• Title/Summary/Keyword: liquid chromatography-fluorescence

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Microcystin Detection Characteristics of Fluorescence Immunochromatography and High Performance Liquid Chromatography

  • Pyo, Dong-Jin;Park, Geun-Young;Choi, Jong-Chon;Oh, Chang-Suk
    • Bulletin of the Korean Chemical Society
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    • v.26 no.2
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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.

Multiresidue Determination of Quinolones in Porcine, Chicken, and Bovine Muscle Using Liquid Chromatography with Fluorescence Detection

  • Lee, Sang-Hee;Shim, You-Sin;Kim, Hyun-Ju;Shin, Dong-Bin
    • Food Science and Biotechnology
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    • v.18 no.4
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    • pp.978-984
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    • 2009
  • An analytical method for the simultaneous determination of 9 quinolones (QNs) in porcine, chicken, and bovine muscles was developed and validated using liquid chromatography-fluorescence detector (LC-FLD). The samples were extracted using a liquid-liquid extraction (LLE) process. Chromatographic separation was achieved on a reverse phase $C_8$ column with a gradient elution using a mobile phase of 200 mM ammonium acetate buffer (pH 4.5) and acetonitrile (ACN). The proposed method was validated according to the Food and Drug Administration (FDA) guideline for bioanalytical assay procedures. Recoveries of QNs were 83.1-111.9% with relative standard deviations (RSDs) below 15%. Linearity within a range of 30-500 ${\mu}g/kg$ was obtained with the correlation coefficient ($R^2$) of 0.9967-0.9999. The limits of detection (LOD) were 1-16 ${\mu}g/kg$. These values were lower than the maximum residues limits (MRLs) established by the European Union (EU). The present method was successfully applied to determine QNs in edible muscles.

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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In vitro Folding of Recombinant Hepatitis B Virus X-Protein Produced in Escherichia coli: Formation of Folding Intermediates

  • Kim, Sun-Ok;Sohn, Mi-Jin;Jeong, Soon-Seog;Shin, Jeh-Hoon;Lee, Young-Ik
    • BMB Reports
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    • v.32 no.6
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    • pp.521-528
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    • 1999
  • The folding of recombinant hepatitis B virus X-protein (rHBx) solubilized from Escherichia coli inclusion bodies was investigated. By sequential dialysis of urea, rHBx was folded into its native structure, which was demonstrated by the efficacy of its transcriptional activation of the adenovirus major late promoter (MLP), fluorescence spectroscopy, and circular dichroism (CD) analysis. The decrease in CD values at 220 nm and a corresponding blue shift of the intrinsic fluorescence emission confirmed the ability of rHBx to refold in lower concentrations of urea, yielding the active protein. Equilibrium and kinetic studies of the refolding of rHBx were carried out by tryptophan fluorescence measurements. From the biphasic nature of the fluorescence curves, the existence of stable intermediate states in the renaturation process was inferred. Reverse phase-high performance liquid chromatography (RP-HPLC) analysis further demonstrated the existence of these intermediates and their apparent compactness.

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Microprocessor Based Laser Induced Fluorometry I. Development of System and Application to Liquid Chromatography

  • Kim, Ha-Suck;Park, Chan-Seung;Hwang, Eui-Jin;Chol, Q.-Won
    • Bulletin of the Korean Chemical Society
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    • v.5 no.6
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    • pp.253-259
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    • 1984
  • An analytical applicability of the fluorescence detection with an optical multichannel analyzer to organic dyes was studied in this work. Continuous acquisition of spectra was possible with the use of a microcomputer. The maximum acquisition rate of a spetrum with 70-point average was about 3 seconds. Floppy discs were used to store data for later use in processing. Laser induced fluorescence detector in High Performance Liquid Chromatography was chosen for an application. Fluorescein below $10^{-15}g$ was detected satisfactorily using this system. With the help of microcomputer, three dimensional chromatograms of time-wavelength-intensity were obtained.

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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Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3971-3976
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    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

Trace-level Determination of N-nitrosodimethylamine(NDMA) in Water Samples using a High-Performance Liquid Chromatography with Fluorescence Derivatization (HPLC와 Fluorescence Derivatization 기법을 이용한 극미량 NDMA의 수질분석)

  • Cha, Woo-Suk;Fox, Peter;Nalinakumari, Brijesh;Choi, Hee-Chul
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.2
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    • pp.223-228
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    • 2006
  • High-performance liquid chromatography(HPLC) and fluorescence derivatization were applied for a trace-level N-nitrosodimethylamine(NDMA) analysis of water samples. Fluorescence intensity was optimized with the excitation wavelength of 340 nm and the emission wavelength of 530 nm. pH adjustment after denitrosation was necessary to get a maximum intensity at pH between 9 and 12. Maximum intensity was found with a dansyl chloride concentration of 330 to 500 mg/L. Percentile error in the water sample analyses through solid phase extraction was 12-162% and 6-23% for the lower concentration level(10-200 ng/L NDMA) and the higher level(100-1000 ng/L NDMA), respectively, showing more discrepancy in lower level. However, the average ratios of estimated NDMA to the standard NDMA were close to 1 for both concentration ranges, presenting this HPLC method could detect from tens to hundreds nanograms NDMA per liter. Accurate determination of NDMA, which was injected to a wastewater effluent, revealed the selectivity of fluorescence derivatization for the target compound(NDMA) in the presence of complex interfering compounds. The HPLC with fluorescence derivatization may be applicable for determining NDMA of water and wastewater samples fur various research purposes.

Examination of ivermectin residues in raw milk after skin administration (원유중 Ivermectin 구충제의 잔류실태 조사)

  • Bark, Jun-Jo;Youk, Ji-Hea;Kim, Hu-Kyoung;Park, Hye-Won;Kim, In-Kyung;Lee, Woo-Seong
    • Korean Journal of Veterinary Service
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    • v.30 no.3
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    • pp.421-428
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    • 2007
  • This study was conducted two kinds of aims: 1) to modify the analytical methods (conditions) by high performance liquid chromatography - fluorescence detector for the detection of residual ivermectin in raw milk, 2) to provide basic information for the evaluation of standard of the residual ivermectin in raw milk. It could be considerable that negative ion spectra can be better method in the LC/MS analysis for the detection of residues, Characteristic daughter ions were observed in negative ion spectra, however, linear line was not formed in positive ion one. Three Holstein cows ($500{\pm}10kg$) were applied to commercial ointment of ivermectin just one time at the first day of test, and residues in raw milk were examined for 20day after administration. The limit of detection (LOD) was 0.65ng (n=5) by HPLC/FLD, and recovery rates were $87.85%{\sim}99.47%$. The peak was observed at the 4th day, and residues lasted to the end. Thus ivermectin was prohibited when lactating.

CdTe Quantum Dots as Fluorescent Probes for Josamycin Determination

  • Peng, Jinyun;Nong, Keliang;Mu, Guangshan;Huang, Fengying
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2727-2731
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    • 2011
  • A new method for the determination of josamycin has been developed based on quenching of the fluorescence of 3-mercaptopropionic acid-capped CdTe quantum dots (MPA-CdTe QDs) by josamycin in ethanol. Reaction time, interfering substances on the fluorescence quenching, and mechanism of the interaction of CdTe QDs with josamycin were investigated. Under optimum conditions, the relative fluorescence intensity was linearly proportional to the concentration of josamycin between 12.0 and 120.0 ${\mu}g\;mL^{-1}$ with a correlation coefficient of 0.9956 and a detection limit of 2.5 ${\mu}g\;mL^{-1}$. The proposed method was successfully applied to commercial tablets, and the results were satisfactory, i.e. consistent with those of high-performance liquid chromatography (HPLC).