$ {\alpha}-pinene,\;{\beta}-pinene,\;{\beta}-myrcene$, dl-limonene, naphthalene and unknown monoterpenes with 5.49 and 16.27 of retenstion time were present in high concentrations of compounds identified on the leaf and stem of A. princeps var. orientalis. The cmounts of total monoterpenes of leaf were from two to five times higher than stem and rapidly decreased with the time, while that of stem was constnat except early spring. Most of the high percentage of monoterpenes in the leaf were those with later retention time. These results indicated that monoterpenes yields are considered to be more variable than monoterpene composition in responding to the time in both the leaf and stem.

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