• Title/Summary/Keyword: High performance Liquid Chromatography

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Identification and Growth Inhibition of Phytotoxic Substances from Tomato Plant (토마토식물의 독성물질 확인과 생장억제작용)

  • 김영식
    • Journal of Plant Biology
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    • v.32 no.1
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    • pp.41-49
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    • 1989
  • Phenolic compounds such as gallic acid, ferulic acid, p-hydroxybenzoic acid, vanillic acid, salicylic acid, tannic acid, and hydroquinone were identified from the aqueous extracts and volatile substances of tomato plant by paper chromatography, high performance liquid chromatography and gas chromatography. The seed germination and seedling growth of the experimental species, lettuce and egg plant, were severely inhibited in 5$\times$10-3M of phenolic reagents identical to those identified from tomato plant. Germination and growth rate of test species in 5$\times$10-4M and 5$\times$10-5M were higher than that of 5$\times$10-3M. Therefore, 5$\times$10-3M of phenolic compounds would be assumed to be threshold concentration for allelopathic effects.

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Isolation and Identification of Free Phenolic Acids in Korean Ginseng (인삼의 유리 페놀성 분획중 phenolic acid의 순수분리 동정)

  • Kim, Man-Wook;Wee, Jae-Joon;Park, Jong-Dae
    • Korean Journal of Food Science and Technology
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    • v.19 no.5
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    • pp.392-396
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    • 1987
  • A method for isolation of some phenolic acids from Korean ginseng(Panax ginseng C.A.Meyer)was studied using silicic acid column chromatography. preparative thin layer chromatography and high performance liquid chromatography. Two phenolic compounds were isolated and identified as ferulic acid, mp $156-157^{\circ}C$ and vanillic acid. mp $154-156^{\circ}C$ by spectral data of Mass and NMR spectroscopy.

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Studies on the Anthocyanin Pigments in Fruits of Panax Species - Part I. Identfication of major Pigment - (Panax속(屬)의 과피(果皮) Anthocyanin 색소(色素) - 제1보(第一報). 주색소(主色素)의 동정(同定) -)

  • Parklee, Qwi-Hee;Park, Hoon
    • Applied Biological Chemistry
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    • v.23 no.4
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    • pp.242-245
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    • 1980
  • The anthocyanin pigments in the fruit skin of Panax ginseng and Panax quinquefolius were extracted with 1% HCl/propanol. The pigments were purified by preparative thin layer and paper chromatography. The major bands in the 2 varieties were identified as pelragonidin-3-monoglucoside by chromatographic, spectrophotometric and high performance liquid chromatographic methods. The possibility of the anthocyanin acylation was not studied in this report. One of minor red band found in the Panax ginseng (not identified) was missing in the Panax quinquefolius.

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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.

Depolymerization of PET by Ethylene Glycol (에틸렌글리콜을 이용한 PET 해중합 특성)

  • Hwang, Hwidong;Kim, Bokyung;Woo, Daesik;Han, Myungwan
    • Korean Chemical Engineering Research
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    • v.47 no.6
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    • pp.683-687
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    • 2009
  • A method for depolymerization of PET by catalyzed glycolysis with an excess ethylene glycol(EG) to recover bis-hydroxyethyl terephthalate(BHET) was investigated. The product was analyzed by high-performance liquid chromatography(HPLC). Effects of operation variables such as reaction temperature, reaction time, EG/PET weight ratio were examined and kinetics of the glycolysis was studied. High temperature increases the rate of depolymerization and the yield of BHET. But, repolymerization rate was also high at too high temperature and the yield at $250^{\circ}C$ was shown to be lower than that at $230^{\circ}C$. First order reaction model was proposed to describe the glycolysis reaction. Activation energies for the reaction were obtained to be 37.8 kJ/mol above $210^{\circ}C$ and 149.6 kJ/mol below $210^{\circ}C$, which shows the glycolysis reaction is a multiple reaction. A maximum yield of BHET of 71% was achieved at a reaction temperature of $230^{\circ}C$ for 6 hr with an EG/PET weight ratio 4.

Chiral Purity Test of Bevantolol by Capillaryelectrophoresis and High Performance Liquid Chromatography

  • Long, Pham Hai;Trung, Tran Quoc;Oh, Joung-Won;Kim, Kyeong-Ho
    • Archives of Pharmacal Research
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    • v.29 no.9
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    • pp.808-813
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    • 2006
  • Two methods for the chiral purity determination of bevantolol were developed, namely capillary electrophoresis (CE) using carboxymethyl-${\beta}$-cyclodextrin (CM-${\beta}$-CD) as a chiral selector and high-perfomance liquid chromatography (HPLC) using a chiral stationary phase. In the HPLC method, the separation of bevantolol enantiomers was performed on a Chiralpak AD-H column by isocratic elution with n-hexane-ethanol-diethylamine (10:90:0.1, v/v/v) as mobile phase. In the CE method, bevantolol enantiomers were separated on an uncoated fused silica capillary with 50 mM amonium phosphate dibasic adjusted to a pH 6.5 with phosphoric acid containing 15 mM CM-${\beta}$-CD as running buffer. Validation data such as linearity, recovery, detection limit, and precision of the two methods are presented. The detection limits of S-(-)-bevantolol were 0.1% and 0.05% for CE and HPLC method, respectively and R-(+)-bevantolol were 0.15% and 0.05% for CE and HPLC method, respectively. There was generally good agreement between the HPLC and CE results.

Characterization of phenolic compounds biosynthesized in pink-colored skin of Japanese indigenous Vitis vinifera cv. Koshu grape

  • Kobayashi, Hironori;Suzuki, Yumiko;Ajimura, Kosei;Konno, Tomonori;Suzuki, Shunji;Saito, Hiroshi
    • Plant Biotechnology Reports
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    • v.5 no.1
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    • pp.79-88
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    • 2011
  • Vitis vinifera cv. Koshu is a traditional grape cultivar that has been grown for centuries in Japan. The Koshu grape has pink-colored skin and Koshu wines have slight astringency. We demonstrated for the first time the characterization of hydroxycinnamic acids, flavan-3-ols, and flavonoids in Koshu grape using high-performance liquid chromatography and liquid chromatography-mass spectrometry. The gross weight of phenolic compounds excluding anthocyanins and proanthocyanidins in Koshu grape at harvest was higher than those in Sauvignon Blanc, Chardonnay, and Merlot grapes. In addition, hydroxycinnamic acid and monomeric flavonol contents in Koshu grape were also higher than those in the other grape cultivars. Transcription analysis of cinnamic acid 4-hydroxylase, p-coumarate 3-hydroxylase, caffeate methyltransferase, and flavonol synthase genes indicated high accumulation of hydroxycinnamic acids and flavonols in Koshu grape skin compared with the other cultivars. These findings obtained by chemical and molecular approaches partially explained the phenolic characteristics and the peculiar astringency of Koshu grape.

1H-NMR and HPLC analysis on the chiral discrimination of β-blockers using (S)-2-tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid

  • Seo, Sang Hun;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.34 no.1
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    • pp.9-16
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    • 2021
  • In the group of commonly prescribed β-blocker drugs, one of the enantiomers is generally relatively more active than the others. This study aims to develop a technique for the chiral analysis of select β-blockers based on proton nuclear magnetic resonance (1H-NMR) spectrometry. (S)-2-Tert-butyl-2-methyl-1,3-benzodioxole-4-carboxylic acid ((S)-TBMB) was synthesized and utilized as a chiral derivatizing agent. Pure β-blocker enantiomers were isolated from racemates by semi-preparative liquid chromatography prior to derivatization. The reaction time and concentration of (S)-TBMB were controlled to improve the derivatization procedure. No racemization was found during the analysis. High-performance liquid chromatography (HPLC) analysis was also performed for comparative purposes. High agreement between the NMR and HPLC methods was achieved in the determination of (R)-metoprolol in a standard solution of the (S) isomer.

Development and Validation of a Unique HPLC-ELSD Method for Analysis of 1-Deoxynojirimycin Derived from Silkworms (누에에 함유된 1-Deoxynojirimycin의 분석을 위한 HPLC-ELSD 분석법 밸리데이션)

  • Hyejin Cho;Sullim Lee;Myoung-Sook Shin;Joohwan Lee;Sanghyun Lee
    • Korean Journal of Pharmacognosy
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    • v.54 no.1
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    • pp.38-43
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    • 2023
  • A simple and accurate assay was developed for the quantitative analysis of 1-deoxynojirimycin (1-DNJ) derived from the silkworm (Bombyx mori). Normal-phase high-performance liquid chromatography coupled with an evaporative light scattering detector (HPLC-ELSD) and a hydrophilic interaction liquid chromatography column was used. Various parameters were applied to optimize the analysis method. The limits of detection and quantification of 1-DNJ were 2.97 × 10-3 and 9.00 × 10-3 mg/mL, respectively. The calibration curve showed good linearity results. The concentration range and the r2 value were 0.0625-1.0 mg/mL and 0.9997, respectively. The accuracy test demonstrated a significantly high recovery rate (89.95-103.22%). The relative standard deviation was ≤ 1.00%. Thus, a method for the accurate identification and quantitative analysis of 1-DNJ in silkworms was developed. Moreover, in this procedure, the process of derivatization of 1-DNJ, which was required in previous experiments, could be eliminated. This technique may be actively utilized for the development of pharmaceuticals and health functional foods using 1-DNJ.

Reducing the LC Column's Internal Diameter to Drive Sustainable Chromatography (LC 컬럼의 내경을 줄여 분석 효율을 높이고 환경 친화적인 크로마토그래피를 수행하는 방법)

  • Matt James;Arianne Soliven;Tony Edge
    • FOCUS: LIFE SCIENCE
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    • no.1
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    • pp.11.1-11.7
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    • 2024
  • The white paper provides detailed guidance on optimizing chromatographic separations with Avantor ACE® columns. It emphasizes key factors for improving method development in HPLC, including the selection of stationary phases, understanding particle size effects, and adjusting operating parameters like flow rate and temperature to maximize resolution and efficiency. The document addresses challenges in method scalability and transfer, offering practical solutions for translating methods between instruments with differing column dimensions or flow rates. It includes mathematical equations and examples to ensure accurate method adjustments during translation. Additionally, the paper underscores the importance of selecting appropriate mobile phase compositions to minimize retention time variability and maximize peak sharpness. With a focus on achieving reproducibility and robustness in separations, this resource is tailored for chromatographers aiming to streamline complex analytical workflows while maintaining high performance across diverse applications.

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