• Title/Summary/Keyword: liquid-phase

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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.

Determination of Non-Steroidal Anti-Inflammatory Drugs in Human Urine Sample using HPLC/UV and Three Phase Hollow Fiber-Liquid Phase Microextraction (HF-LPME)

  • Cha, Yong Byoung;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3444-3450
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    • 2013
  • Three phase hollow fiber-liquid phase microextraction (HF-LPME), which is faster, simpler and uses a more environmentally friendly sample-preparation technique, was developed for the analysis of Non-Steroidal Anti-Inflammatory Drugs (NSAIDs) in human urine. For the effective simultaneous extraction/concentration of NSAIDs by three phase HF-LPME, parameters (such as extraction organic solvent, pH of donor/acceptor phase, stirring speed, salting-out effect, sample temperature, and extraction time) which influence the extraction efficiency were optimized. NSAIDs were extracted and concentrated from 4 mL of aqueous solution at pH 3 (donor phase) into dihexyl ether immobilized in the wall pores of a porous hollow fiber, and then extracted into the acceptor phase at pH 13 located in the lumen of the hollow fiber. After the extraction, 5 ${\mu}L$ of the acceptor phase was directly injected into the HPLC/UV system. Simultaneous chromatographic separation of seven NSAIDs was achieved on an Eclipse XDB-C18 (4.6 mm i.d. ${\times}$ 150 mm length, 5 ${\mu}m$ particle size) column using isocratic elution with 0.1% formic acid and methanol (30:70) at a HPLC-UV/Vis system. Under optimized conditions (extraction solvent, dihexyl ether; $pH_{donor}$, 3; $pH_{acceptor}$, 13; stirring speed, 1500 rpm; NaCl salt, 10%; sample temperature, $60^{\circ}C$; and extraction time, 45 min), enrichment factors (EF) were between 59 and 260. The limit of detection (LOD) and limit of quantitation (LOQ) in the spiked urine matrix were in the concentration range of 5-15 ng/mL and 15-45 ng/mL, respectively. The relative recovery and precision obtained were between 58 and 136% and below 15.7% RSD, respectively. The calibration curve was linear within the range of 0.015-0.96 ng/mL with the square of the correlation coefficient being more than 0.997. The established method can be used to analyse of NSAIDs of low concentration (ng/mL) in urine.

Liquid Crystalline Technology of Cosmetic Industry and Moisturizing Effect of Skin (화장품 산업의 액정기술과 피부보습효과)

  • 김인영;조춘구;유희창
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.30 no.2
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    • pp.279-294
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    • 2004
  • This study described about a liquid crystalline technology that is used in cosmetics industry. Various intermediate phases may exist between solid and liquid. At high surfactant concentration, several liquid crystalline phases can be made to have formed. Although molecular arrangement with crystallization is not regular, it is known that more relative regular state is liquid crystalline or meso-phase than liquid phase. Usually, it described in detail about manufacturing method that explained about a kind of liquid crystalline technology in cosmetics, a new liquid crystalline technology, and makes liquid crystalline. Specialty, it introduced about kind of special an emulsifier to form liquid crystalline. There were hydrogenated lecithin, ceramide, dipalmitoylhydroxyproline, DEA-cetyl phosphate, Gemini-surfactant in representative raw material to form liquid crystalline. Liquid crystalline extent that used polarization microscope to observe formation, and appears best from 400times, 600times, 1,000times well appeared. Also, droplet particle size that liquid crystal is made best 1.0-10.0$\mu\textrm{m}$ be. General emulsion more than superior result that measures the skin moisturizing effect to take advantage of liquid crystalline technology of vitamin was seen. As presence at a clinical result, wave and general emulsion more than superior result (more than 20%) that measures skin moisturizing effect about liquid crystalline of vitamin B$\_$5/ were seen (ANOMA t-test, p<0.05)

Headspace Hanging Drop Liquid Phase Microextraction and GC-MS for the Determination of Linalool from Evening Primrose Flowers

  • Kim, Nam-Sun;Jung, Mi-Jin;Yoo, Zoo-Won;Lee, Sun-Neo;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1996-2000
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    • 2005
  • Headspace hanging drop liquid phase micro-extraction (HS-HD-LPME) is studied as a novel solvent-based sample pretreatment method for floral volatile aroma compounds. This paper reports on application of the HSHD- LPME combined with GC-MS for the analysis of linalool component emitted from evening primrose flowers. The effect of several variables on the method performance was investigated. Additionally, the separation of enantiomers on a cyclodextrin capillary column was performed to identify chirality of (−)-linalool component. Since the unsurpassed volume of a few micro-liters of solvent is used, there is minimal waste or exposure to toxic organic solvents. This method enables to combine extraction, enrichment, clean-up, and sample introduction into a single step prior to the chromatographic process.

Electro-optical devices from polymer-stabilized liquid crystals with molecular shape polarity

  • Kim, Sang-Hwa;Chien, Liang Chy;Komitov, Lachezar
    • 한국정보디스플레이학회:학술대회논문집
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    • 2004.08a
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    • pp.839-842
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    • 2004
  • We present a fast-switching electro-optical device based on flexoelectro-optic effect in short pitch cholesterics oriented in uniform lying helix texture. The device has two operating modes: amplitude and phase modulation mode. The amplitude modulation mode is a fast in-plane switching of the device optic axis that enables to achieve a high percent of modulation of the transmitted light intensity whereas the phase mode gives a continuous change of the refractive index and thus of the phase shift of the transmitted light. By using a small concentration of diacrylate monomer and selecting the illumination conditions we have been able to create a inhomogeneous polymeric network mostly localized at both substrate surfaces and stabilize the two switching modes.

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Effect of Organic Admixture(Calcium Lignosulfonate) on the Early Hydration Process of Portland Cement(III) (시멘트 초기수화과정에 대한 유기혼화제의 영향(III))

  • 문정연;최상홀
    • Journal of the Korean Ceramic Society
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    • v.22 no.1
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    • pp.5-10
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    • 1985
  • The effect of calcium lignosulfonate (CLS) on the early hydration characteristics for clinker minerals was investigated. In the presence of CLS and unsufficient gypsum The hydration of $C_3$A lowered CLS adsorption to form ettrin-gite and the residual CLS in the liquid phase accelerated the solubility of C4AF hydration. As the result unreacted $Fe^{3+}$ in the liquid phase would be precipitated gelatinously on $C_3$ hydrates and the hydration of $C_3$ could be retarded. But by addition of optimum gypsum into the cement with CLS the presence of $Fe^{3+}$ in the liquid phase were lowered and $C_3$ hydration would be normallized.

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Effects of Particle Size of Alumina on the Behaviors of Tape Casting and Sintering of Alumina-Talc System (알루미나-활석계에서 알루미나의 입자 크기가 테이프 케스팅 및 소결 거동에 미치는 영향)

  • 윤원균;김호양;이정아;김정주
    • Journal of the Korean Ceramic Society
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    • v.34 no.12
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    • pp.1213-1220
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    • 1997
  • Effect of particle size of alumina and amount of talc on tape casting and densification behaviors of alumina-talc system were investigated. The pseudoplastic behaviors of slurries increased with increase in amount of talc addition and decrease in alumina particle size. In case of using coarse alumina powder, densification of specimens were accelerated with increase of sintering temperature and amount of talc addition. On the contrary, fine alumina powder retarded of rearrangement of alumina particle during liquid phase sintering due to premature densification of alumina matrix region before formation of liquid phase and then densification of specimens were suppressed with increase of sintering temperature and amount of talc addition.

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Development of Performance Test Apparatus and Design Program of Liquid-Phase Plate Heat Exchanger (액상 판형열교환기 성능실험장비 및 설계프로그램 개발)

  • Park, Sang-Il;Song, Young-Ho
    • Proceedings of the KSME Conference
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    • 2004.11a
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    • pp.1306-1311
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    • 2004
  • The performance test apparatus of liquid-phase plate heat exchanger was installed and the computer program for design was developed in this study. The detail temperature distribution of hot and cold fluids in each path of heat exchanger was calculated by numerical method and the correlation for the heat transfer coefficient was defined. The heat transfer coefficients were measured using the working fluids of water and glycerine to investigate the effect of fluid viscosity. The measured heat transfer coefficients were compared with the calculated values obtained from the computer program and it was shown that error of the calculated values was generally less than 5%.

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Liquid-phase Dehydration of 1-Phenylethanol to Styrene over an Acidic Resin Catalyst

  • Khan, Nazmul Abedin;Hwang, Jin-Soo;Jhung, Sung-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.32 no.4
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    • pp.1327-1330
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    • 2011
  • Dehydration of 1-phenylethanol to produce styrene has been studied in liquid phase with three solid acid catalysts such as H-ZSM-5, H-Y and Amberlyst-15. Amberlyst-15 shows the highest conversion and styrene yield, suggesting the applicability of a resin catalyst in the dehydration. The good performance of the Amberlyst-15 may be due to high acid concentration and ready diffusion of reactants and products. A possible reaction scheme (such as the formation of styrene from diphenylethylether) has also been suggested.

Prediction of Pressure Drop in Venturi Scrubber Using the Eulerian - Lagrangian Method (오일러-라그랑지 방법을 이용한 벤튜리 스크라버의 압력강하 계산)

  • Pak S, I.;Moon Y. W.;Chang K. S.
    • 한국전산유체공학회:학술대회논문집
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    • 2004.03a
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    • pp.190-195
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    • 2004
  • The pressure drop in a Venturi Scrubber is predicted using the Eulerian-Lagrangian Method, which is one of the numerical methods to solve the dispersed two-phase flow. KIVA-3V Code is modified to solve the coupled gas-liquid two-phase flow field. The liquid is assumed to be injected through the nozzles with the Rosin-Rammler drop size distribution. The computational results shows good agreement with the experimental data.

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