• Title/Summary/Keyword: ether extraction

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Bioavailability Test of TestoTM Tablets (Methyltestosterone, 25 mg) in Male Healthy Volunteers by a Gas-chromatography/Mass Selective Detector

  • Kwon, Oh-Seung;Kim, Hye-Jung;Pyo, Hee-Soo;Kim, Dae-Duk;Chung, Youn-Bok
    • Journal of Pharmaceutical Investigation
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    • v.35 no.5
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    • pp.383-388
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    • 2005
  • A simple and specific method for determination of methyltestosterone (MT) has been established by a gas chromatography/mass selective detector and applied in plasma of healthy male volunteers received a single oral dose of 50 mg MT $(Testo^{TM}\;tablets,\;25\;mg)$ for bioavailability test. This method involves using liquid-liquid extraction of the sample with diethyl ether and derivatization with MSTFA. MT showed good resolution in this condition. The detection limit of quantitation was 5 ng/ml. A good linearity (r>0.996) was obtained at the range of 5-250 ng/ml of MT. Intra-day precision and accuracy were 2.76-12.56% and 0.39-8.01 %, and inter-day precision and accuracy were 2.29-17.69% and 0.42-7.99%, respectively. The established method was applied on bioavailability test of MT in human volunteers. The value of $AUC_{0\;to\;last}$ to last was $264.5{\pm}123.9\;ng{\cdot}hr/ml$ and that of $AUC_{0\;to\;inf}$ was determined to be $275.2{\pm}126.5\;ng{\cdot}hr/ml$. The values of $C_{max}$ and $T_{max}$ were $95.9{\pm}67.1\;ng/ml$ and $1.13{\pm}0.9\;hr$, respectively. The mean elimination half-life $(t_{1/2})$ was $4.4{\pm}0.9\;hr$. This analytical method is suitable and useful for the pharmacokinetics and bioequivalence studies of MT.

Separation of Radiostrontium from Environmental Sample Using Strontim Selective Chromatographic Resin$(Sr.\;Spec^{TM})$ (스트론튬 선택적이온교환수지$(Sr.\;Spec^{TM})$를 이용한 환경시료중의 방사성 스트론튬의 분리)

  • Hong, Kwang-Hee;Lee, Chang-Woo;Choi, Yong-Ho;Lee, Myung-Ho
    • Journal of Radiation Protection and Research
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    • v.20 no.1
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    • pp.1-7
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    • 1995
  • Strontium selective chromatographic material $(Sr-Spec^{TM})$ was investigated for separation of radiostrontium from environmental soil and water sample. This chromatographic material has great capacity of binding of strontium ion in nitric acid media, and has selectivity to permit the separation of stontium from bulk amount of calcium. But the extraction of strontium was reduced by the other interfering ions such as K and Ba. So, in order to apply this material to the soil sample, prior removal treatment of K and Ba was needed. But the Sr-Spec material could provides simple and effective methods for the separation and removal of radiostrontium from liquid sample.

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Volatile Flavor Components in Various Edible Portions of Capsella bursa-pastoris (냉이의 식용부위별 휘발성 향기성분)

  • Lee, Mie-Soon;Choi, Hyang-Sook
    • Korean Journal of Food Science and Technology
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    • v.28 no.5
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    • pp.822-826
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    • 1996
  • Volatile flavor components from various edible portions of Capsella bursa-pastoris were collected by simultaneous steam distillation-extraction (SDE) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Thirty four volatile flavor components, including 12 hydrocarbons, 2 aldehydes, 2 ketones, 5 alcohols, 1 ester, 10 acids and 2 miscellaneous ones were confirmed in whole samples. Thirty one components, including 11 hydrocarbons, 5 aldehydes, 4 ketones, 5 alcohols, 1 esters and 5 miscellaneous ones were confirmed in leaves. Twenty four components, including 5 hydrocarbons, 1 aldehyde, 2 ketones, 6 alcohols, 2 esters, 1 acid and 7 miscellaneous ones were confirmed in roots. The kinds and amounts of volatile flavor components revealed different patterns depending upon various edible portions. Relatively greater numbers of volatile flavor components were identified in leaves compared with roots of these wild plants. The characteristic aroma of Capsella bursa-pastoris appeared to be due to combination of C6 alcohol and acids, terpene alcohol and sulfur containing compounds.

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Volatile Flavor Components of Capsella bursa-pastoris as Influenced by Drying Methods (건조방법에 따른 냉이의 휘발성 향기성분)

  • Lee, Mie-Soon;Choi, Hyang-Sook
    • Korean Journal of Food Science and Technology
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    • v.28 no.5
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    • pp.814-821
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    • 1996
  • An attempt was made to determine the effects of drying methods including shady air drying, presteamed and shady air drying, microwave drying, and freeze drying on the volatile flavor components of Capsella bursapastoris. Essential oils from the samples were isolated by Simultaneous steam distillation-extraction (SDE) method using diethyl ether as solvent. Concentrated samples were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Respective 30, 18, 29, and 26 volatile flavor components were identified in shady air dried samples, presteamed and shady air dried samples, microwave dried samples, and freeze dried samples. The kinds and amounts of volatile flavor components evidently depended upon the drying methods. Trimethyl sulfide was regarded as the most abundant component in shady air dried samples, dimethyl trisulfide in presteamed and shady air dried samples, and phytol in microwave or freeze dried samples.

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Analysis of Volatile Flavor Components of Pleurospermum kamtschaticum (누룩치의 휘발성 향미성분 분석)

  • 정미숙;이미순
    • Korean journal of food and cookery science
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    • v.14 no.5
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    • pp.541-546
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    • 1998
  • Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.

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Analysis of Volatile Flavor Components of Aster glehni (섬쑥부쟁이의 휘발성 향미성분 분석)

  • 이미순;정미숙
    • Korean journal of food and cookery science
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    • v.14 no.5
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    • pp.547-552
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    • 1998
  • Essential oils in leaf of fresh Aster glehni were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. The yield of the essential oils was 0.05%. And their volatile flavor components were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) and identified by the RI of GC and mass spectrum of GC-MS. A total of 31 components, including 17 hydrocarbons, 2 aldehydes, 7 alcohols, 3 esters, 1 acid and 1 oxide were identified. The major volatile flavor components of fresh Aster glehni were ${\alpha}$-pinene, limonene, $\delta$-elemene, ${\beta}$-pinene, cis-3-hexenol and myrcene. Volatile flavor patterns of fresh ind dried Aster glehni were analyzed using an electronic nose. Sensor PA2 that was sensitive to alcohols showed the highest resistance for fresh and dried Aster glehni. Resistance of six metal oxide sensors was decreased in fresh sample compared with dried one.

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Production Condition, Purification and Properties of Anticaries Microbial Agent by Bacilluse alkalo-philshaggy JY-827 (Bacillus alkalophilshaggy JY-827가 생산하는 항우식균물질의 생산조건과 분리, 정제 및 특성)

  • 전주연;류일환;이상욱;이갑상
    • Microbiology and Biotechnology Letters
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    • v.28 no.5
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    • pp.270-278
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    • 2000
  • The study was performed to investgate the excellent microbial anticaries substance which is more effective that the chlorhexidine in the dental caries treatment. A typi-cal strain which produced the most excellent antimicrobial subatance was selected. and identified novel alkalophillic Bacillus alkalophilshaggy JY-827. For the maximal production of themicrobial antibiotic against Streptococcus mutans from B. alkalophilshaggy JY-827, the optimal culture condition was in the medium containing glucose 15g/ L, pepton 10g/L and $K_2$$HPO_4$ 2g/L the highest production of antibiotic against S.mutans was obtained at $25^{\circ}C$ and pH 11.0 for 5 days. The antibiotic from B. alkalophilshaggy JY-827 was purified by organic solvent extraction, silica gel and sephadex LH-20 column chromatograpies, and then crystallized with methanol. The crystallin compoma-tion of this antibiotic was as a curcular shape. The melting point and rm[$\alpha$]$D^{20}$ were 152-154$^{\circ}C$ and +55。, respec-tively. Based on Instumental analyses such as FT-IR, $^{1}$H-NMR $^{13}$ C-NMR and GC-mass, the antibiotic was identified as aminoglycoside. It was obtained as amorphous white power, and soluble in water power, and soluble in water, methanol but insoluble in ether, chroloform. This antibiotic inhibited the growth of S.mutans to about 3 day at the concentration of $2.5$\times$10^{-7}$ /M. It was stable at the alkalli condition but unstable within the acid condition. It was also stable up to $70^{\circ}C$.

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Analytical Method of Polybrominated Biphenyl Ethers(PBDEs) in Environmental Samples (환경시료 중 폴리브롬화비페닐에테르(Polybrominated Biphenyl Ethers) 분석법)

  • Kim, T.S.;Hwang, S.Y.;Shin, S.K.
    • Analytical Science and Technology
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    • v.15 no.4
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    • pp.346-359
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    • 2002
  • The brominated flame retardants (BFRs) are one of the unregulated pollutants in Korea, which is recently highlighted the new pollutants of environmental contamination. In this study, the previous research papers related the BFRs were surveyed, and the analytical methods of BFRs were established. The results are followed; The 40 kinds of PBDEs standards were used to establish the analytical methods to perform the experiments of recoveries and detection limits in water and soil. The detection limits of PBDEs using GC/MS represented 5.0~10.0 pg/L for water and 0.5~2.0 ng/g for soil samples. The average recoveries of water samples were 89~98% with ethylacetate, n-hexane and dichloromethane, and 89~103% in combined solvent with n-hexane and acetone. In soxhlet extraction, the higher recoveries obtained the acetone:n-hexane(1:1) comparing with acetone:dichloromethane(1:1).

Study on Isolative Determination Methylephedrine Hydrochloride and Ephedrine Hydrochloride in the Mixed Preparation (혼합제제중 Methylephedrine Hydrochloride와 Ephedrine Hydrochloride의 분리정량에 관한 연구)

  • Ko, In-Suk
    • Korean Journal of Pharmacognosy
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    • v.1 no.3
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    • pp.93-99
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    • 1970
  • There have been reported by several workers for the isolation and determination of the amine derivatives as Metbylephedrine Hydrochloride and Ephedrine Hydrochloride adopting neutralization method, steam distillation method, non-aqous titration method, ion-exchange resin method, titration method after acetylation, colorimetric method, gravimetric method, iodine titration method and gas chromatography. Those methods mentioned in above, can be practically applied for the sample which is not mixed one mith the other amine compounds. Presently, it has not shown on the isolative determination of the mixed sample of amine derivatives. In this paper, it is discussed on the isolative determination of Methylephedrine Hydrochloride as the tertiary amine compound and Ephedrine Hydrochloride as the secondary amine compound. According to the results of the experiment, it could be summarized as follows: 1. There is no time-variation on the color reaction of Methylephedrine Hydrochloride and Ephedrine Hydrochloride with the color reagent, bromcresolgreen. And Methylephedrine Hydrochloride and Ephedrine Hydrochloride, respectively, can be determined spectrophotometrically by means oft his color reaction. 2. For the isolation of Methylephedrine Hydrochloride and Ephedrine Hydrochloride from the mixed sample, Methylephedrine Hydrochloride can be eluted by chloroform, while Ephedrine Hydrochloride by the mixed solvent of chloroform and ethylalcohol (2:1), from the celite column adsorbed at pH6.4 followed by extraction with ether undersodium hydroxide alkali re action. 3. When the sample is mixed with quinine hydrochloride, dihydrocodeine bitartate, and noscapine, these mixed compounds can be eliminated by means of stram distillation. 4. When the sample is mixed with chlorpheniramine maleate, dextromethorphan hydrobromide and diphenhydramine hydrochloride, the mixed compounds can be eliminated by means of steam distillation and celite adsorption column chromatography, In conclusion, the isolative determination method for Methylephedrine Hydrochloride and Ephedrine Hydrochloride studied in this paper, indicates with the excellent reproducibility and accuracy.

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The Study of the Anti-oxidative Effects of Polygonati Multiflori Caulis on Oxidized Brain and Liver Cells in Rats (야교등(夜交藤)이 흰쥐 뇌와 간에서의 산화 억제에 미치는 영향)

  • Lee, Han-Goo;Han, Hyo-Sang;Lee, Young-Jong
    • The Korea Journal of Herbology
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    • v.25 no.1
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    • pp.13-21
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    • 2010
  • Objectives : This study was purposed to the anti-oxidative effects of Polygonati Multiflori Caulis(henceforth PMC) on oxidized brain and liver cells in rats. Methods : After extraction of PMC with water, the water extract was divided into five fractions : hexane, ethyl ether, ethyl acetate, butanol and an aqueous fraction. The phenol contents of each fraction were measured. The lipid peroxidation inhibition effect were then investigated. Results : After processing PCM water and PCM fractionations on oxidized brain cells in rats, the SOD (super oxide dismutase) activity and glutathione content were increased, and the NO (nitric oxide) content was decreased. It had much higher SOD activity than liver cells in rats excluded in the n-BuOH and aqueous fractions. In case of oxidized liver cells in rats, the SOD activity and glutathione content increased, while both the NO content and the MDA (malondialdehyde) content decreased. It had much higher glutathione content than brain cells in rats in the every fractions. It had much lower MDA content than brain cells in rats in the Aqueous fractions and brain cells in rats had much lower MDA content than liver cells in rats in the total extract, n-hexane, EtOEt, EtOAc and n-BuOH fractions. Conclusions : PMC has anti-oxidative effect on oxidized liver cells and brain cells in rats, through there are differences in fraction. Additionally, Anti-oxidative effect of brain cells can be relaxed the mental nerve and it is related PMC effect.