• Title/Summary/Keyword: micellar chromatography

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Ultrasonic-assisted Micellar Extraction and Cloud-point Pre-concentration of Major Saikosaponins in Radix Bupleuri using High Performance Liquid Chromatography with Evaporative Light Scattering Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2637-2642
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    • 2011
  • A new ultrasonic-assisted micellar extraction and cloud-point pre-concentration method was developed for the determination of major saikosaponins, namely saikosaponins -A, -C and -D, in Radix Bupleuri by high performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD). The non-ionic surfactant Genapol X-080 (oligoethylene glycol monoalkyl ether) was chosen as the extraction additive and parameters affecting the extraction efficiency were optimized. The highest yield was obtained with 10% (w/v) Genapol X-080, a liquid/solid ratio of 200:1 (mL/g) and ultrasonic-assisted extraction for 40 min. In addition, the optimum cloud-point pre-concentration was reached with 10% sodium sulfate and equilibration at $60^{\circ}C$ for 30 min. Separation was achieved on an Ascentis Express C18 column (100 ${\times}$ 4.6 mm i.d., 2.7 ${\mu}M$) using a binary mobile phase composed of 0.1% acetic acid and acetonitrile. Saikosaponins were detected by ELSD, which was operated at a $50^{\circ}C$ drift tube temperature and 3.0 bar nebulizer gas ($N_2$) pressure. The water-based solvent modified with Genapol X-080 showed better extraction efficiency compared to that of the conventional solvent methanol. Recovery of saikosaponins ranged from 93.1 to 101.9%. An environmentally-friendly extraction method was successfully applied to extract and enrich major saikosaponins in Radix Bupleuri.

Phytochemical analysis of Panax species: a review

  • Yang, Yuangui;Ju, Zhengcai;Yang, Yingbo;Zhang, Yanhai;Yang, Li;Wang, Zhengtao
    • Journal of Ginseng Research
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    • v.45 no.1
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    • pp.1-21
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    • 2021
  • Panax species have gained numerous attentions because of their various biological effects on cardiovascular, kidney, reproductive diseases known for a long time. Recently, advanced analytical methods including thin layer chromatography, high-performance thin layer chromatography, gas chromatography, high-performance liquid chromatography, ultra-high performance liquid chromatography with tandem ultraviolet, diode array detector, evaporative light scattering detector, and mass detector, two-dimensional high-performance liquid chromatography, high speed counter-current chromatography, high speed centrifugal partition chromatography, micellar electrokinetic chromatography, high-performance anion-exchange chromatography, ambient ionization mass spectrometry, molecularly imprinted polymer, enzyme immunoassay, 1H-NMR, and infrared spectroscopy have been used to identify and evaluate chemical constituents in Panax species. Moreover, Soxhlet extraction, heat reflux extraction, ultrasonic extraction, solid phase extraction, microwave-assisted extraction, pressurized liquid extraction, enzyme-assisted extraction, acceleration solvent extraction, matrix solid phase dispersion extraction, and pulsed electric field are discussed. In this review, a total of 219 articles published from 1980 to 2018 are investigated. Panax species including P. notoginseng, P. quinquefolius, sand P. ginseng in the raw and processed forms from different parts, geographical origins, and growing times are studied. Furthermore, the potential biomarkers are screened through the previous articles. It is expected that the review can provide a fundamental for further studies.

Molecular Analysis using High Performance Capillary Electrophoresis

  • Yoo, Young Sook;Ban, Eun Mi;Kim, Young Sook;Han, Yeosun;Park, Jongsei
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.881-886
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    • 1995
  • Several forms of gangliosides have been separated from various types of biological matrices using cyclodextrin-modified capillary zone electrophoresis (CZE). Quantitative analysis of phospholipids from biological fluids was achieved by micellar electrokinetic capillary chromatography (MECC) using 35mM sodium dodecyl sulfate. Phosphorylation, one of the most important post-translational modifications of proteins at serine, threonine and tyrosine residues in small peptides were identified and quantitative analyses of phosphopeptides were performed. Seven different neuropeptides which are relative the pain reachanism in the vertebrate central nervons system were also separated by CZE.

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Application of Capillary Electrophoresis for Quality Control Analysis of Complex Medicine (모세관 전기영동 분석법의 복합약물제제의 품질관리 분석에 응용을 위한 연구)

  • Heo, Yoo-Jeong;Lee, Kong-Joo
    • YAKHAK HOEJI
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    • v.41 no.5
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    • pp.539-546
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    • 1997
  • Capillary electrophoresis (CE) is perceived as an attractive tool for the analysis of pharmaceuticals and biological materials because of their high separation efficiency, easy separation and low running cost. New concept of micellar electrokinetic capillary chromatography (MECC) expanded the application of CE to the separation of neutral molecules. Validation of CE as an analytical technique for quality control of pharmaceuticals should be confirmed by quantitative analysis and the peak confirmation. In this study, the quantitative analyses of various types of neutral, acidic and basic components (acetaminophen, caffeine, ascorbic acid, riboflavin, thiamine, chlorpheniramine, phenylpropanolamine, dl-methylephedrine and dextromethorphan) in complex cold medicines have been accomplished using CE. Combined methods of MECC using SDS and capillary zone electrophoresis lowering the pH of running buffer were adopted to determine the ingredients in capsule type or liquid formula complex medicines without particular sample pretreatment. The results indicate that CE is a promising technique for quality control analysis of pharmaceuticals as a validation method.

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Effect of SDS on Retention of Nucleic Acid Components in High-Performance Liquid Chromatography

  • Kim Yong-Nam;Choi Kyeung-Soo;Lee Dai-Woon;Phyllis R. Brown
    • Bulletin of the Korean Chemical Society
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    • v.13 no.3
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    • pp.240-245
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    • 1992
  • The effect of the addition of sodium dodecyl sulfate (SDS) to a buffered mobile phase (pH 3.4) on the retention of nucleotides, nucleosides and bases was investigated with a polyvinyl alcohol (PVA) column. Depending on the concentration of SDS, two different trends in the retention of nucleosides and bases containing an $NH_2$ group were observed. If the concentration of SDS was less than 5.5 mM, the retention of compounds containing an $NH_2$ group increased as the concentration of SDS in the mobile phase increased. In contrast, if the concentration was greater than 5.5 mM, the retention of compounds containing an $NH_2$ group decreased. Thus, the SDS acted as an ion-pairing reagent at lower concentration but formed micelles at higher concentrations. The retention behavior of the nucleosides and bases in the presence of a micellar concentration of SDS in the mobile phase on the PVA column was compared to the retention behavior on other types of columns.

Synthesis and Characterization of MPEG-b-PDPA Amphiphilic Block Copolymer via Atom Transfer Radical Polymerization and Its pH-Dependent Micellar Behavior

  • Dayananda, Kasala;Kim, Min-Sang;Kim, Bong-Sup;Lee, Doo-Sung
    • Macromolecular Research
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    • v.15 no.4
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    • pp.385-391
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    • 2007
  • Block copolymer micelles are generally formed via the self-assembly of amphiphilic block copolymers in an aqueous medium. The hydrophilic and hydrophobic blocks form shell and core micelles, respectively. The block copolymers of methoxy poly(ethylene glycol) (MPEG)-b-poly(2-diisopropylamino)ethyl methacrylate (PDPA) were synthesized via atom transfer radical polymerization, with the macro initiator synthesized by the coupling of 2-bromoisobutyryl bromide with MPEG in the presence of a triethyl amine base catalyst. The atom transfer radical polymerization of 2-diisopropylamino)ethyl methacrylate was performed in conjunction with an N,N,N',N",N"-pentamethyl-diethylenetriamine/copper bromide catalyst system, in DMF, at $70^{\circ}C$. The pH induced micellization/demicellization was studied using fluorescence, with a pyrene probe. Furthermore, the pH dependent micellization was confirmed using the microviscosity method, with a dipyme fluorescence probe. The pH dependant micelle size distribution was studied using dynamic light scattering. The characterization of the synthesized polymers was established using gel permeation chromatography and from the $^1H-nuclear$ magnetic resonance spectroscopy.

Studies on the Destructible Surfactants(1);Synthesis of Cleavable Surfactant with Dioxolane Ring (분해성계면활성제에 관한 연구(제1보);1,3-Dioxlane고리를 갖는 분해성계면활성제의 합성)

  • Ha, J.W.;Jeong, N.H.;Kim, J.H.;Nam, K.D.
    • Journal of the Korean Applied Science and Technology
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    • v.12 no.1
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    • pp.93-99
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    • 1995
  • As the surfactants that were used in micellar reaction, emulsion polymerization and phase-transfer reaction etc. have the problems, the cleavable surfactant that was converted to inactive compound after such as the reaction was synthesized to above 90% yield. And this surfactant and intermediates were separated through thin layer chromatography and column chromatatography and their molecular structures were confirmed from IR. $^{1}H$-NMR and elementary analysis spectra. And its surface-active properties and acid hydrolysis will be serialized in II.

Determination of Recombinant Human Epidermal Growth factor (rhEGF) in a Pharmaceutical Preparation by Capillary Electrophoresis

  • Hwang, Kyung-Hwa;Lee, Kang-Woo;Kim, Chang-Soo;Han, Kun;Chung, Youn-Bok;Moon, Dong-Cheul
    • Archives of Pharmacal Research
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    • v.24 no.6
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    • pp.601-606
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    • 2001
  • A simple assay method of recombinant human epidermal growth factor (rhEGF) in a pharmaceutical preparation was studied and validated by capillary electrophoresis (CE) using micellar electrokinetic chromatography (MEKC) techniques. Factors affecting the migration behavior and separation performances of the peptide; type of buffers pH, butler concentration, and concentration of sodium dodecyl sulfates (SDS) were investigated to optimize the analytical performance. CE was performed using running buffers 50.0 mM borate (pH 8.5) containing 12.5 mM SDS at 20 $mutextrm{V}$ of the applied voltage. Calibration curves for the rhEGF showed good linearity (r>0.999) over the wide dynamic range from 1.25 to $100{\mu\textrm{g}}/ml$. Sample analysis was performed by using standard addition method to eliminate the matrix effects of dosage vehicle. This method is assumed to be useful for quality control (QC) of various forms of pharmaceutical products of the peptide.

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Solubilization of Mixture of Hydrocarbon Oils by C12E8 Nonionic Surfactant Solution (C12E8 비이온 계면활성제 수용액에 의한 탄화수소 오일 혼합물의 가용화 특성에 관한 연구)

  • Lim, JongChoo
    • Applied Chemistry for Engineering
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    • v.19 no.1
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    • pp.59-65
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    • 2008
  • The equilibrium solubilization capacity of the mixture of hydrocarbon oils by $C_{12}E_8$ nonionic surfactant micellar solution was measured at $23^{\circ}C$ by gas chromatography (GC) analysis. Experimental results indicated that the solubilization capacity for pure alkanes was found to decrease almost linearly with the alkane carbon number (ACN) of the hydrocarbon oil. For the binary mixture systems of the hydrocarbon oils both selective and nonselective solubilization behaviors were observed depending on the difference in ACN of the two hydrocarbon oils. Equilibrium solubilization tests for the hydrocarbon oil mixtures in $C_{12}E_8$ surfactant solutions such as the three n-octane/n-nonane, n-nonane/n-decane and n-decane/n-undecane mixture systems suggest almost non-selective solubilization. On the other hand, the n-octane/n-decane and n-octane/n-undecane systems, where difference in ACN of the two hydrocarbon oils is greater than 1, selective solubilization in favor of n-octane was conclusively demonstrated.

Preparation and Characterization of Cy5.5-conjugated Biocompatible Polymeric Micellar Nanoparticles for Optical Imaging (광학 영상을 위한 Cy5.5가 결합된 생체적합성 고분자 마이셀 나노입자의 제조 및 특성분석)

  • Kim, Hyo-Jeong;Kim, Byung-Jin;Lee, Ha-Yeong;Jung, Suk Hyun;Jeong, Seo-Young;Yuk, Soon-Hong;Shin, Byung-Cheo;Seong, Ha-Soo;Choi, Youn-Woong;Ha, Dae-Chul;Choi, Sun-Hang;Lee, Soo-Min
    • Journal of Pharmaceutical Investigation
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    • v.39 no.6
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    • pp.393-400
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    • 2009
  • PHEA (hydroxyethyl-aspartamide)-mPEG (methoy-polyethyleneglycol)-$C_{16}$ (hexadecylamine)-ED (ethylenediamine) was prepared as a drug delivery carrier. The structure and molecular weight of polymers were characterized by $^1H$-NMR and gel permeation chromatography. Micelle size and shape were measured by electro-photometer light scattering and transmission electron microscope. The mean diameter of micelles was 23 nm in aqueous solution. To evaluate the potential of these polymeric micelles as a drug carrier, PSI-mPEG-$C_{16}$-ED was conjugated with Cy5.5 for Near-Infrared Fluorescent (NIRF) based optical imaging. PSI-mPEG-$C_{16}$-ED-Cy5.5 was injected intravenously into mice (n=5) and in vivo NIRF imaging was performed during 48 h after injection. The biodistribution study at 24 h after injection showed the longcirculation property of PSI-mPEG-$C_{16}$-ED-Cy5.5. Therefore, PSI-mPEG-$C_{16}$-ED micelles could be a promising drug carrier and imaging agent.