• Title/Summary/Keyword: HPLC/Fluorescence

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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.

Haematococcus pluvialis Cell-Mass Sensing Using Ultraviolet Fluorescence Spectroscopy

  • Lababpour, Abdolmajid;Hong, Seong-Joo;Lee, Choul-Gyun
    • Journal of Microbiology and Biotechnology
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    • v.17 no.12
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    • pp.1922-1929
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    • 2007
  • A simple whole-cell-based sensing system is proposed for determining the cell mass of H. pluvialis using ultraviolet fluorescence spectroscopy. An emission signal at 368 nm was used to detect the various kinds of green, green-brown, brown-red, and red H. pluvialis cells. The fluorescence emission intensities of the cells were highest at 368 nm with an excitation wavelength of 227 nm. An excitation wavelength of 227 nm was then selected for cell-mass sensing, as the emission fluorescence intensities of the cell suspensions were highest at this wavelength after subtracting the background interference. The emission fluorescence intensities of HPLC-grade water, filtered water, and HPLC-grade water containing a modified Bold's basal medium (MBBM) were measured and the difference was less than 1.6 for the selected wavelengths. Moreover, there was no difference in the emission intensity at 368 nm among suspensions of the various morphological states of the cells. A calibration curve of the fluorescence emission intensities. and cell mass was obtained with a high correlation ($R^2=0.9938$) for the various morphological forms of H. pluvialis. Accordingly, the proposed method showed no significant dependency on the various morphological cell forms, making it applicable for cell-mass measurement. A high correlation was found between the fluorescence emission intensities and the dry cell weight with a mixture of green, green-brown, brown-red, and red cells. In conclusion, the proposed model can be directly used for cell-mass sensing without any pretreatment and has potential use as a noninvasive method for the online determination of algal biomass.

Analysis of Melatonin Content from Domestic Edible Plants (국내산 식용식물체의 멜라토닌 함량 분석)

  • Kim, Seok-Joong
    • Korean Journal of Food Science and Technology
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    • v.34 no.6
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    • pp.1145-1148
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    • 2002
  • Melatonin, which is a hormone secreted from pineal gland of brain and known to prevent oxidative damages of various tissues, was analyzed in 26 domestic edible plants. For the preparation of melatonin fraction, 50% ethanol extract prepared from lyophilized plant powder was filtered and applied on TLC plate. Melatonin position on TLC developed with acetone was identified by fluorescence light and extracted with methanol. This methanolic fraction was injected into HPLC comprising ODS-A column, fluorescence detector, and mobile phase consisting of a mixture (30 : 70, v/v) of 70% ammonium acetate and methanol at a flow rate of 1.0 mL/min. Melatonin was identified at the retention time of 17 min. Results revealed that celery, leek, broccoli, and cauliflower had higher melatonin contents than others.

Simultaneous Determination of Polycyclic Aromatic Hydrocarbons and Their Nitro-derivatives in Airborne Particulates by Using Two-dimensional High-performance Liquid Chromatography with On-line Reduction and Fluorescence Detection

  • Boongla, Yaowatat;Orakij, Walaiporn;Nagaoka, Yuuki;Tang, Ning;Hayakawa, Kazuichi;Toriba, Akira
    • Asian Journal of Atmospheric Environment
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    • v.11 no.4
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    • pp.283-299
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    • 2017
  • An analytical method using high-performance liquid chromatography (HPLC) with fluorescence (FL) detection was developed for simultaneously analyzing 10 polycyclic aromatic hydrocarbons (PAHs) and 18 nitro-derivatives of PAHs (NPAHs). The two-dimensional HPLC system consists of an on-line clean-up and reduction for NPAHs in the 1st dimension, and separation of the PAHs and the reduced NPAHs and their FL detection in the 2nd dimension after column-switching. To identify an ideal clean-up column for removing sample matrix that may interfere with detection of the analytes, the characteristics of 8 reversed-phase columns were evaluated. The nitrophenylethyl (NPE)-bonded silica column was selected because of its shorter elution band and larger retention factors of the analytes due to strong dipole-dipole interactions. The amino-substituted PAHs (reduced NPAHs), PAHs and deuterated internal standards were separated on polymeric octadecyl-bonded silica (ODS) columns and by dual-channel detection within 120 min including clean-up and reduction steps. The limits of detection were 0.1-9.2 pg per injection for PAHs and 0.1-140 pg per injection for NPAHs. For validation, the method was applied to analyze crude extracts of fine particulate matter ($PM_{2.5}$) samples and achieved good analytical precision and accuracy. Moreover, the standard reference material (SRM1649b, urban dust) was analyzed by this method and the observed concentrations of PAHs and NPAHs were similar to those in previous reports. Thus, the method developed here-in has the potential to become a standard HPLC-based method, especially for NPAHs.

MEASUREMENT OF PESTICIDES RESIDUES USING SPECTROSCOPY ON AGRICULTURAL PRODUCTS

  • Kim, Y. W.;S. H. Noh
    • Proceedings of the Korean Society for Agricultural Machinery Conference
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    • 2000.11c
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    • pp.525-532
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    • 2000
  • A new spectroscopic method for pesticide residues detection on agricultural products was developed. The general determination methods are high performance liquid chromatography (HPLC), gas chromatography (GC) or GC-mass spectrometry. They have provided relatively good detection limit and accuracy with complicated and time-consuming (5hrs above) procedures. In addition freshness is very important for evaluating qualities of agricultural products. This requires a simple and fast method for detection of pesticides. Reflectance, transmittance and fluorescence spectrometry of pesticides were tested using UV range because most of pesticides contain conjugation band in the molecular structures. Fluorescence spectrometry showed better sensitive to detect pesticide residues than did reflectance and transmittance spectrometry. Intensity and shape of fluorescence spectra showed different patterns with different structures of pesticides. Detection limit for fluorescence spectrometry was 0.1 ppm to 10 ppm depending on the structures of pesticides. Application of fluorescence spectrometry appears to be an easy method for detection of pesticide residues on agricultural products.

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Determination of Aflatoxins Using High-Performance Liquid Chromatography with Optimized Fluorescence Detection (HPLC에 의한 aflatoxin 분석법에 관한 연구-형광검출의 최적조건)

  • 김종규
    • Journal of Food Hygiene and Safety
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    • v.13 no.1
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    • pp.41-46
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    • 1998
  • A postcolumn derivatization method was tried for the simultaneous determination of four major aflatoxins ($B_1,\;B_2,\;G_1,\;and\;G_2$) by high-performance liquid chromatography with fluorescence detection. As compared with a previous precolumn derivatization method, it was found that the postcolumn derivatization combined with an electrochemical cell (Kobra cell) was less time-consuming, safer, improved the sensitivity and selectivity, and provided good recoveries for aflatoxin $B_1$ (88.9%) and $G_1$ (100.5%). This method showed linearity from 10~100 ppb for aflatoxin $B_1\;and\;G_1$, and from 3~30 ppb for aflatoxin $B_2\;and\;G_2$. However, aflatoxin Bz and Gz were not detected satisfactorily although they showed good resolution.

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Analysis of Ginseng Saponins by HPLC with Photoreduction Fluorescence Detection

  • Kim, Bae-Yuan;Lee, Mi-Young;Cho, Kyung-Hee;Park, Jeong-Hill;Park, Man-Ki
    • Archives of Pharmacal Research
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    • v.15 no.4
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    • pp.328-332
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    • 1992
  • A new high performance liquid chromatographic procedure is described for the analysis of ginseng saponins. Ginseng saponins were separated on Lichrosorb $NH_2$ column and anthraquinone-2, 6-disulfonate (AQDS) solution was added to the column effluent. The effluent was passed through 1.5m-PTFE capillary coiled around 10 W-UV lamp to reduce AQDS to highly fluorescent 9. 10-dihydroxyanthracene-2, 6-disulfonate which was detected by fluorescence detector. The detection limit for the ginsenoside $Rg_1$ by this method was found to be about 350 ng, the dynamic linear range was $10^2$ and the correlation coefficient of the calibration curve was 0.9999.

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A study on simultaneous determination of carbamate pesticides by HPLC (HPLC를 이용한 carbamate계 농약의 다성분 동시분석)

  • Song, Young-Gak;Seo, Young-Chul;Hyun, Gong-Yul;Cho, Woo-Young;Lee, Jong-In
    • Korean Journal of Veterinary Service
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    • v.26 no.2
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    • pp.145-149
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    • 2003
  • To explore the most sensitive and useful method for simultaneous determination of 8 carbamate pesticides in livestock productions, the mixture of 8 carbonates was determined by HPLC with scanning fluorescence detector. For mobile phase water, acetonitrile and methanol program gradient showed more applicable sensitivity than water and acetonitrile program gradient used ExW 339 nm and EmW 445 nm for fluorescence detector. On using carbamate columns, the retention time was within 4 to 20 minutes. And this made it possible to separate and detect simultaneously. therefore we could analyze it exactly and efficiently and reduce time. The preparation process of MSPD method showed that the high recovery rate was more than 88.5% in most of the carbamate pesticides. Therefore we could say that it was an efficient and fast method analyzing out of lots of samples.

A Study on the Separation of n-Hexane by Molecular Sieve 5A and the Purification for HPLC use (분자체 5A를 이용한 n-헥산의 분리와 HPLC급으로의 정제에 관한 연구)

  • Choi, Beom Suk;Kim, Young Man;Kim, Sun Tae
    • Analytical Science and Technology
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    • v.6 no.1
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    • pp.21-27
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    • 1993
  • Technical grade n-hexane whose purity is 54% has been purified for HPLC use. Methylcyclopentane, 2-methylpentane, and 3-methylpentane which are hardly isolated by fractional distillation were separated by the liquid-solid chromatography using molecular sieve 5A. UV and fluorescence impurities whose contents are critically regulated for HPLC solvent were removed by the adsorptive separation with alumina and silica gel. The present method also reduced the impurities of color(APHA), acidity, water, residue after evaporation, sulfur, and thiophene content, and the impurity contents were well within the specifications of HPLC solvent.

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