• 제목/요약/키워드: Retention Time of Liquid Phase

검색결과 73건 처리시간 0.024초

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

  • 김진흥;정낙규;김창오
    • 대한설비공학회:학술대회논문집
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    • 대한설비공학회 2005년도 동계학술발표대회 논문집
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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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    • 제34권6호
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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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    • 제5권1호
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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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RP-HPLC법에 의한 무우의 매운 성분인 4-methylthio-3-butenyl isothiocyanate의 분리 및 정제 (Purification of 4-Methylthio-3-butenyl isothiocyanate the Pungent Principle in Radish Roots by RP-HPLC)

  • 김미리;이혜수
    • 한국식품조리과학회지
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    • 제2권2호
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    • pp.16-20
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    • 1986
  • 무우 속의 매운 맛 성분을 용매추출법 ($CCl_4$,사용)으로 분리하여 RP-HPLC법에 의해 정제한 후에 관능검사에 의해 pungency test를 하고, UV spectrum분석, GC/MC 분석을 수행한 결과 4-methylthio-3-butenyl isothiocyanate 임을 확인하였다. RP-HPLC에서 mobile Phase로 70% acetonitrile을 사용하였는데, 정제된 4-methylthio-3-butenyl isothiocfanate는 단일 peak로 분리되어 나왔고 이때의 retention time은 5.2분이였다. 아울러 RP-TLC에서 Rf치는 0.9이었다.

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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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    • 제12권1호
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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.

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

  • Matt James;Colin Pipe;Mark Fever;Jen Field;Seungho Chae
    • FOCUS: LIFE SCIENCE
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    • 제1호
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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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TMA 농도에 따른 포접화합물의 냉각특성에 대한 연구 (A Study on Cooling Characteristics of Clathrate Compound with Concentration of TMA)

  • 김진흥;정낙규;김창오
    • 에너지공학
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    • 제14권1호
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    • pp.18-23
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    • 2005
  • 본 연구는 저온축열물질로서 TMA(Tri-methyl-amine, (CH₃)₃N)를 20~25 wt%로 포함하고 있는 TMA-물계 포접화합물의 냉각특성에 대하여 냉열원온도 -5℃에서 실험적으로 연구를 수행하였다. 연구결과, TMA의 질량농도가 증가할수록 상변화온도와 비열이 증가하였으며, 과냉도가 감소하고 액상유지시간이 단축되었다 특히, TMA 25wt%를 포함한 TMA-물계 포접화합물은 상변화온도 평균 5.8℃, 과냉도 8.0℃, 액상유지시간 10분, 비열 4.099kJ/kg℃를 나타내었다. 본 연구의 결과로부터 TMA-물계 포접화합물은 물보다 높은 상변화온도를 나타내었으며, 과냉도가 감소하고, 액상유지시간이 단축되는 과냉각 억제효과를 확인 할 수 있었다.

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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    • 제23권4호
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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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    • 제9권1호
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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.

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

  • 박대진;김우미
    • 생명과학회지
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    • 제19권12호
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    • pp.1698-1704
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    • 2009
  • Gemcitabine은 다양한 고형암 치료에 사용되는 항암제이다. 혈장내에서 cytidine deaminase에 의해 빠르게 대사되며, 친수성 성질로 인해 역상 액체크로마토그라피(reversed-phase liquid chromatography)를 이용한 농도 분석이 어렵다. 본 연구에서는 역상칼럼(reversed-phase column)을 이용한 초고속 액체크로마토그라피(ultra-performance liquid chromatography, UPLC) 방법에 의해 빠르고 정확한 속력(velocity)과 최고효능(peak efficiency)를 갖춘 분석법을 개발하고자 하였다. Gemcitabine과 2'-deoxycytidine의 머무름 시간(retension time)은 293 nm에서 각각 3.2분과 2.1분이었다. 검량선의 직선성 검정은 $0.1{\sim}20{\mu}g/ml$의 농도범위에서 높은 직선성을 나타내었다($r^2$>0.999). 일내(intra-day) 변이게수(coefficients of variation)와 일간(inter-day) 변이게수는 모두 10% 이하였다. 정확성(accuracy) 검정을 위한 일내 및 일간 평균농도 측정치가 97.3~113.5% 범위로 나타났다. 이러한 결과를 토대로, gemcitabine 농도를 측정하기 위한 새로운 분석법으로 빠르고 정확한 역상 UPLC 방법을 제안하고자 한다.