• Title/Summary/Keyword: Retention Time of Liquid Phase

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A Study on the Supercooling Improvement of TMA -Clathrate Compound by Ethanol (에탄올에 의한 TMA- 포접화합물의 과냉각 개선에 대한 연구)

  • Kim, Jin-Heung;Chung, Nak-Kyu;Kim, Chang-Oh
    • Proceedings of the SAREK Conference
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    • 2005.11a
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    • pp.392-397
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    • 2005
  • This study is investigated the supercooling improvement and the phase change temperature of the TMA clathrate compound including TMA(Tri-Methyl-Amine, ($(CH_3)_3N$) of 25 wt% with additive as a low temperature storage material at $6^{\circ}C$ and $-7^{\circ}C$ of heat source. The additive is ethanol of 0.1, 0.3 wt% and 0.5 wt%. The results showed that as the concentration of ethanol is increased, the phase change temperature, the degree of supercooling and the retention time of liquid phase are decreased. Especially, TMA 25 wt% clathrate compound with ethanol of 0.5wt% has the average of phase change temperature of $3.8^{\circ}C$, degree of supercooling of $0.9^{\circ}C$, $0.8^{\circ}C$ and retention time of liquid phase for 6, 5 minutes at $-6^{\circ}C$, $-7^{\circ}C$ of heat source. From the results of this study, TMA 25wt% clathrate compound with ethanol 0.5wt% showed supercooling repression effect.

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Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

Chiral Separation of Tryptophan Enantiomers by Liquid Chromatography with BSA-Silica Stationary Phase

  • Kim Kwonil;Lee Kisay
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.5 no.1
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    • pp.17-22
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    • 2000
  • The separation of tryptophan enantiomers was carried out with medium-pressure liquid chromatography using BSA (bovine serum albumin)-bonded silica as a chiral stationary phase. The influence of various experimental factors such as pH and ionic strength of mobile phase, separation temperature, and the presence of organic additives on the resolution was studied. In order to expand this system to preparative scale, the loadability of sample and the stability of stationary phase for repeated use were also examined. The separation of tryptophan enantiomers was successful with this system. The data indicated that a higher separation factor (a) was obtained at a higher pH and lower temperature and ionic strength in mobile phase. Addition of organic additives (acetonitrile and 2-propanol) in mobile phase contributed to reduce the retention time of L-tryptophan. About $30\%$ of the separation factor was reduced after 80 days of repeated use.

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Purification of 4-Methylthio-3-butenyl isothiocyanate the Pungent Principle in Radish Roots by RP-HPLC (RP-HPLC법에 의한 무우의 매운 성분인 4-methylthio-3-butenyl isothiocyanate의 분리 및 정제)

  • Kim, Mee-Ree;Rhee, Hei-Soo
    • Korean journal of food and cookery science
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    • v.2 no.2
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    • pp.16-20
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    • 1986
  • The major pungent component from Korean radish roots was purified by reverse phase high performance liquid chromatography (RPHPLC), and characterized as 4-methylthio-3-butenyl isothiocyanate on the basis of the sensory test (pungency), UV spectrum and mass spectrum analysis. The purified isothiocyanate moved as a single peak(retention time, 5.2 min) in RP-HPLC analysis, and as a single spot(Rf, 0.9) in TLC analysis.

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Effects of Polyurethane as Support Material for the Methanogenic Digester of a Two-Stage Anaerobic Wastewater Digestion System

  • Woo, Kyung-Soo;Yang, Han-Chul;Lim, Wang-Jin
    • Journal of Microbiology and Biotechnology
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    • v.12 no.1
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    • pp.14-17
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    • 2002
  • To increase the efficiency of a two-stage anaerobic wastewater digestion system, various polymers were added to the methanogenic reactor as supports. The addition of polyurethane addition (6%, w/v) to the methanogenic reactor facilitated the organic loading rate (2-day Hydraulic Retention Time), higher than that of the conventional methanogenic reactor (6-day HRT). During the operation of the polyurethane-added reactor, a significant decrease in the organic mass in the effluent (COD 5-6 kg/l) was achieved, compared to that of the conventional reactor (COD 15-20 kg/l). The methane gas production rate also improved about 3-fold in the polyurethane-added reactor. More biomass was found to accumulate in the polyurethane-liquid phase (volatile solid, 26-28kg) than in the free-liquid phase (volatile solid, 5- 7 kg/l) after 90 days of operation. A scaled-up experiment with a polyurethane-added 2.5-1 reactor confirmed the previous results, and no adverse effects such as plugging or channeling due to decreased efficiency was observed even after 4 months of operation.

Hydrophilic Interaction Liquid Chromatography (HILIC 분석법 개발을 위한 지능형 솔루션)

  • Matt James;Colin Pipe;Mark Fever;Jen Field;Seungho Chae
    • FOCUS: LIFE SCIENCE
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    • no.1
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    • pp.6.1-6.9
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    • 2024
  • The document is a white paper on Hydrophilic Interaction Liquid Chromatography (HILIC) analysis method development. HILIC is a type of chromatography that uses an organic/aqueous mobile phase and a polar stationary phase. In HILIC, water is a strong solvent, and unlike in Reversed Phase Liquid Chromatography (RPLC), increasing the proportion of water in the mobile phase reduces the retention time of the analyte. The paper discusses when to consider HILIC analysis methods, the advantages of HILIC, and the challenges often encountered due to the lack of understanding of HILIC mechanisms compared to RPLC. It also provides a systematic flowchart for intelligent solutions for HILIC analysis method development, which includes a three-step approach for chromatography analysis method development. The first step involves gathering as much information as possible about the analyte (e.g., pKa, log P, log D). The second step involves analyzing the sample under different pH conditions using three HILIC columns in either isocratic or gradient mode to identify the suitable column/pH combination for the analyte. The third step involves optimizing the separation by investigating other parameters such as temperature and ionic strength, and assessing the robustness of the method. The paper emphasizes that the selection of the appropriate stationary/mobile phase combination, based on the differences between the HILIC stationary phases and the mobile phase pH, can provide high selectivity in the analysis. This step-by-step approach can help users develop an efficient analysis method.

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A Study on Cooling Characteristics of Clathrate Compound with Concentration of TMA (TMA 농도에 따른 포접화합물의 냉각특성에 대한 연구)

  • Kim Jin-Heung;Chung Nak-Kyu;Kim Chang-Oh
    • Journal of Energy Engineering
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    • v.14 no.1
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    • pp.18-23
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    • 2005
  • This study is investigated the cooling characteristics of the TMA clathrate compound including TMA (Tri-methyl-amine, (CH₃)₃N) of 20~25 wt% as a low temperature storage material at -5℃ heat source. The results showed that as the concentration of TMA is increased, phase change temperature and specific heat are increased, but the supercooling and retention time of liquid phase are decreased. Especially, low temperature storage material containing TMA 25 wt% has the average of phase change temperature of 5.8℃, supercooling of 8.0℃, retention time of liquid phase for 10 minutes and specific heat of 4.099 kJ/kg℃ in the cooling process. From the results of this study, TMA clathrate compound showed higher phase change temperature than water md supercooling repression effect.

Quantitative Determination of Salidroside and Tyrosol from the Underground Part of Rhodiola rosea by High Performance Liquid Chromatography

  • Linh, Pham-Tuan;Kim, Young-Ho;Hong, Seon-Pyo;Jian, Jiang-Ji;Kang, Jong-Seong
    • Archives of Pharmacal Research
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    • v.23 no.4
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    • pp.349-352
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    • 2000
  • A reversed-phase high performance liquid chromatographic method was developed to determine salidroside and tyrosol simultaneously in the Rhodiola rosea. The optimum condition was Nova-pak $C_18$as stationary phase, 6.5% methanol in water as mobile phase and detection at UV 225 nm. The identification was carried out by comparing the retention time and LC/MS spectrum of the relevant peaks with those of isolated standards. The contents of salidroside and tyrosol in the samples gathered from various area in China were ranged over 1.3-11.1 ${m}g/g$ and 0.3-2.2 ${m}g/g$, respectively.

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Mobile Phase Compositions for Ceramide III by Normal Phase High Performance Liquid Chromatography

  • Hong, Seung-Pyo;Lee, Chong-Ho;Kim, Se-Kyung;Yun, Hyun-Shik;Lee, Jung-Heon;Row, Kyung-Ho
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.9 no.1
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    • pp.47-51
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    • 2004
  • Ceramide III was prepared by the cultivation of Saccharomyces cerevisiae. Ceramide III was partitioned from the cell extracts by solvent extraction and analyzed by Normal Phase High Performance Liquid Chromatography (NP-HPLC) using Evaporative Light Scattering Detector (ELSD). We experimentally determined the mobile phase composition to separate ceramide III with NP-HPLC. Three binary mobile phases of n-hexane/ethanol, n-hexane/lsoprophyl Alcohol(IPA) and n-hexane/n-butanol and one ternary mobile phase of n-hexane/IPA/methanol were demonstrated. For the binary mobile phase of n-hexane/ethanol, the first mobile phase composition, 95/5(v/v), was step-increased to 72/23(v/v) at 3 min. In the binary mobile phase, the retention time of ceramide III was 7.87min, while it was 4.11 min respectively in the ternary system, where the mobile phase composition of n-hexane/IPA/methanol, 85/7/8(v/v/v), was step-increased to 75/10/15(v/v/v) at 3 min. However, in the ternary mobile phase, the more peak area of ceramide III was observed.

The Rapid Determination of Gemcitabine by Reversed-phase Ultra-Performance Liquid Chromatography (역상 초고속액체크로마토그라피에 의한 gemcitabine의 빠른 농도 분석법)

  • Park, Dae-Jin;Kim, Woo-Mi
    • Journal of Life Science
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    • v.19 no.12
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    • pp.1698-1704
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    • 2009
  • Gemcitabine is an anticancer drug used to treat a variety of solid tumors. The drug is rapidly inactivated by cytidine deaminase in plasma and its hydrophilicity restricts the extent of quantification that is possible using reversed-phase liquid chromatography. In this paper, we report a rapid and precise method to analyze velocity and peak efficiency using ultra-performance liquid chromatography (UPLC) with a reversed-phase column. The retention periods of gemcitabine and 2'-deoxycytidine at 283 nm were 3.2 and 2.1 min, respectively. The assay provided highly linear results in the range of $0.1{\sim}20{\mu}g/ml$ ($r^2$ > 0.999). The coefficients of variation of the intra-day and inter-day assays were less than 10.0%. We observed that the estimated average concentrations of the intra-day and inter-day assays ranged from 97.3 to 113.5% to verify the accuracy. These results suggest that this new reversed-phase UPLC method is a rapid and reliable way of determining gemcitabine levels.