• 제목/요약/키워드: methanol separation column

검색결과 144건 처리시간 0.034초

인삼 사포닌의 High Performance Liquid Chromatography에 의한 분리 (High Performance Liquid Chromatographic Determination of Ginseng Saponins)

  • 홍순근;박은규;이춘영;김명운
    • 약학회지
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    • 제23권3_4호
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    • pp.181-186
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    • 1979
  • A high performance liquid chromatograpic procedure is described for determining ginseng saponins such as ginsenoside-Rb1, -Rb2, -Rc, -Rd, -Re, -Rf, -Rg1, and-Rg2. Ginseng saponins extracted with 90% methanol and water-saturated butanol were compared with pure standard ginsenosides. The resolution of the saponins was satisfactory and detection limit for each saponin was about 5.mu.g. Separation of the saponins was accomplished using a .mu. Bondapak carbohydrate analysis column, mobile phase of acetonitrile-water-butanol (80:20:15) and differential refractive index (RI) detector. The reproducibility and the recovery were also studied. This method was applied for determining the saponin contents of several parts of leaf, fresh ginseng, white ginseng, and red ginseng.

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Hydrolysis kinetics of Metampicillin by High Performance Liquid Chromatography

  • Lee, Hee-Yong;Jang, Won-Cheoul;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • 제17권5호
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    • pp.378-380
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    • 1994
  • The hydrolysis of metampicillin to ampicillin was investigated using high perofrmance liquid chromatography. We developed the simultaneous determination of metampicillin and ampicilin using a Zorbox CN column and 5% acetonitrile and 8% methanol in 0.02 M phosphate buffer (pH 7.0) as mobile phase. Matampicillin was hdyrolyzed to ampicillin with half life of 41.5 min at physiological pH and temperature. In acdic pH, metampicillin was rapidly hydrolyzed to ampicillin within a chromatogrphic separation.

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Chiral Separation of $\beta$-Blockers after Derivatization with (-)-Menthyl chloroformate by Reversed-Phase High Performance Liquid Chromatography

  • Kim, Kyeong-Ho;Choi, Pok-Wha;Hong, Seon-Pyo;Kim, Hyun-Ju
    • Archives of Pharmacal Research
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    • 제22권6호
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    • pp.608-613
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    • 1999
  • Optimum conditions of chiral derivatization reaction of $\beta$-blockers (acebutolol, arotinolol, betaxolol, bisoprolol, celiprolol, metoprolol and pindolol) with (-)-menthyl chloroformate were investigated for the resolution by HPLC. With more than 30 times molar excess of (-)-methyl chloroformate chiral derivatization reactions were completed within one hour at room temperature except arotinolol and celiprolol. Diastereomeric derivatives of $\beta$-blockers were well resolved on the ODS column using acetonitrile-methanol-water as a mobile phase.

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한국산 식용식물의 화학성분 및 생리활성에 관한 연구 (II) - HPLC에 의한 참죽나무 잎중 Flavonoid 성분의 확인 및 정량 - (Studies on the Chemical Components and Biological Activities of Edible Plants in Korea (II) - Isolation and Quantitative Analysis of Flavonoids from the Leaves of Cedrela sinensis A. Juss. by HPLC -)

  • 박종철;전순실;양한석;김성환
    • 한국식품영양과학회지
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    • 제22권5호
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    • pp.581-585
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    • 1993
  • 참죽나무(Cedrela sinensis A. Juss.) 잎의 ethyl acetate분획으로부터 분리한 5종의 flavonoid성분들은 HPLC에 의한 용매계 THF-dioxane-MeOH-HOAc-5% $H_3PO_4-H_2O$(145 : 125 : 50 : 20 : 2 : 658)에서 양호한 분리능을 나타내었다. 또한 주성분인 quercitrin의 함량은 MeOH엑스 및 EtOAc 분획에서 각각 9.48%(w/w) 및 37.06%(w/w) 함유되어 있음을 알 수 있었다.

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Distribution of (-)-Yatein in Cupressaceae Family Analysed by High Performance liquid Chromatography

  • Hwang, Gwi-Seo;Phuong, Nguyen-Thi;Park, Kyung-Rae;Kim, Young-Ho;Kim, Kyeong-Ho;Kang, Jong-Seong
    • Archives of Pharmacal Research
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    • 제27권1호
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    • pp.35-39
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    • 2004
  • The method for the chiral analysis of (-)-yatein was developed and the distribution of this component in the plants of three genera like Juniperus, Thuja and Chamaecyparis belonging to Cupressaceae family was examined. The chiral analysis of (-)-yatein from the plants was carried out by high performance liquid chromatography on (R,R)-Whelk-O1 column using 81 v/v% methanol as mobile phase. The yatein content in the leaves of Juniperus was the highest in compare with that of the other two genera, providing the possibility of the chemical discrimination of the plants in Juniperus from the other plants in the Cupressaceae family. In general, the yatein content in the leaves was much higher than that in the twigs. This method could be applied for the quality control of (-)-yatein in the plants belonging to Cupressaceae family.

Quantitative determination of pseudoephedrine in human plasma by reversed-phase liquid chromatography-electrospray ionization mass spectrometry

  • Kim, Jin-Ki;Cho, Jung-Hye;Woo, Jong-Soo;Kim, Chong-Kook
    • 대한약학회:학술대회논문집
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    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
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    • pp.394.2-394.2
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    • 2002
  • A sensitive and selective reversed-phase LC-ESI-MS method to quantitate pseudoephedrine in human plasma was developed and validated. Phenacetin was used as an internal standard. Samples were prepared simply by acetonitrile precipitation without an evaporation step. Chromatographic separation was achieved on a XTerra MS C18 column ($150{times}2.1$ mm I.D.. 3.5 $\mu\textrm{m}$ particles). using gradient elution with 0.5% (v/v) trifluoroacetic acid (TFA) in water and 0.5% (v/v) TFA in methanol at a flow-rate of 0.1 ml/min. (omitted)

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Studies on the quantification of sobrerol by high-performance liquid chromatography

  • Lee, Dong-Mi;Won, Young-Jun;Yoon, Chang-Yong;Seo, Il-Won;Nam, Hye-Seon;Park, Dong-Hee;Lee, Hyang-Mi;Kim, Se-Sil;Jung, Eun-Mi
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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    • pp.283.1-283.1
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    • 2003
  • This study was designed to develop and validate an isocratic reversed phase high performance liquid chromatographic(HPLC) method for the quantitation of sobrerol in drug preparations, and obtain the data pool that can be used in the revision of pharmacopoeia. The separation of sobrerol and the other compounds (S-carboxymethylcysteine, acetaminophen, methyl paraben, propyl paraben, and sobrerol degradants) was achieved in a C18 column with an acetonitrile-methanol-water(24.5:10.5:65.0) mobile phase. (omitted)

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Comparison of Anthocyanin Content in Seed Coats of Black Soybean [Glycine max(L.) Merr.] Cultivars Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

  • Shin, Sung-Chul;Lee, Soo-Jung;Lee, Sung-Joong;Chung, Jong-Il;Bae, Dong-Won;Kim, Soo-Taek;Sung, Nak-Ju
    • Food Science and Biotechnology
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    • 제18권6호
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    • pp.1470-1475
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    • 2009
  • The seed coat of the black soybean contains 3 main anthocyanins such as delphinidin-3-O-$\beta$-glucoside, cyanidin-3-O-$\beta$-glucoside, and petunidin-3-O-$\beta$-glucoside. As a part of our effort on discovering and breeding new black soybean cultivars which possesses specific anthocyanin component rich, we determined the anthocyanin profiles of the 2 cultivars recently developed soybean cv. Gaechuck #1 and cv. Gyeongsang #1, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and compared their content and identity with those of previously known 10 cultivar controls. The Cosmosil-$5C_{18}$-AR-II column were selected for the analysis because of the best peak separation. The column temperature was set up at $35^{\circ}C$. The mobile phase consisting of water containing 0.5%(v/v) formic acid and methanol gave good separation between the 3 anthocyanin analytes and internal standard (quercetin 3-O-$\beta$-rutinoside) and peaks with suppressed tail. The MS/MS spectra of each individual anthocyanin standard were detected in positive electron spray ionization (ESI) modes. It was disclosed that the anthocyanin contents of the soybean cv. Gaechuck#1 and cv. Gyeongsang#1 are roughly higher than those of the 10 controls.

인체 혈장 중 Ginsenoside Rg1의 정량을 위한 LC-MS/MS 분석법 검증 (Validation of LC-MS/MS method for determination of ginsenoside Rg1 in human plasma)

  • 김윤정;한송희;전지영;황민호;임용진;이선영;채수완;김민걸
    • 분석과학
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    • 제26권4호
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    • pp.221-227
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    • 2013
  • LC-MS/MS를 이용하여 인체 혈장 중 ginsenoside Rg1의 신속하고 정확한 분석법을 개발하고 이 분석법에 대한 검증을 수행하였다. 혈장 분석을 위하여 internal standard인 digoxin을 첨가한 후 acetone과 methanol용액 (80:20)으로 전처리하고, 그 상층액을 진공농축 한 후, LC-MS/MS로 분석하였다. 최적 크로마토그래피 분석은 0.1% formic acid 첨가된 water와 methanol을 이동상으로 하여 Agilent Eclipse XDB-C18 column ($4.6{\times}150mm$, $5{\mu}m$)을 이용하여 0.9 mL/min의 유속으로 gradient mode로 수행하였다. 혈장 중 ginsenoside Rg1의 표준 검량선은 1~500 ng/mL의 농도 범위에서 우수한 직선성($r^2=0.9995$)을 보였으며, 일내, 일간 정밀성은 변동계수 7.53% 이하, 정확성은 98.28% 이상이었다. 결과적으로 본 분석법은 ginsenoside Rg1의 약동학 연구에 적용되기에 충분한 감도와 특이성, 직선성, 정밀성 및 정확성을 가지고 있음을 확인하였다.

The Simulation and Control of the Reactive Distillation Process for Dimethylcarbonate(DMC) Production

  • Jang, Yong-Hee;Yang, Dae-Ryook
    • 제어로봇시스템학회:학술대회논문집
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    • 제어로봇시스템학회 2004년도 ICCAS
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    • pp.1215-1220
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    • 2004
  • Reactive distillation (RD) is a combination process where both separation and reaction are considered simultaneously in a single vessel. This kind of combination to enhance the overall performance is not a new attempt in the chemical engineering areas. The recovery of ammonia in the classic Solvay process for soda ash of the 1860s may be cited as probably the first commercial application of RD. The RD system has been used for a long time as a useful process and recently the importance of the RD is enlarged more and more. In addition to that, the application fields of RD are diversely diverged. To make the most of the characteristic of RD system, we must decide the best operating condition under which the process shows the most effective productivity and should decide the best control algorithm which satisfies an optimal operating condition. Phosgene which is a highly reactive chemical is used for the production of isocyanates and polycarbonates. Because it has high reactivity and toxicity, its utilization is increasingly burdened by growing safety measures to be adopted during its production. Dimethyl Carbonate (DMC) was proposed as a substitute of phosgene because it is non-toxic and environmentally benign chemical. In this study, RD is used for DMC production process and the transesterification is performed inside of column to produce DMC. In transesterification, the methanol and ethylene carbonate (EC) are used as the reactants. This process use homogeneous catalyst and the azeotrope exists between the reactant and product. Owing to azeotrope, we should use two distillation columns. For this DMC production process, we can suggest two configurations. One is EC excess process and the other is methanol excess process. From the comparison of steady state simulation results where the Naphtali-Sandholm algorithm is used, it showed the better performance to use the methanol excess process configuration than EC excess process. Then, the dynamic simulation was performed to be based on the steady state simulation results and the optimal control system was designed. In addition to that, the optimal operating condition was suggested from previous results.

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