• Title/Summary/Keyword: HPLC-analysis

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Development of Analytical Methods for Micro Levels of Naphthalene and TNT in Groundwater by HPLC-FLD and MSD (HPLC-FLD와 MSD를 이용한 지하수 중 나프탈렌 및 TNT의 미량 분석법 개발)

  • Park, Jong-Sung;Oh, Je-Ill;Jeong, Sang-Jo;Choi, Yoon-Dae;Her, Nam-Guk
    • Journal of Soil and Groundwater Environment
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    • v.14 no.6
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    • pp.35-44
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    • 2009
  • Naphthalene and TNT (2,4,6-trinitrotoluene) are defined by U.S. EPA as possible carcinogenic compounds known to have detrimental effects on the aquatic ecosystem and human body. There are, however, few researches on methods of analyzing micro-levels of naphthalene and TNT dissolved in groundwater. This study introduces and evaluates the newly developed analytical methods of measuring naphthalene and TNT in groundwater by using HPLC-FLD (Fluorescence detector) and MSD (Mass detector). The MDL, LOQ and salt effect of these methods, respectively, are compared with those of conventional methods which use HPLC-UV. For the analysis of naphthalene, HPLC-FLD was set in the maxima wavelength (Ex: 270 nM, Em: 330 nM) obtained from 3D-Fluorescence to be compared with HPLC-UV in 266 nM wavelength. The MDL ($0.3\;{\mu}g/L$) and LOQ ($2.0\;{\mu}g/L$) of naphthalene by using HPLC-FLD were approximately 80 times lower than those analyzed by HPLC-UV (MDL: $23.3\;{\mu}g/L$, LOQ: $163.1\;{\mu}g/L$). HPLC-MSD were used in comparison with HPLC-UV in 230 and 254 nM wavelength for the analysis of TNT. The MDL ($0.13\;{\mu}g/L$) and LOQ ($0.88\;{\mu}g/L$) of TNT analyzed by using HPLC-MSD were approximately 130 times lower than those obtained by using HPLC-UV in 230 nM (MDL: $16.8\;{\mu}g/L$, LOQ: $117.5\;{\mu}g/L$). The chromatogram of TNT analyzed by using HPLC-UV in 230 nM displayed elevated baseline as the concentration of ${NO_3}^-$ increases beyond 21 mg/L, while the analysis using HPLC-MSD did not demonstrate any change in baseline in presence of ${NO_3}^-$ of 63.7 mg/L which is 3.5 times higher than average concentration in groundwater. In conclusion, HPLC-FLD and HPLC-MSD may be used as suitable methods for the analysis of naphthalene and TNT in groundwater and drinking water. These methods can be applied to the monitoring of naphthalene and TNT concentration in groundwater or drinking water.

Comparative Analysis of Fritillaria Species by HPLC (Fritillaria속 식물의 HPLC에 의한 비교분석)

  • Kwon, Yong-Soo;Hong, Sung-Sook;Kim, Chang-Min
    • Korean Journal of Pharmacognosy
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    • v.32 no.4 s.127
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    • pp.307-310
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    • 2001
  • In order to investigate alkaloid contents in different Fritillaria species, we analyzed 17 Fritillaria species by HPLC using prederivatization method. The contents of alkaloid $fr.5(11-deoxo-6-oxo-5{\alpha},6-dihydrojervine)$, delavinone and delavine were analyzed and compared.

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Microanalysis of Pancuronium Bromide in Urine and Blood by HPLC (HPLC를 이용한 뇨 및 혈액중의 Pancuronium Bromide의 미량분석)

  • 김박광;김양숙;박성배;이종숙;정규혁;김경님
    • YAKHAK HOEJI
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    • v.37 no.1
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    • pp.30-35
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    • 1993
  • HPLC/fluorescence detection method for the analysis of pancuronium bromide in biological fluids was developed. The method depends on the formation of insoluble red complex between pancuronium bromide and rose bengal in aqueous layer. This complex is quantitatively extracted from aqueous layer into chloroform layer. The complex is stable for 1 day in chloroform layer at room temperature. It was possible to analyze pancuronium bromide in the range of 0.05~0.5 $\mu\textrm{g}$/ml without the effect of co-prescribed drugs.

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Application of Competitive ELISA Method for Estimation of Urinary Aflatoxin M1 Level (ELISA 방법을 이용한 요중 아플라톡신 M1 측정)

  • Kim, Yong-Dae;Kim, Heon
    • Journal of Life Science
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    • v.23 no.2
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    • pp.306-310
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    • 2013
  • We compared the efficacy of the competitive ELISA method for measuring the level of urinary aflatoxin M1 (AFM1) with that of the HPLC-fluorescence detector (HPLC-FLD) method. The recovery rate of AFM1 with the ELISA method was 105% (73-124%), and the coefficient of variation of the analysis was 6.85%. The ELISA method showed a 0.20 pg/ml and 0.62 pg/ml limit of detection and limit of quantitation, respectively. In correlation analysis, the two methods showed a very strong and statistically significant correlation (R=0.96, p<0.01). However, in spite of the strong correlation, the ELISA method tended to overestimate the urinary AFM1 concentration compared to the HPLC-FLD method. These results suggest that the competitive ELISA method may be a useful technique for measuring the AFM1 level in high-throughput urine samples, but it needs to be corrected with a regression equation from regression analysis with the HPLC-FLD method.

Determination of residual flumethrin in honey products by HPLC (HPLC를 이용한 벌꿀 중 플루메쓰린 분석)

  • Won, So-Young;Jeong, Young-Ji;Lee, Hwee-Jae;Chang, Hye-Sook;Bahn, Kyeong-Nyeo;Kang, Ho-Il;Kim, So-Hee
    • Analytical Science and Technology
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    • v.22 no.6
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    • pp.458-463
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    • 2009
  • A new quantitative analytical method has been established for the rapid determination of flumethrin in honey products using high performance liquid chromatography (HPLC). Sample was dissolved and extracted in the mixture of water and acetonitrile (1:2). The extracts were purified with silica cartridge eluted by the mixture of hexane and dichloromethane (55:45) and analyzed at 266 nm using HPLC. The percentage recovery of flumethrin spiked in sample was found to be 90.2-97.8% and the limit of detection is 0.003 mg/kg. We validated the method for the linearity, the precision and the reproducibility. We investigated the residues of flumethrin in honey products retailed in market using the established method. Flumethrin was not detected at all among 130 samples of honey.

Absence of Tocotrienol Form of Vitamin E in Purple Perilla (Perilla frutescens var. acuta Kudo) Seeds Confirmed by Comparative Analysis Using HPLC and GC (GC 및 HPLC 비교분석에 기초한 차조기 종실내 tocotrienol 부재의 평가)

  • Lee, Young-Sang;Kim, Min-Kyoung
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.53 no.spc
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    • pp.115-120
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    • 2008
  • Lipid soluble vitamin E consists of tocopherols and tocotrienols depending upon double bonds in phytyl side chains attached to chromanol ring. Recent reports on antioxidative, anticancer, and cholesterol-lowering effects of tocotrienols have increased researches and commercialization of tocotrienols. Purple perilla (Perilla frutescens var. acuta Kudo) has been reported as a plant containing tocotrienols along with tocopherol forms of vitamin E based upon normal phase HPLC analysis. To confirm the existence or absence of tocotrienol form of vitamin E in purple perilla, comparative analysis using HPLC, GC/FID, and GC/MSD has been conducted for 14 purple perilla genetic accessions collected from Korea and Japan. Normal phase HPLC analysis showed ${\alpha}-$, ${\beta}-$, ${\gamma}-$, and ${\delta}-tocopherols$ along with peaks with retention times quite similar to ${\beta}-$ and ${\gamma}-tocotrienols$. Same purple perilla samples, analysed by GC exhibited ${\alpha}-$, ${\beta}-$, ${\gamma}-$, and ${\delta}-tocopherols$ quantitatively equivalent to HPLC results. However, no peaks for ${\beta}-$ and ${\gamma}-tocotrienols$ could be observed and unknown two peaks of similar retention times with ${\beta}-$ and ${\gamma}-tocotrienols$ were identified not corresponding tocotrienols by GC/MSD. These results suggest the absence of tocotrienol form of vitamin E in purple perilla as well as the necessity of using GC-based qualitative and quantitative vitamin E analysis to avoid misinterpretation of peaks with similar retention times as tocotrienol isomers when analysed by an HPLC.

Quantitative Analysis of Acanthopanacis Cortex and Achyranthis Radix for Standardization of GCSB-5 Preparation (생약복합제 GCSB-5의 품질 표준화를 위한 오가피 및 우슬의 함량 분석)

  • Lee, Eun-Hee;Cha, Bae-Cheon
    • Korean Journal of Pharmacognosy
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    • v.39 no.4
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    • pp.316-323
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    • 2008
  • In this study, we have investigated the HPLC analysis methods and quantitative analysis of standard compounds for quality standardization of a medicinal crude drug GCSB-5, a herbal formulation consisting of 6 medicinal plants (Acanthopanacis Cortex, Achyranthis Radix, Ledebouriellae Radix, Cibotii Rhizoma, Glycine Semen, Eucommiae Cortex) which are used in traditional medicine to treat various bone disorders. HPLC analysis methods of acanthoside D(Acanthopanacis Cortex), 20-hydroxyecdysone(Achyranthis Radix) which were known standard compounds among 6 medicinal plants were developed on crude material and product. And validation of HPLC analysis methods were conformed for verification of HPLC methods by check to specificity, linearity, intra-day precision, inter-day precision and accuracy following ICH guideline. Content of acanthoside D and 20-hydroxyecdysone on raw material of GCSB-5 were decided at 0.577-0.578 mg/g and 0.311-0.312 mg/g. And we confirmed that content of acanthoside D and 20-hydroxyecdysone on GCSB-5 preparation were 0.302-0.303 mg/capsule and 0.113-0.115 mg/capsule.

Recent Developments in High-performance Liquid Chromatography of Lipids

  • Christie, William W.
    • Journal of the Korean Applied Science and Technology
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    • v.10 no.1
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    • pp.1-8
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    • 1993
  • The possibilities for HPLC analysis of lipids have been revolutionised by the availability of evaporative light-scattering detectors, with which the response is independent of the nature of the mobile phase and does not depend On the presence of specific chromophores in the lipids. It was thus possible to develop an HPLC procedure, involving ternary gradient elution, for separating all the lipid classes in animal tissues in a single step. Although reversed-phase HPLC has been widely used for the analysis of molecular species of lipids, sliver ion chromatography can be a valuable alternative. For example, a stable silver ion column for HPLC was developed which permitted resolution of molecular species of triacylglycerols, even from such complex samples as fish oils, again With light-scattering detection and gradient elution. The capacity for HPLC resolution of diastereomeric diacyl-sn-glycerol derivatives, prepared from triacylglycerols. has lead to a new simple method for stereospecific analysis of the latter.

Purification of 4-Methylthio-3-butenyl isothiocyanate the Pungent Principle in Radish Roots by RP-HPLC (RP-HPLC법에 의한 무우의 매운 성분인 4-methylthio-3-butenyl isothiocyanate의 분리 및 정제)

  • Kim, Mee-Ree;Rhee, Hei-Soo
    • Korean journal of food and cookery science
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    • v.2 no.2
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    • pp.16-20
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    • 1986
  • The major pungent component from Korean radish roots was purified by reverse phase high performance liquid chromatography (RPHPLC), and characterized as 4-methylthio-3-butenyl isothiocyanate on the basis of the sensory test (pungency), UV spectrum and mass spectrum analysis. The purified isothiocyanate moved as a single peak(retention time, 5.2 min) in RP-HPLC analysis, and as a single spot(Rf, 0.9) in TLC analysis.

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Quantitative Analysis of Lysophosphatidyl Choline (LPC) in Wheat Starch Lipids by High Performance Liquid Chromatography (고속액체크로마토그래피에 의한 밀전분 지방질에 함유된 리소레시친의 정량)

  • Shin, Myung Gon;Min, Bong Kee;Chang, Pahn Shick
    • Analytical Science and Technology
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    • v.5 no.3
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    • pp.339-343
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    • 1992
  • The content of lysophosphatidyl choline (LPC) in wheat starch lipids from six cultivar representing three classes of wheat was determined by a high performance liquid chromatography using UV-detection (HPLC-UV). The HPLC-UV assay had a sensitivity of LPC concentrations above $5{\mu}g/50{\mu}l$ and required 80 minutes per chromatogram.

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