• Title/Summary/Keyword: Analytical Chromatography

Search Result 1,121, Processing Time 0.029 seconds

Simultaneous Analysis of Bioactive Metabolites from Lonicera japonica Flower Buds by HPLC-DAD-MS/MS (HPLC-DAD-MS/MS를 이용한 금은화 생리활성 물질의 동시분석)

  • Ryu, Sung-Kwang;Jeon, Ju-Eun;Kang, Gyoung-Won;Kang, Sam-Sik;Shin, Jong-Heon
    • YAKHAK HOEJI
    • /
    • v.52 no.6
    • /
    • pp.446-451
    • /
    • 2008
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of chlorogenic acid (1), sweroside (2), luteolin-7-O-glucoside (3), (E)-aldosecologanin (4) and 3,5-dicaffeoylquinic acid (5) from Lonicera joponica flower buds. The optimal chromatographic conditions were obtained on an ODS column (5 ${\mu}m$, 4.6${\times}$150 mm) with the column temperature $25^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) acetonitrile with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 250 nm. All calibration curves showed good linear regression ($r^2$>0.994) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.05${\sim}$1.95% and 0.15${\sim}$2.26%, respectively, and the overall recoveries of 97.71${\sim}$103.65% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the three types (phenolic compounds, iridoids and flavonoids) of bioactive compounds in 21 commercial L. japonica flower buds samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.

The Identification of Type II DNA Topoisomerase-Associated Protein Kinase Activity from Regenerating Rat Liver (재생 쥐간에서 분리한 DNA topoisomerase II에 결합된 protein kinase 활성)

  • 이치건;박세호;남궁록;김찬길;박상대
    • The Korean Journal of Zoology
    • /
    • v.36 no.3
    • /
    • pp.367-372
    • /
    • 1993
  • We have found a protein kinase activity that is tightly associated with type II DNA topoisomerase purified from regenerating rat liver. The activities of protein kinase and topoisomerase II were not separable when the enzyme was subjected to analytical chromatographies (Hydroxyapatite, phosphocellulose, and double strand DNA cellulose) and glycerol gradient sedimentation. The kinase activity from purified rat topoisomerase II was also inactivated by the topoisomerase II inhibitors such as N-ethylmaleimide or novobiocin. The evidences, however, do not rule out a possibility that the kinase activity resides in a polypeptide other than the topoisomerase II protein. The topoisomerase II-associated protein kinase required Mg++ for its activity, and this requirement was not substituted by any other mono- or divalent ions. Histone H1 act as a strong stimulator and a good substrate for the kinase activity and other histones and ${\alpha}$-casein could not substitute the effect of histone H1.

  • PDF

Quantitative Analysis of Citrate in Foods Using a Potentiometric Enzyme Biosensor (전위차법 효소 바이오센서를 이용한 식품의 구연산 정량분석)

  • Kwon, Ji-Young;Kim, Mee-Ra
    • Korean Journal of Food Science and Technology
    • /
    • v.38 no.2
    • /
    • pp.169-175
    • /
    • 2006
  • Potentiometric biosensor using flow injection analysis system was developed to determine citrate concentration in foods. Biosensor system consisted of sample injector, peristaltic pump, enzyme reactor, carbonate ion selective solid-state electrode, reference electrode, detector, and recorder. Enzyme reactor was prepared with immobilized citrate lyase and oxaloacetate decarboxylase. Carbonate ions produced through enzyme reactions of citrate were potentiometrically detected by ion selective electrode. Optimum conditions for biosensor system were investigated. Interference effect of major sugars and organic acids was less than 5% on citrate biosensor system. Citrate concentrations in fruit juices were determined by biosensor and gas chromatography. No significant difference was observed between two analytical methods. Results indicate citrate biosensor is useful in determining citrate concentration in foods.

Analytical Method of L-Ascorbic Acid Content in Green Tea (녹차중(綠茶中)의 L-Ascorbic Acid의 정량법(定量法)에 관한 연구(硏究))

  • Shin, Mee-Gyung;Nam, Chang-Woo
    • Korean Journal of Food Science and Technology
    • /
    • v.11 no.2
    • /
    • pp.77-80
    • /
    • 1979
  • Effects of interfering substances on the determination of L-ascorbic acid (AsA) in green tea and it's extracts by 2,4-dinitrophenylhydrazine (DNP) method was studied. and the removal of these interfering substances was also investigated. Under the condition prescribed for DNP method, AsA content of green tea are effected by some sugar, reductones, dicarbonyl compounds, organic acids, amino acids and others. All interfering substances except amino acids were eliminated by the chloroform extraction after adding o-phenylendiamine to sample solution. and remaining amino acids were eliminated almost completely by the treatment with ion exchange resin$(Amberlite{\;}IR-120H^{+})$. After removing the interfering substances by the above mentioned procedure, total AsA in green tea was determined by DNP method. The values obtained by this method were in good agreement with those by thin layer chromatography (TLC) method. and the method was more rapid and simple than TLC method.

  • PDF

Application of On-Line SPE-LC/MSD to Measure Perfluorinated Compounds (PFCs) in Water (On-Line SPE-LC/MSD 시스템을 이용한 수중의 과불화 화합물(PFCs) 분석)

  • Son, Hee-Jong;Yoom, Hoon-Sik;Jung, Jong-Moon;Jang, Seung-Ho
    • Journal of Korean Society of Environmental Engineers
    • /
    • v.35 no.2
    • /
    • pp.75-83
    • /
    • 2013
  • We applied a sensitive method based on on-line solid-phase extraction (SPE) and liquid chromatography/mass spectrometry (LC/MSD) using an electrospray interface for the determination of eleven perfluorinated compounds (PFCs) in water. The on-line connection suppressed the target loss by keeping the cartridge from drying, which resulted in improvement of the recovery and saving of the analytical time. For the on-line solid-phase extraction of 10 mL water samples, recoveries were between $80.4{\pm}5.2%{\sim}109.5{\pm}1.4%$ and limit of quantification (LOQ) were 3.6~15.9 ng/L for the PFCs. The total PFCs concentrations of the tributaries and main stream of Nakdong River water samples were in the range of $8.0{\sim}678.6{\mu}g/L$.

Distribution of organophosphorus pesticides in Asan and Kyeonggi Bay, Korea (아산만과 경기만의 유기인계 잔류농약 분포)

  • Yu Jun;Yang Dong Beom;Kim Kyung Tae;Lee Kwang Woo
    • Journal of the Korean Society for Marine Environment & Energy
    • /
    • v.5 no.1
    • /
    • pp.38-50
    • /
    • 2002
  • To study the distribution of organophosphorus pesticides which are extensively used for agriculture in Korea. Surface sea water samples were taken from 2 coastal areas during July and :;eptember of 1999 and sediment samples were collected from Kyeonggi bay in July of 1999. These samples were analyzed using a Gas Chromatography/Nitrogen Phosphorus Detector(GC/NPD). In coastal waters of the study areas IBP was commonly found the most compound. Traces of Diazinon, DDVP, Ethoprouhos and Chlorpyrifos were also encountered. Concentration of the other major organophosphorus pesticides(Disulfoton, Parathion Methyl, Fenchlorfos, Prothiofos, EDDP) were generally be below the detection limit of the employed analytical method. Tn sediment of the study areas Chlorpyrifos w3s found the most compound. Temporal and geographical distribution of individual organophosphorus pesticides is likely to be affected by types of agricultural practices in the watershed.

  • PDF

Residue Analysis of Quinclorac in Soil by Supercritical Fluid Extraction and Fluorogenic Derivatization Coupled with High Performance Liquid Chromatography (초임계추출과 형광유도체를 이용한 HPLC 에서의 Quinclorac 의 토양중 잔류분석)

  • Kim, Yong-Whan
    • Applied Biological Chemistry
    • /
    • v.40 no.5
    • /
    • pp.442-446
    • /
    • 1997
  • A new analytical method was developed by HPLC after supercritical fluid extraction and fluorogenic derivatization for the determination of quinclorac (3,7-dichloro-8-quinoline carboxylic acid) in soil. The graminicide quinclorac was extracted from soil by supercritical fluid extraction. Supercritical carbon dioxide at 7000 psi $(80^{\circ}C)$ modified with 30% of methanol extracted quinclorac from soil samples at the level of $0.1ng\;g^{-1}$ with 96% recovery. Extracted quinclorac was determined by HPLC as a fluorescent derivative. Derivatization was made with 4-bromomethyl-7-methoxycoumarin (4-Br-Mmc) using 18-crown-6-ether as a catalyst. The conversion was completed within 30 min and the limit of detection was 0.5 ppb to prove that the procedure could be used in the residue analysis of the pesticides containing carboxylic acid group.

  • PDF

Effect of Arrowroot Flower (Puerariae flos) Extract on Lowering of Ethanol Concentration in Rat Blood (갈화(Puerariae flos)추출물이 Rat 혈중 Ethanol 농도에 미치는 영향)

  • Kim, Jeong-Han;Min, Sun-Sik;Kim, Sung-Hoon;Hong, Heu-Do;Kim, Jong-Soo;Kim, Soo-Un
    • Applied Biological Chemistry
    • /
    • v.38 no.6
    • /
    • pp.549-553
    • /
    • 1995
  • Ethanol concentration in blood, brain and liver of rats was shown to be effectively lowered by arrowroot flower extract. The lowering effect for ethanol concentration in blood was maximum when measured after 1 hour from ethanol feeding. Hot water extract was more effective than 80% ethanol extract. The treatment of extract at 10 min. before ethanol feeding gave a better result than that at 10 min after or 1 hour before ethanol feeding. The ethanol concentration in brain and liver was lowered as found in the blood ethanol concentration. Acetaldehyde was not detected either in blood or the tissues. The optimal amount of the Puerariae flos was 55.7 mg/kg body weight. The newly developed analytical method using dichloromethane as extracting solvent was proven to be very effective in terms of speed and simplicity.

  • PDF

Quantitative Analysis of Anthraquinones in Cassiae Semen by Processing Method (수치에 따른 결명자 주요 Anthraquinone의 함량분석)

  • Seo, Chang-Seob;Kim, Jung-Hoon;Shin, Hyeun-Kyoo;Hwang, Seock-Yeon;Kim, Byoung-Soo
    • Korean Journal of Pharmacognosy
    • /
    • v.45 no.3
    • /
    • pp.200-208
    • /
    • 2014
  • In this study, we performed quantification determination of four major components including aurantio-obtusin, emodin, chrysophanol, and physcion in the 70% ethanol extracts of non-processed Cassiae Semen and processed Cassiae Semen using a high-performance liquid chromatography coupled with photodiode array detector. The analytical column for separation of the 4 constituents used a Gemini $C_{18}$ column kept at $40^{\circ}C$ by the gradient elution with 1.0% (v/v) acetic acid in water and 1.0% (v/v) acetic acid in acetonitrile as mobile phase. The flow rate was 1.0 mL/min and the injection volume was $10{\mu}L$. The amount of aurantio-obtusin, emodin, chrysophanol, and physcion in non-processed Cassiae Semen were 0.07%, 0.02%, 0.25%, and 0.10%, respectively. The amount of aurantio-obtusin, emodin, chrysophanol, and physcion in processed Cassiae Semen were 0.04-0.14%, 0.01-0.03%, 0.02-0.42%, and 0.01-0.24%, respectively. Consequently, the optimal processing condition of Cassiae Semen for the improvements of amounts of four anthraquinone compounds was obtained by roasting at $240^{\circ}C$ for 15 min.

Simultaneous Analysis of Bioactive Metabolites from Rehmannia glutinosa by HPLC-DAD-MS/MS

  • Won, Tae-Hyung;Ryu, Sung-Kwang;Kang, Sam-Sik;Shin, Jong-Heon
    • Natural Product Sciences
    • /
    • v.16 no.2
    • /
    • pp.116-122
    • /
    • 2010
  • A high-performance liquid chromatography (HPLC) with diode array detector (DAD) and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of five representative metabolites of the iridoid and phenolic classes from Rehmannia glutinosa. The optimal chromatographic conditions were obtained on an ODS column (5 mm, $4.6{\times}250\;mm$) with the column temperature at $25^{\circ}C$. The mobile phase was composed of water and acetonitrile using a gradient elution with the flow rate 0.3 mL/min. Detection wavelength was set at 205 nm. All calibration curves showed good linear regression ($r^2$ > 0.997) within test ranges. Limits of detection (LOD) and quantitation (LOQ) values were lower than 0.123 and $0.373\;{\mu}g/mL$, respectively. The developed method provided satisfactory precision and accuracy with overall intra-day and inter-day variations of 0.09 - 0.76% and 0.16 - 1.41%, respectively, and the overall recoveries of 99.03 - 102.67% for all of the compounds analyzed. In addition, effectiveness of diverse extraction methods was compared to each other for the development of standard analytic method. The verified method was successfully applied to the quantitative determination of five representative metabolites in twenty-one commercial Rehmannia glutinosa samples from different markets in Korea and China. The analytical results showed that the contents of the five analytes vary significantly with sources.