• 제목/요약/키워드: acetonitrile-water mixtures

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Quantitative Analysis of Marker Substances in Solid Fermented Angelicae Gigantis Radix by HPLC (HPLC를 이용한 고체발효 당귀의 지표성분 분석)

  • Um, Young-Ran;Lee, Ji-Hye;Ma, Jin-Yeul
    • Korean Journal of Oriental Medicine
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    • v.16 no.1
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    • pp.173-178
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    • 2010
  • The purpose of this study was investigation of quantitative analysis of marker substances in solid fermented Angelicae Gigantis Radix by High performance liquid chromatography(HPLC). HPLC was performed for determination of nodakenin and decursin in solid fermented Angelicae Gigantis Radix extract, the separation method was performed on C18 column ($250\;mm\;{\times}\;4.6\;mm$, $5\;{\mu}m$, RS tech) using gradient solvent mixtures of water-acetonitrile with photodiode array detector (330 nm). The flow rate was 1.0 ml/min. Retention time of nodakenin and decursin was about 11.47, 46.79 min and linearity of calibration was showed good result(r2=0.9999, 0.9999), respectively. Content of nodakenin was $0.76\;{\pm}\;0.02%$ in control, $0.31\;{\pm}\;0.00%$ in Angelicae Gigantis Radix extract fermented with Paecilomyces japonica(SDT)(p<0.01), $0.51\;{\pm}\;0.02%$ in Angelicae Gigantis Radix extract fermented with Ganoderma lucidum(SYT)(p<0.01), $0.82\;{\pm}\;0.03%$ in Angelicae Gigantis Radix extract fermented with honey(SST)(p<0.05) and $0.88\;{\pm}\;0.01%$ in Angelicae Gigantis Radix extract fermented with Nuruk(SNT)(p<0.01). Content of decursin was $4.50\;{\pm}\;0.08%$ in control, $2.90\;{\pm}\;0.05%$ in Angelicae Gigantis Radix extract fermented with Paecilomyces japonica(SDT)(p<0.01), $2.65\;{\pm}\;0.08%$ in Angelicae Gigantis Radix extract fermented with Ganoderma lucidum(SYT)(p<0.01), $4.46\;{\pm}\;0.11%$ in Angelicae Gigantis Radix extract fermented with honey(SST) and $4.73\;{\pm}\;0.04%$ in Angelicae Gigantis Radix extract fermented with Nuruk(SNT)(p<0.05), respectively.

Oxygen Ring Formation Reaction of Mono-Oxo-Bridged Binuclear Molybdenum(V) Complex (II). Reaction of $[Mo_2O_3(Phen)_2(NCS)_4]$ with Solvent Water in Water + Co-Solvent Mixtures (한개의 산소다리를 가진 몰리브덴(V) 착물의 산소고리화 반응 (II). 2성분 혼합용매에서 용매물과 $[Mo_2O_3(Phen)_2(NCS)_4]$의 반응)

  • Sang-Oh Oh;Huee-Young Seok
    • Journal of the Korean Chemical Society
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    • v.32 no.3
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    • pp.203-210
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    • 1988
  • Mono-oxo-bridged binuclear molybdenum(V) complex, $[Mo_2O_3(Phen)_2(NCS)_4]$ produces di-oxo-bridged binuclear molybdenum(V) complex, $[Mo_2O_4(Phen)_2(NCS)_2]$ in water + co-solvent, where the co-solvent are acetone, acetonitrile and N,N-dimethylformamide. The rate of conversion of $[Mo_2O_3(Phen)_2(NCS)_4]\;into\;[Mo_2O_4(Phen)_2(NCS)_2]$ has been measured by spectrophotometric method. Temperature was $10^{\circ}C$ to $40^{\circ}C$ and pressure was varied up to 1500 bar. The rate constants are increased with increasing water mole fraction and decreased with increasing concentration of hydrogen ion. The order of oxygen ring formation reaction rate in various cosolvent is as follows, ACT > AN > DMF which is agreed with solvent dielectric constants. The observed negative activation entropy ($[\Delta}S^{\neq}$), activation volume($[\Delta}V^{\neq}$) and activation compressibility coefficient(${\Delta}{\beta}^{\neq}$) values show that the solvent water molecule is strongly attracted to the complex at transition state. From these results, the oxygen ring formation reaction of $[Mo_2O_3(Phen)_2(NCS)_4]$ is believed association mechanism.

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Study of the Separation and Elution Behavior of Phenols as Priority Pollutants in Reversed Phase Liquid Chromatography (역상 액체 크로마토그래피에서 유기오염물질로서의 페놀류들의 분리 및 용리거동에 관한 연구)

  • Dai Woon Lee;Sun Kyung Lee;Keun Sung Yook;Won Lee
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.287-294
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    • 1989
  • The optimum condition for the separation of priority pollutant phenols using isocratic elution has been determined. The elution behavior of eleven phenols has been also studied to interpret the retention. The reversed phase liquid chromatographic methods were performed on a ${\mu}$-Bondapak $C_{18}$ column with methanol-water, acetonitrile-water, and THF water mixtures as mobile phases. The COF method, where Snyder's solvent triangle concept was combined with a mixture-design statistical technique, was used to optimize the strength and selectivity of solvents for the separation of phenols. The optimum solvent composition, which gives a complete separation of eleven phenols, was found to be $MeOH:ACN:H_2O$ = 7:40:53. The plots of ln k' vs. -${\Delta}H^{\circ}$ and ${\Sigma}{\pi}$ of phenols showed relatively good linearities. Effect of van der Waals volume, pi-energy and hydrogen bonding on the retention of phenols were investigated. The following equation with the correlation coefficient of 0.9927 for ACN-water solvent system was obtained; $log^{k'}=2.515{\times}10^{-2}VWV-1.301{\times}10^{-1}E-3.674{\times}10^{-1}$

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Effect of Interaction of BPMC, Carbaryl and Chlorothalonii on short-term Bioconcentration Factor in Carassius auratus(goldfish) (BPMC, Carbaryl 및 Chiorothalonil의 상호작용이 Carassius auratus(goldfish)를 이용한 단기간 생물농축계수의 측정에 미치는 영향)

  • 민경진;차춘근;전봉식;김근배
    • Journal of Environmental Health Sciences
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    • v.23 no.2
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    • pp.72-82
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    • 1997
  • This study was performed to investigate the effect of co-existence of BPMC, carbaryl and chlorothalonil on the short-term bioconcentration factor in Carassius auratus(goldfish). The fishes were exposed to the combined treatment of BPMC, carbaryl and chlorothalonil (0.05 ppm+0.05 ppm+0.005 ppm, 0.05 ppm+0.05 ppm+0.010 ppm, 0.05 ppm+0.10 ppm+0.005 ppm, 0.10 ppm+0.05 ppm+0.005 ppm, 0.10 ppm+0.10 ppm+0.005 ppm) for 3 and 5 days, respectively. BPMC, carbaryl and chlorothalonil in fish and in test water were extracted with n-hexane and acetonitrile. GC-ECD was used to detect and quantitate BPMC, carbaryl and chlorothalonil. 3-day and 5-day bioconcentration factors(BCF$_3$ and BCF$_5$) of each pesticide were calculated from the quantitation results. The depuration rate of each pesticide-from the whole body of fish was determined over the 72-h period after combined treatment.The results were as follows: BCF$_3$ values of BPMC were 4.163, 4.011, 4.122, 4.750 and 4.842 when the concentration of BPMC+ carbaryl+chlorothalonil in combined treatment were 0.05 ppm+0.05 ppm+0.005 ppm, 0.05 ppm+0.05 ppm+0.010 ppm, 0.05 ppm+0.10 ppm+0.005 ppm, 0.10 ppm+0.05 ppm+0.005 ppm and 0.10 ppm+ 0.10 ppm+0.005 ppm. BCF$_5$ values of BPMC were 3.465, 3.270, 3.472, 3.162, 4.227 and 4.157, respectively, under the above conditions. While BCF$_3$ values of carbaryl were 4.583, 4.642, 4.571, 3. 637 and 3.529, respectively, and BCF$_5$ values of carbaryl were 3.932, 3.797, 3.843, 4.293 and 4.132, respectively, under the conditions. While BCF$_3$ values of chlorothalonil were 2.024, 3.532, 2.213, 2.157 and 2.271, respectively, and BCF$_5$ of chlorothalonil were 6.712, 7.013, 6.457, 6.694 and 6.597, respectively, under the conditions. Depuration rate constants of BPMC were 0.019, 0.018, 0.020, 0.022 and 0.021 when the concentration of BPMC+carbaryl+chlorothalonil in combined treatment were the same as above. And depuration rate constants of carbaryl were 0.030, 0.029, 0.030, 0.029 and 0.031, respectively, under the same condition of pesticide mixtures. While depuration rate constants of chlorothalonil were 0.004, 0.004, 0.003, 0.004 and 0.003, respectively, under the same condition. It was observed that no significant differences of BCFs and concentrations of the compounds in fish extracts, test water between combined treatment and single treatment. It was considered that no appreciable interaction at experimental concentrations was due to low concentrations, near environmental level, 0.005-0.1 ppm. Coexistence of BPMC, carbaryl and chlorothalonil had no effect on depuration rate of each pesticide and depuration rate of chlorothalonil was investigated 1/8 and 1/6 slower than those of carbaryl and BPMC in combined treatment. It is similar result in comparison with single treatment. Therefore, it is considered that the persistence of chlorothalonil in fish body would be higher than those of carbaryl and BPMC.

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Retention Behavior and Separation of Phenol Derivatives through Cyclodextrin Complexes in Reversed-Phase Liquid Chromatography (역상 액체 크로마토그래피에서 씨클로덱스트린 착물을 이용한 페놀유도체들의 머무름 거동 및 분리)

  • Moon, Young-Ja;Kang, Sam-Woo
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.179-188
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    • 1998
  • The capacity factor of fifteen phenol derivatives was determined with respect to the concentration of ${\alpha}$- or ${\beta}$-cyclodextrin [CD], the type as well as the content of organic solvent in the mobile phase, and the temperature. The effect of the inclusion complex formation between solutes and ${\alpha}$- or ${\beta}$-cyclodextrin on their retention and selectivity has been investigated. The inclusion effect of ${\beta}$-cyclodextrin was the most effective in aqueous methanol, whereas only a poor effect was observed in aqueous tetrahydrofuran and aqueous acetonitrile. A plot of the reciprocal of the capacity factor against $[CD]_T$ gives a straight line and the dissociation constant, $K_D$ of the inclusion complex can be calculated from the slope. It was possible to estimate the $k_D$ values in 100% water from a linear plot of $pK_D$ vs. water content in the solution by extrapolation. The separation factor, ${\alpha}$, of two compounds has been found to be affected not only by the $[CD]_T$ but also by their $K_D$ values. Under optimum conditions, some mixtures of phenol derivatives were able to separate successfully.

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A Study on the Analytical Method of Artificial Sweeteners in Foods (식품 중 인공감미료의 분석법에 관한 연구)

  • Kim, Hee-Yun;Yoon, Hae-Jung;Hong, Ki-Hyung;Lee, Chang-Hee;Park, Sung-Kwan;Choi, Jang-Duck;Choi, Woo-Jeong;Park, Sun-Young;Kim, Ji-Hye;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.36 no.1
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    • pp.14-18
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    • 2004
  • Analysis methods of artificial sweeteners, aspartame, acesulfame potassium, sodium saccharin, and sucralose isolated from foods were developed using high performance liquid chromatography, HPLC conditions for aspartame, acesulfame potassium, and sodium saccharin were: column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, 0.05M sodium phosphate monobasic : acetonitrile (9 : 1, pH 3.5, containing 0.01M tetrapropylammonium hydroxide); detector, UV detector at 210 nm. HPLC condition for sucralose were : column, Symmetry $C_{18}(3.9mm\;i.d{\times}150mm,\;5{\mu}m)$; mobile phase, water:methanol (7 : 3); detector, refractive index detection (sensitivity = 16). Recoveries of artificial sweeteners in foods including soft drinks, fruit and vegetable beverages, alcoholic beverages, fermented milk beverages, soybean milk, ice cream, snacks, chewing gums, jam, honey, kimchi salted food, special dietary products, processed fish products, candies, food additive mixtures, chocolate and cocoa were 76.1-101.3%, 82.3-103.2%, 83.1-103.7%, and 80,6-99.5% for aspartame, acesulfame potassium, sodium saccharin, and sucralose, respectively.