• Title/Summary/Keyword: HPLC-UV

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Preconcentration and Detection of Herbicides in Water by Using the On-line SPE-HPLC System and Photochemical Reaction

  • 이승호;이성광;박영훈;김현주;이대운
    • Bulletin of the Korean Chemical Society
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    • v.20 no.10
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    • pp.1165-1171
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    • 1999
  • The analysis of trace herbicides using the on-line SPE-HPLC system and a photochemical reaction was studied. 18 compounds of herbicides including eight triazines, six phenoxy acids and esters, and four other herbicides were examined. The on-line SPE-HPLC system developed for selection of eluting solvent improved chromatographic efficiency. The recoveries of herbicides were higher than 77%. With 100 mL tap water samples, the detection limits for all analytes were in the 0.1-2.3×10-10 M range. Detection was done by a UV or fluorescence spectrometer after photochemical reaction at the end of the column with 2W or 450W mercury lamp. Without a photochemical reaction, all compounds responded to 230 nm UV detector, but phenoxy acids and esters were weakly detected. However, with a photochemical reaction, these compounds were selectively detected at 320 nm wavelength of UV absorption and 400 nm emission of the fluorescence detectors. This method can be used for the analysis of environmental water containing herbicides at trace levels.

Analysis of Microcystins(LR, YR and RR) in Water (Micro-HPLC/IS/MS에 의한 수 중의 Microcystins (LR, YR 및 RR)의 분석)

  • Park, Kwan Su;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.45 no.6
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    • pp.524-531
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    • 2001
  • Micro-HPLC/IS/MS after solid phase extraction has been employed to enhance the accu-racy in the determination of toxic microcystins, such as microcystin-LR, -YR and -RR. The absorbance at 238 nm in HPLC/UV and characteristic spectra of 135 m/z and $[M+H]^+$ m/z in MS have been widely monitored to identify those microcystin-LR, -YR and -RR. In this study, new lines at 507 m/z for LR, 520 m/z for RR and 532 m/z for YR have been additionally detected in the micro-HPLC/IS/MS spectrum, corresponding to double charge. The micro-HPLC/IS/MS methodology has been applied to investigate the presence of the toxic microcystins in Taecheong lake.

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Simultaneous determination of sunscreen agents in cosmetics by HPLC (HPLC를 이용한 화장품 중의 자외선 차단제 동시분석방법 연구)

  • Lee, Yong-Hwa;Yang, Jae-Chan
    • Journal of the Korean Applied Science and Technology
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    • v.29 no.4
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    • pp.577-584
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    • 2012
  • The simultaneous analysis of sun screen agents in commercial cosmetic samples was carried out by High Perfomance Liquid Chromatography(HPLC). The cosmetic samples are directly dissolved in Tetrahydrofurane(THF) and filtered using $0.45{\mu}m$ filter. The water/methanol/THF was used for the mobile phase of gradient conditions. An Extend C18 reversed-phase column and the selected UV/Visible detector was applied. The analysis results of HPLC showed good linearity with correlation coefficient of $r^2$=0.9992 in the rage of $50{\sim}800{\mu}g/mL$ and detection limit of $0.01{\mu}g/mL$.

A Study on Contents of Anti-impotence drug/drug-like compounds in Food (식품중 발기부전 치료제 및 유사물질 함량에 관한 조사연구)

  • Hong, Hae-Geun;Bang, Seon-Jae;Park, Kwang-Hee;Lee, In-Sook;Park, In-Jung;Park, Jeung-Hwa;Kim, Jong-Chan
    • Journal of environmental and Sanitary engineering
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    • v.22 no.3
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    • pp.89-96
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    • 2007
  • To determine 8 anti-impotence drug/drug-like compounds such as sildenafil, vardenafil, tadalafil, homosildenafil, hydroxyhomosildenafil, aminotadalafil, pseudovardenafil and hongdenafil in foods, simultaneously, high performance liquid chromatography(HPLC) and liquid chromatography-mass spectrometry (LC/MS) were used. The HPLC/UV analysis was performed on a column of capcellpak $C_{18}$ with 0.1% sodium-1-hexansulfonate in 0.2M ammonium formate/acetonitrile as a mobile phase. Mass spectra of the compounds by LC/MS were investigated with SCAN mode(Mass range and Fragment voltage) and SIM(Selected Ion Monitoring) mode (Ion target and Fragment voltage). The results follow as; 1. The HPLC/UV analysis was detected from 5 out of 63 samples. The content of sildenafil was in the range of 32.80 ppm ${\sim}$ 60.13 ppm from 4 out of 5 samples. The contents of sildenafil, vardenafil, homosildenafil were in the range 47.14 ppm from 1 out of 5 samples. 2. The conformed result of LC/MS was equal of detected from 5 out of 63 samples in HPLC/UV analysis. An easily available, simultaneous determination of 8 standards in adulterated health related foods was established by using a combination of LC/MS methods.

Quantitative Determination of Bakkenolide D in Petasites japonicus and Farfugium japonicum by HPLC/UV

  • Quilantang, Norman G.;Lee, Ki Ho;Lee, Dong Gu;Lee, Ju Sung;Cho, EunJu;Kim, Hyun Young;Lee, Sanghyun
    • Natural Product Sciences
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    • v.23 no.4
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    • pp.270-273
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    • 2017
  • A quantitative analysis of bakkenolide D in the different parts of Petasites japonicus and Farfugium japonicum was performed by HPLC. A gradient HPLC elution system with a mobile phase consisting of water: acetonitrile solution (20:80 to 0:100 for 45 min) was followed and an INNO $C_{18}$ column was used for the chromatographic separation. The injection volume, flow rate, and UV detection were $10{\mu}L$, 1 mL/min, and 290 nm, respectively. Results show that both species showed the highest amount of bakkenolide D in the roots being 107.203 and 166.103 mg/g for P. japonicas and F. japonicum, respectively. Content analysis on the different parts of both plants displayed remarkably lower values which ranged from 0.403 - 4.419 and 7.252 - 32.614 mg/g for P. japonicas and F. japonicum, respectively. The results show that the roots of both plants are rich in bakkenolide D showing a promising use in the development of nutraceuticals and industrial application of the compound.

Establishment of HPLC-UV Analysis Method Validation for Simultaneous Analysis of Standard Compounds of Oplopanax elatus Nakai Stem (HPLC-UV를 이용한 땃두릅나무 줄기의 지표 성분 동시 분석법 확립)

  • Yoo, Nam Ho;Kwon, Yongsoo;Kim, Myong Jo
    • Korean Journal of Pharmacognosy
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    • v.50 no.2
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    • pp.133-140
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    • 2019
  • In our previous study, we found uracil, adenosine, protocatechuic acid, syringin (eleutheroside B) and scoparone (6, 7-dimethoxycoumarin) in the Oplopanax elatus Nakai Stem. High-performance liquid chromatography (HPLC) -UV was used to quality and quantify the internal marker compounds in the O. elatus extract after validation of method with linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. The specificity assessment visually confirmed that the substance was detected without the introduction of other substances. The established method showed high linearity of the calibration curve and coefficient of correlation ($R^2$) of over the 0.999. HPLC was reported as five standard compounds equivalent using the following linear equation based on the calibration curve. The accuracy of measurement was 84.34 ~ 119.74% and the relative standard deviation (RSD) value was 0.28 ~ 1.60%. In addition, our established method showed high repeatability. The RSD value was 1.10 ~ 6.81%. So, we found the amount of the internal marker compounds in the O. elatus extract. These results demonstrated that can be used to quality evaluation of the O. elatus.

Simultaneous Analysis of Cholesterol Oxidation Products (COPs) in Powdered Milk Using HPLC/UV-Vis

  • Lee, Jin Joo;Myung, Seung-Woon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.9
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    • pp.2787-2794
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    • 2013
  • Cholesterol and cholesterol oxidation products (COPs) may accumulate in foods of animal origin during processing or storage. An effective and sensitive analytical method was developed by increasing the UV absorption of compounds through derivatization by attaching a chromophore to the functional groups of cholesterols (cholesterol, 20-hydroxycholesterol, 7-ketocholesterol, cholestane-$3{\beta}$-$5{\alpha}$-$6{\beta}$-triol, 25-hydroxycholesterol, and $5,6{\alpha}$-epoxycholesterol). The influences of the reaction time, volume of reaction solvent, amounts of derivatizing reagent, and extraction solvents were investigated, as they may influence the reaction and extraction yield. The derivatized COPs were analyzed simultaneously on a C18 column (2.1 mm i.d. ${\times}$ 100 mm length, $3.5{\mu}m$ particle size) using a gradient elution with water and acetonitrile. The derivatized COPs showed increased sensitivity and selectivity in HPLC/UV-Vis. The LOD and LOQ were in the concentration ranges of 0.018-0.55 mg/kg and 0.059-1.84 mg/kg from the powdered milk. And the accuracy and precision were 78.1-116.7% and 1.1-9.9%, respectively.

Content Analysis of Rutin in the Leaves of Boehmeria nivea Harvested in Different Regions of South Korea by HPLC-UV

  • Cho, Sunghun;Quilantang, Norman G.;Lee, Ju Sung;Kim, Young-Mi;Kim, Ho Bang;Cho, Eun Ju;Jung, Yong-Su;Lee, Sanghyun
    • Natural Product Sciences
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    • v.24 no.1
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    • pp.36-39
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    • 2018
  • Phytochemical analysis of Boehmeria nivea (Bn) leaves by medium pressure liquid chromatography led to the isolation of a flavonoid glycoside identified by spectroscopic analysis as rutin. The amount of rutin in the leaves of Bn harvested from nine regions in South Korea (Bn 1-9) which were collected on the months of June, July, August, and September was determined by HPLC-UV analysis. A gradient elution program that utilizes a $Discovery^{(R)}$ C18 ($4.6{\times}250mm$, $5{\mu}m$) column and mobile phase composed of 1% acetic acid-water: acetonitrile (90:10 to 60:40 for min) was followed. The injection volume and flow rate were $10{\mu}l$ and 1 mL/ min, respectively. UV detection was set at 350 nm. Results show that Bn-8 harvested in September reported the highest content of rutin among the samples analyzed. This study provides a basis for the optimal harvest time of Bn which maximizes the yield of rutin.

Development of Analytical Methods for Insect Moulting Hormone $({\beta}-Ecdysone)$ by HPLC/UV Using Boronate Derivatization

  • Shim, Jae-Han;Kim, In-Seon;Lim, Kye-Taek
    • Applied Biological Chemistry
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    • v.41 no.4
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    • pp.251-256
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    • 1998
  • The analytical method of ${\beta}-ecdysone$, the insect moulting hormone, by high performance liquid chromatograph (HPLC) with UV detector was developed using boronic ester derivatization and applied to the extracts of Ajuga iva, Silene otites and Schistocerca egg. Derivatization of yield with methyl-, butyl-, and phenyl-boronate was completed under mild conditions with 20-hydroxyecdysone. The conversion ratios of boronate were estimated to be 70% in methylboronic acid, 89% in butylboronic acid and 93% in phenylboronic acid. Phenylboronate showed a high sensitivity and demonstrated an effective separation on HPLC. The optimum temperature and reaction time for derivative formation were $25^{\circ}C$ and 20 min. respectively. ${\beta}-Ecdysone$ was effectively identified in extracts of Ajuga iva, Silene otites and Schistocerca egg by the HPLC method.

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Rapid Identification of the ${\alpha}$-Glucosidase Inhibitory Compounds from Geranium thunbergii Sieb. et Zucc. by HPLC-micro-fractionation and HPLC-UV-$MS^n$

  • Choi, Se-Jin;Kim, Jin-Kyu;Lee, Yeon-Sil;Lim, Soon-Sung
    • 한국약용작물학회:학술대회논문집
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    • 2010.10a
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    • pp.430-430
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    • 2010
  • In this study ethanol extracts of aerial part of Geranium thunbergii Sieb. et Zucc. was investigated for their ability to inhibit a-glucosidase, and thus was fractionated using two organic solvents, including dichloromethane, ethyl acetate. The ethyl acetate-soluble fraction, which manifested potent enzyme inhibitory properties, was then followed by tracking down the active compound by combining HPLC micro-fractionation to an enzyme assay in 96-well plate. The ${\alpha}$-glucosidase inhibitory activity profile showed that two peaks exhibited potent inhibitory activity, and then the structural analyses of the two peaks were carried out by HPLC-UV-MS. The main ${\alpha}$-glucosidase inhibitory compounds in the ethyl acetate-soluble fractions of ethanol extracts of Geranium thunbergii Sieb. et Zucc. were tentatively identified as geraniin and kaempferol-7-rhamnoside.

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