• Title/Summary/Keyword: Liquid chromatography- fluorescence detector

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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.

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.

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.

Comparison of Extraction Procedures for the Determination of Capsaicinoids in Peppers

  • Jeon, Geonuk;Lee, Jun-Soo
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1515-1518
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    • 2009
  • The objective of this study was to compare 3 extraction methods including, solid phase extraction (SPE), acetonitrile extraction, and methanol extraction, for their usefulness as extraction methods to determine capsaicinoids. The determination of capsaicinoids in the extracts was carried out on a reverse-phased high performance liquid chromatography (HPLC) using a fluorescence detector. Three extraction methods, i.e., SPE, acetonitrile extraction, and methanol extraction were compared for the quantification of capsaicinoids using raw peppers and pepper powder. The highest analytical values were observed using methanol extraction and the lowest values using SPE. Also, the analytical method validation parameters such as accuracy, precision, limit of detection, limit of quantitation, and specificity were calculated to ensure the method's validity. This method provides a fast and accurate approach for the determination of capsaicinoids in peppers.

Sialylated oligosaccharide analyses using high-performance liquid chromatography with a fluorescence detector

  • Cho, Due-Hyeon;Ryu, Chang-Soo;Park, Jee-Hun;Kim, Ha-Hyung
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.316.1-316.1
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    • 2003
  • N-acetylneuraminic acid is one of the major derivatives of sialic acid. is widely distributed in mammalian cells as the ${\alpha}$2-3- or ${\alpha}$2-6-linked nonreducing terminal residue of oligosaccharide chains of glycoconjugates, and plays important structural and functional roles at the cell membrane surface. The analysis of sialylated glycoproteins is an important part of glycoprotein characterization, especially because sialylation or desialylation in oligosaccharides often causes dramatic changes in the function of glycoproteins. (omitted)

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Compositional Sugar Analysis of Antitumor Polysaccharidees by High Performance Liquid Chromatography and Gas Chromatography

  • Kim, Yeong-Shik;Park, Kyung-Shin;Park, Ho-Koon;Kim, Sung-Whan
    • Archives of Pharmacal Research
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    • v.17 no.5
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    • pp.337-342
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    • 1994
  • Carbohydrate analysis is important in studying structure and activity of complex polysaccharides. New analytical method was applied to get an information on the composition of polysaccharides showing antitumor activity. Monosaccharides were labeled with 7-amino-1, 3-naph-thalenedisulfonic acid (7-AGA) by reductive amination and separated by HPLC. Five kinds of polysaccharides from Basidiomycetes were hydrolyzed and analyzed in combination with electrophresis and HPLC. At the same time, alditol acetate derivatives were prepared and analyzed by gas chromatography. Two different techniques using different derivatization methods showed very similar results. The monosaccharides from Coriolus versicolor and Cordyceps militaris were glucose and galactose. Phellinus linteus composed of glucose, glactose, mannose, arabinose and fucose. The HPLC method with fluorescence detector was very sensitive compared to other methods.

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Study on Decomposition of Several Pesticides by Gamma-Irradiation (감마선 조사에 의한 농약 성분의 분해 연구)

  • Lee, Joo-Sang;Jung, Su-Yeon;Oh, Seung-Yeol;Jang, Beom-Su;Park, Sang Hyun
    • Journal of Radiation Industry
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    • v.6 no.3
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    • pp.205-209
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    • 2012
  • The decomposition of 50 pesticides present in an aqueous solution using ${\gamma}-irradiation$ from a $^{60}Co$ gamma-ray source was investigated using laboratory-scale experiment. The rates of decomposition were determined using a gas chromatography-electron capture detector (GC-ECD), high-performance liquid chromatography-photo diode array detector (HPLC-PDA), and HPLC-fluorescence detector (FLD). When the initial concentration of pesticides was 10 ppm, and the radiation dose was 2, 5, 10, 20, and 30 kGy, respectively, 14 pesticide samples showed high removal rates (>50%) at absorbed doses of more than 10 kGy. With the exception of procymidone, they were all completely removed at a 30 kGy irradiation dose. These results provide fundamental data on the reactivity between gamma-irradiation and pesticides in an aqueous solution. Further, an evaluation of the toxicity of radiolytic intermediate products is required.

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.

Analysis of Saikosaponins by HPLC with Photoreduction Fluorescence Detection (광반응 HPLC를 이용한 시호 사포닌의 분석)

  • Shin, Young-Geun;Cho, Kyung-Hee;Kwon, Soo-Jin;Do, Young-Mi;Hwang, Gwi-Seo;Park, Jeong-Hill;Park, Man-Ki
    • YAKHAK HOEJI
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    • v.40 no.1
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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.

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A New Analytical Method for Fluoroquinolones in Fisheries Products by High Performance Liquid Chromatography (HPLC를 이용한 어패류 중의 fluoroquinolone계 항균제의 분석법)

  • Jo Mi-Ra;Kim Poong-Ho;Lee Hee-Jung;Lee Tae-Seek
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.39 no.2
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    • pp.59-65
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    • 2006
  • Fluoroquinolones are the most common group of antibacterial agents currently used in the Korean aquaculture industry, and use of these agents has been increasing steadily. High performance liquid chromatography (HPLC) with fluorescence detection was used for the simultaneous determination of five fluoroquinolones in fish and shellfish: ofloxacin (OFL), pefloxacin (PEF), norfloxacin (NOR), ciprofloxacin (CIP), and enrofloxacin (ENRO). Fish and shellfish muscle was homogenized, and protein, lipid, and low molecular weight pigments were then excluded from the homogenate. The final eluates were analyzed by HPLC equipped with a Shiseido UG-120 type C18 reverse-phase column ($4.6{\times}250 mm$, $5{\mu}m$) and a fluorescence detector (excitation at 280 nm, emission at 450 nm). The mobile phase was 0.1 M phosphoric acid and acetonitrile solution (91:9, v/v) and tetrahydrofuran (THF) was added to it at a rate of 5 mL per a liter of the mobile phase. Adequate chromatography separation was obtained using the above method. Average recoveries of fortified samples at levels from 0.05 to 0.5 mg/kg were $72.3{\pm}2.5-84.5{\pm}1.2%$ for OFL, $82.7{\pm}3.3- 109.3{\pm}7.5%$ for NOR, $85.3{\pm}6.6-116.0{\pm}7.9%$ for PEF, $76.0{\pm}4.3-109.3{\pm}12.4%$ for CIP, and $78.7{\pm}5.9-100.0{\pm}9.8%$ for ENRO. The limit of detection of OFL was $5{\mu}g/L$, the others were $1{\mu}g/L$. We concluded that the new analytical method was suitable for the determination of fluoroquinolones in fish and shellfish.