• 한국환경보건학회지
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• 제22권1호
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• pp.36-44
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• 1996

A comparison was made of two detection methods(UV absorbence detection and fluorescence detection with pre-column derivatization, with trifluoroacetic acid) coupled with HPLC for the simultaneous determination of aflatoxin $B_1, B_2, G_1$ and $G_2$. A good separation of the four aflatoxins was achieved on a reversed-phase $C_{18}$ column (30 cm x 3.9 mm) with methanol-acetonitrile-water(20+20+60) for absorbence detection or acetonitrile-water(25+75) for fluorescence detection at the flow rate of 1.0 ml/min. The calibration graphs were linear over the ranges 100 ppb-1 ppm for $B_1/G_1$ and 30~300 ppb for $B_2/G_1$ with absorbence detection, and 1~500 ppb for $B_1/G_1$ and 0.3~150 ppb for $B_2/G_2$ with fluorescence detection. The correlation coefficients were greater than 0.94 and 0.99 for absorbance detection and for fluorescence detection, respectively. The detection limit was 100 ng for $B_1/G_1$ and 30 ng for $B_2/G_2$ with absorbence detection, and 1 ng for $B_1/G_1$ and 0.3 ng for $B_2/G_2$ with fluorescence detection. Recovery rates of aflatoxin $B_1, B_2, G_1$ and $G_2$ added to yeast-extract sucrose broth medium were 66.6%, 59.4%, 67.5% and 59.2%, respectively, for absorbence detection and 82.9%, 71.5%, 80.0% and 69.3%, respectively, for fluorescence detection. The four aflatoxins in culture medium were quantitatively detected by the two methods. The aflatoxins in the rice sample were not detected the absorbence detection method, but were below 10 ppb using the fluorescence detection method. Analysis of aflatoxins by both the absorbence and fluorescence methods coupled with HPLC showed acceptable linearity and good recovery. The absorbence detection was less timeconsuming and safer for treatment. The fluorescence detection was more elective and sensitive though elevated $B_1$ and $G_1$ contents were determined from the TFA-induced conversion of $B_1$ to $B_{2a}$ and $G_1$ to $G_{2a}$.

• Bulletin of the Korean Chemical Society
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• 제26권2호
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• pp.268-272
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• 2005

Different detection characteristics of fluorescence immunochromatography method and high performance liquid chromatography (HPLC) method for the analysis of cyanobacterial toxins were studied. In particular, low and high limits of detection, detection time and reproducibility and detectable microcystin species were compared when fluorescence immunochromatography method and high performance liquid chromatography method were applied for the detection of microcystin (MC), a cyclic peptide toxin of the freshwater cyanobacterium Microcystis aeruginosa. A Fluorescence immunochromatography assay system has the unique advantages of short detection time and low detection limit, and high performance liquid chromatography detection method has the strong advantage of individual quantifications of several species of microcystins.

• 약학회지
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• 제45권4호
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• pp.347-351
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• 2001

A rapid and sensitive method for the determination of glyphosate, a phosphated amino acid herbicide, in whole blood is presented. After removal of protein, the whale blood was purified by using the anion exchange resin (Dowex 1), and derivatized with 9-fluorenylmethyl chloroformate (FMCL). Derivatized glyphosate from blood sample was injected onto a Whatman partisil 10SAX column and separated with 0.1M phosphate buffer (pH 2.5) and acetonitrile (ratio=3:1). The high performance liquid chromatography-fluorescence detection gave the detection limit of 86pg and linearity of 0.9999 in the range of 0.25 $\mu$g/ml and 25 $\mu$g/ml. The recoveries of glyphosate added to the blood samples were ranged from 75.3% to 100.4% compared to the samples prepared in water. The derivatized glyphosate was stable at various acidity and temperature. This method has been successfully applied to the blood samples of lethal intoxication with the herbicide glyphosate.

• Archives of Pharmacal Research
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• 제19권6호
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• pp.562-565
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• 1996

The photoreactivity of twelve anthraquinone derivatives was examined to evaluate its usefulness as a photo-reagent for the analysis of ginsenosides using photoreduction fluorescence (PRF) detection method. Among the tested compounds, 2-tert-butylandthraquinone (TBAQ), 2-chloroanthraquinone (CAQ) and anthraquinone (AQ) showed good characteristics as photoreagents. The detection limits of ginsenoside $Rg_{1}$PRF-HPLC method using TBAQ, CAQ or AQ as a photo-reagent were found to be ca. 35 ng, 50 ng and 50 ng, respectively.

• 약학회지
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• 제40권1호
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• pp.41-45
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• 1996

A high performance liquid chromatography using photoreduction fluorescence detection was described for the analysis of saikosaponins. Saikosaponins were separated on an $NH_2$ column using acetonitrile and aqueous 2-tert-butylanthraquinone(t-BAQ) as mobile phase. Column effluent was passed through a 40cm PTFE capillary tube coiled around a 10W UV lamp to reduce t-BAQ to a highly fluorescent dihydroxyanthracene derivative which was detected by a fluorescence detector. The optimal concentration of t-BAQ was found to be $6{\times}10^{-5}M$ and the optimal reaction time to be 2 seconds. The detection limit for saikosaponin a and d by this method was found to be about 280ng and 80ng. The dynamic linear range was over two orders and the correlation coefficient of the calibration curve of them was 0.998.

• 분석과학
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• 제16권6호
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• pp.499-503
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• 2003

Biotin을 4-bromomethyl-6,7-dimethoxycoumarin (BrMDMC), 18-crown-6와 $K_2CO_3$를 사용하여 형광성 유도체로 만들어 (들뜸 파장 360 nm, 방출파장 410 nm에서) 기울기 용리 HPLC 분석을 하였다. 검정선의 농도범위는 5 ~ 400 ng, 검출한계는 2 ng, 회수율 98.75%, 그리고 상대표준편차는 1.1% 이었다. 시료의 전처리는 Sep-Pak $C_{18}$ catridge를 이용하였고, 유도체 제조의 중탕온도는 $50^{\circ}C$에서 30분간 시행하였다.

• 한국농업기계학회:학술대회논문집
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• 한국농업기계학회 2000년도 THE THIRD INTERNATIONAL CONFERENCE ON AGRICULTURAL MACHINERY ENGINEERING. V.III
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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.

• Asian Journal of Atmospheric Environment
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• 제11권4호
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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.

• Bulletin of the Korean Chemical Society
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• 제20권10호
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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.

• 한국식품위생안전성학회지
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• 제13권1호
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• pp.41-46
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• 1998

HPLCdp 의한 주요 afltoxins(aflatoxins $B_1,\;B_2,\;G_1\;및\;G_2$)의 동시 분석에서 postcolumn 유도체화법을 시도하였다. Electrochemical cell (Kobra-cell)을 사용한 postcolumn 유도체화법은 기존의 precolumn 유도체화법보다 분석시간을 단축하였으며 (약 1/2 단축), 더 안전하고 , 향상된 분석능을 보였다. Aflatoxin $B_1과\;G_1의$ 경우 10~100ppb에서, 그리고 B_2와\;G_2의$ 경우 3~30 ppb에서 직선성을 나타내었다. Aflatoxin $B_1과\;G_1은$ 각각 88.9% 및 100.5%로 양호한 회수율을 보였다. Aflatoxin $B_2와\;G_2의$ 경우 분리도는 우수하였으나 회수율에있어서 변이가 크게 나타났다.