• Title/Summary/Keyword: Alpha spectrometry

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Evaluation of Testosterone Metabolites/Dehydroepiandrosterone As the Indicators of Testosterone Administration in Horse Doping (경주마 약물검사에서 testosterone 투여 여부표지자로서의 testosterone 대사체들에 대한 dehydroepiandrosterone의 비율 평가)

  • Kim, Jin Young;Choi, Man Ho;Kim, Sung Jean;Kyong, Jin Burm;Chung, Bong Chul
    • Analytical Science and Technology
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    • v.12 no.3
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    • pp.190-195
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    • 1999
  • The metabolism of testosterone ($17{\beta}$-hydroxy-androst-4-en-3-one) was confirmed in horse after a single intramuscular administration of testosterone cypionate (750 mg). Solvent extracts of urine obtained with enzymatic hydrolysis and methanolysis were analyzed by GC/MS after oxime t-butyldimethylsilyl (oxime-TBDMS) derivatization. The structures of four urinary metabolite after testosterone administration in horse were determined based on EI mass spectra and $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol and $5{\alpha}$-androstane-$3{\beta}$-ol-17-one as major was confirmed with authentic standard. Also the concentrations of $5{\alpha}$-androstane-$3{\beta}$, $17{\alpha}$-diol, $5{\alpha}$-androstane-$3{\beta}$, $17{\beta}$-diol, dehydroepiandrosterone (DHEA), $5{\alpha}$-androstane-$3{\beta}$-ol-17-one and testosterone were determined in the urine of normal subjects and the urine after administration. The recovery and detection limit in the most drugs were 86.3~94.7% and 1~3 ppb, respectively. Correlation coefficients for calibration were in the range of 0.984~0.999. Excretion profile of testosterone presents the rapid and large increasement up to maximum values at days 5 after administration and the slow regression. The relative ratios of testosterone, its metabolites over DHEA were determined for indication of testosterone administration in horse doping.

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Simultaneous Determination of Titanium, Zirconium and Niobium by Reactor Neutron Activation (원자로 중성자에 의한 티탄, 지르코늄 및 니오브의 동시 정량)

  • Chul Lee;Yung Chang Yim;Koo Soon Chung
    • Journal of the Korean Chemical Society
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    • v.18 no.1
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    • pp.40-46
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    • 1974
  • The fission neutron reactions of $^{47}Ti(n.p)^{47}Sc$ and $^{93}Nb(n,{\alpha})^{90m}Y$, along with epicadmium neutron reaction of $^{96}Zr(n,{\gamma})^{97}Zr$ were used for the simultaneous determination of Ti, Nb and Zr in synthetic mixture. Prior to neutron irradiation, Ti, Zr and Nb in the mixture were separated together in one group through the cation exchange column of Dowex $50{\times}8$ resin using 0.5 M ${\alpha}$-hydroxy-iso-butyric acid as the eluent. After irradiation of the eluate the product nuclides, $^{97}Zr$, ^{47}Sc$ and ^{90m}Y$, were eluted sequentially through the same column with 0.5 M ${\alpha}$-HIBA, 0.5 M ${\alpha}$-HIBA-1 N HNO_3 and 0.5 M ${\alpha}$-HIBA-2 N HNO_3$ solution, respectively. The gamma-ray spectrometry was used for the measurement of the gamma-ray activities of the eluted nuclides. The detection limits of Nb, Ti and Zr were found to be 0.2 %, 0.01 % and 0.002 %, respectively.

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Determination of the volatile flavor components of orange and grapefruit by simultaneous distillation-extraction (연속수증기증류추출법에 의한 오렌지와 자몽의 휘발성 유기화합물 확인)

  • Hong, Young Shin;Kim, Kyong Su
    • Food Science and Preservation
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    • v.23 no.1
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    • pp.63-73
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    • 2016
  • The volatile flavor components of the fruit pulp and peel of orange (Citrus sinensis) and grapefruit (Citrus paradisi) were extracted by simultaneous distillation-extraction (SDE) using a solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by gas chromatography-mass spectrometry (GC-MS). The total volatile flavor contents in the pulp and peel of orange were 120.55 and 4,510.81 mg/kg, respectively, while those in the pulp and peel of grapefruit were 195.60 and 4,223.68 mg/kg, respectively. The monoterpene limonene was identified as the major voltile flavor compound in both orange and grapefruit, exhibiting contents of 65.32 and 3,008.10 mg/kg in the pulp and peel of orange, respectively, and 105.00 and 1,870.24 mg/kg in the pulp and peel of grapefruit, respectively. Limonene, sabinene, ${\alpha}$-pinene, ${\beta}$-myrcene, linalool, (Z)-limonene oxide, and (E)-limonene oxide were the main volatile flavor components of both orange and grapefruit. The distinctive component of orange was valencene, while grapefruit contained (E)-caryophyllene and nootkatone. $\delta$-3-Carene, ${\alpha}$-terpinolene, borneol, citronellyl acetate, piperitone, and ${\beta}$-copaene were detected in orange but not in grapefruit. Conversely, grapefruit contained ${\beta}$-pinene, ${\alpha}$-terpinyl acetate, bicyclogermacrene, nootkatol, ${\beta}$-cubebene, and sesquisabinene, while orange did not. Phenylacetaldehyde, camphor, limona ketone and (Z)-caryophyllene were identified in the pulp of both fruits, while ${\alpha}$-thujene, citronellal, citronellol, ${\alpha}$-sinensal, ${\gamma}$-muurolene and germacrene D were detected in the peel of both fresh fruit samples.

Isolation and Identification of Triterpenoids from the Mulberry (Morus alba) Root Bark (상백피(Morus alba root bark)로부터 triterpenoid의 분리 및 동정)

  • Jung, Jae-Woo;Park, Ji-Hae;Jung, Ye-Jin;Lee, Chang-Ho;Han, Daeseok;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.57 no.4
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    • pp.295-299
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    • 2014
  • The mulberry (Morus alba L.) root barks were extracted with 80% aqueous methanol at room temperature. The concentrated extract was partitioned as ethyl acetate (EtOAc), n-BuOH, and $H_2O$ fractions. From the EtOAc fraction, five triterpenoids were isolated through the repeated silica gel and octadecyl $SiO_2$ column chromatographies. According to the results of physico-chemical and spectroscopic data including nuclear magnetic resonance, mass spectrometry, and infrared, the chemical structures of the triterpenoids were respectively determined as ${\alpha}$-amyrin (1), ${\alpha}$-acetyl amyrin (2), lupeol (3), betulinic acid (4), and glutinol (5). Compounds 1, 3, and 5 were isolated for the first time from the mulberry root bark.

Essential Oil Analysis of Illicium anistum L. Extracts

  • Min, Hee-Jeong;Kim, Chan-Soo;Hyun, Hwa-Ja;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • v.45 no.6
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    • pp.682-688
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    • 2017
  • Fresh japanese anise (Illicium anisatum L.) tree leaves were collected and ground after drying. The essential oils of the leaves were analyzed by gas chromatography-mass spectrometry (GC-MS) using headspace (HS) and solid phase-microextra (SPME) methods. Volatile components of the leaves were identified 21 and 65 components in HS and SPME, respectively. The main components of the essential oils obtained by HS method were eucalyptol (36.7%), (+)-sabinene (15.61%), ${\delta}$-3-carene (6.87%), ${\alpha}$-pinene (6.07%), ${\gamma}$-terpinen (5.72%), ${\alpha}$-limonene (5.26%), ${\beta}$-myrcene (4.13%), ${\alpha}$-terpinene (4.04%) and ${\beta}$-pinene (3.73%). The other components were less than 3.5%. SPME method also showed that eucalyptol (17.88%) was main. The other were 5-allyl-1-methoxy-2 (13.29%), caryophyllene (6.09%), (+)-sabinene (5.60%), ${\alpha}$-ocimene (4.89%) and ${\beta}$-myrcene (3.73%), and the rest were less amounts than 3.5%. This work indicated that many more volatile components were isolated, comparing to the previous literature data and that SPME method was much more effective than HS method in the analysis of the volatile components.

Analyses of the Volatile Flavor Composition of Essential Oils from Chrysanthemum zawadskii var. latilobum Kitamura and Aster yomena Makino (구절초와 쑥부쟁이 정유의 휘발성 향기성분 분석)

  • Choi, Hyang-Sook
    • The Korean Journal of Food And Nutrition
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    • v.31 no.3
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    • pp.378-387
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    • 2018
  • This study investigated the volatile flavor composition of essential oils from Chrysanthemum zawadskii var. latilobum Kitamura and Aster yomena Makino. The essential oils obtained by the hydrodistillation extraction method from the aerial parts of the plants were analyzed by gas chromatography (GC) and GC-mass spectrometry (GC-MS). One hundred (95.04%) volatile flavor compounds were identified in the essential oil from the C. zawadskii var. latilobum Kitamura. The major compounds were valencene (10.82%), ${\delta}$-cadinol (9.77%), hexadecanoic acid (8.70%), 2-methyl-4-(2,6,6-trimethylcyclohex-1-enyl) but-2-en-1-ol (3.67%), and 2-(2,4-hexadiynylidene)-1,6-dioxaspiro[4,4]non-3-ene (3.57%). Ninety-eight (93.83%) volatile flavor compounds were identified in the essential oil from the Aster yomena Makino. The major compounds were and 3-eicosyne (13.61%), 9,10,12-octadecatrienoic acid (7.8%), ${\alpha}$-caryophyllene alcohol (6.83%), 9-octadecynoic acid (6.03%), and ${\alpha}$-caryophyllene (5.74%). Although the two plants are apparently very similar, the chemical composition of the essential oils was significantly different in quality and quantity. In the case of C. zawadskii var. latilobum Kitamura, the sesquiterpene, valencene was found to be 10.82%, but it was not identified in A. yomena Makino. ${\delta}$-Cadinol appeared higher in C. zawadskii var. latilobum Kitamura than in A. yomena Makino. A clear characteristic of A. yomena Makino essential oil is that it has a high content of caryophyllene derivatives. The ${\alpha}$-caryophyllene alcohol contained in A. yomena Makino was relatively high at 6.83%, although the compound was not identified in C. zawadskii var. latilobum Kitamura. Also ${\alpha}$-caryophyllene was shown to be higher in A. yomena Makino than in C. zawadskii var. latilobum Kitamura.

Linear Free Energy Relationship on the Chemical Shift of Imidoyl Proton in N-benzylideneaniline Derivatives by PMR Spectrometry (核磁氣 共鳴分光法에 義한 N-Benzylideneaniline 誘導體중 Imidoyl Proton 의 Chemical Shift 에 미치는 自由에너지 關係)

  • Nack Do Sung;Cheon Kyu Park;Moon kyu Park;Ki Sung Kwon;Kim, Tae Rin
    • Journal of the Korean Chemical Society
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    • v.29 no.3
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    • pp.277-282
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    • 1985
  • The effects of linear free energy relationship (LFER) on the imidoyl proton (H${\alpha}$)-substituent chemical shift (SCS) in case of varying para-substituted C-phenyl group in N-benzylideneaniline derivatives were studied. The H${\alpha}$-SCS values and LFER parameters such as ${\sigma}$,${\sigma}^+$, ${\sigma}_I$,${\sigma}_R, F and R were applied to the Hammett, Okamoto-Brown, and Taft, Swain-Lupton's dual substituents parameter (DSP) equations. The results were: (1) the blending coefficient values, ${\lambda}$ = 2.8∼3.2, it's means that the resonance effect (R) was larger than inductive effect (I) and field effect (F), and (2) the values of percent resonance and percent field effects were %R = 66.6 and %F = 33.4, respectively, yielding the ratio of resonance effect (R) to field effect (F) of 2 : 1.

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Determination of hormonal active compounds in meat (육류 식품중 호르몬 성분의 분석)

  • Seo, Jungju
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.526-534
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    • 2008
  • To determine the trace level of synthetic and natural hormones in food, the improvement of official analytical method and new development of simultaneous determination of hormones were established. On the basis of developed analytical method, the background level of natural hormones and distribution of residual hormones were monitored in meat. Target hormones were six natural hormones such as estrogens ($17{\beta}$-estradiol, $17{\alpha}$-estradiol, estrone), androgens ($17{\beta}$-testosterone, $17{\alpha}$-testosterone), and gestagens (progesterone) and three synthetic hormones such as DES, zeranol, and taleranol. These hormones were analyzed by gas chromatographymass spectrometry. Newly developed multi-residue analysis method was applied for meat sample which were collected from market in the capital region and monitored the presence of residues of synthetic and natural steroid hormones. No residue of synthetic hormones were detected and endogenous level of progesterone was detected in cattle, pig and liver samples tested.

Casein Kinase 2 interacts with human mitogen- and stress-activated protein kinase MSK1 and phosphorylates it at Multiple sites

  • Shi, Yan;Han, Guanghui;Wu, Huiling;Ye, Kan;Tian, Zhipeng;Wang, Jiaqi;Shi, Huili;Ye, Mingliang;Zou, Hanfa;Huo, Keke
    • BMB Reports
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    • v.42 no.12
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    • pp.840-845
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    • 2009
  • Mitogen- and stress-activated protein kinase (MSK1) palys a crucial role in the regulation of transcription downstream of extracellular-signal-regulated kinase1/2 (ERK1/2) and mitogen-activated protein kinase p38. MSK1 can be phosphorylated and activated in cells by both ERK1/2 and p38$\alpha$. In this study, Casein Kinase 2 (CK2) was identified as a binding and regulatory partner for MSK1. Using the yeast two-hybrid system, MSK1 was found to interact with the CK2$\beta$ regulatory subunit of CK2. Interactions between MSK1 and the CK2$\alpha$ catalytic subunit and CK2$\beta$ subunit were demonstrated in vitro and in vivo. We further found that CK2$\alpha$ can only interact with the C-terminal kinase domain of MSK1. Using site-directed mutagenesis assay and mass spectrometry, we identified five sites in the MSK1 C-terminus that could be phosphorylated by CK2 in vitro: Ser757, Ser758, Ser759, Ser760 and Thr793. Of these, Ser757, Ser759, Ser760 and Thr793 were previously unknown.

Determination of Heterocyclic Amines and Acrylamide in Agricultural Products with Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Kyung-Jun;Lee, Gae-Ho;Kim, HaeSol;Oh, Min-Seok;Chu, Seok;Hwang, In Ju;Lee, Jee-yeon;Choi, Ari;Kim, Cho-il;Park, Hyun-Mee
    • Toxicological Research
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    • v.31 no.3
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    • pp.255-264
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    • 2015
  • Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, $A{\alpha}C$, $MeA{\alpha}C$, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including $IQ-d_3$, $MeIQx-d_3$, $PhIP-d_3$, $Trp-P-2-^{13}C_2-^{15}N$ and $MeA{\alpha}C-d_3$ was spiked for quantification of HCAs and $^{13}C_3$-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.