• Title/Summary/Keyword: 2중 파장법

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Determination of residual novobiocin in livestock products and fisheries products by HPLC (HPLC를 이용한 축·수산 식품 중 잔류 노보비오신의 분석)

  • Lee, Byung Kyu;Lee, Cheol-Woo;Lee, Sang-Ju;Jung, Eun Ha;Lim, Hyun Kyun;Han, Sang Beom
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.347-354
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    • 2007
  • A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

Intra-laboratory Validation of an HPLC Post-column Oxidation Method for the Analysis of PSP Toxins in Oysters and Mussels (굴과 진주담치 중 마비성 패류독소 분석을 위한 HPLC post-column oxidation method의 시험소 내 유효성 검증)

  • Song, Ki Cheol;Lee, Ka-Jeong;Yu, Hong-Sik;Mok, Jong-Soo;Kim, Ji Hoe;Lim, Keun-Sik;Lee, Mi-Ae;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.45 no.2
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    • pp.241-247
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    • 2013
  • AOAC Mouse Bioassay Analysis (MBA) has been the gold standard for the analysis of paralytic shellfish poisoning toxin (PSP toxin) for more than 50 years. However, this method has inaccurate limit of quantification and cannot be used to determine toxic profiles. An HPLC method (PCOX) was optimized for Korean shellfish to establish an alternative or supplementary method for PSP analysis and was intended to be used for the official monitoring and regulation of food. The recovery rate of the PCOX method was 83.5-112.1% and the limit of quantification for total toxin was about $8.6{\mu}g$/100 g. A long-term comparison study showed a good correlation of the PCOX results with the AOAC MBA results: the correlation factors were 0.9534 and 0.9109 for oyster and mussel matrices, respectively. The PCOX method may be used as an alternative or supplementary method for AOAC MBA to monitor the occurrence of PSP and to analyze PSP toxin profile in oysters and mussels.

Photoluminescent properties of red phosphor (Y,Gd)$_2$O$_3$: Eu for plasma display panel synthesized by homogeneous precipitation method (균일침전법으로 제조한 플라즈마 디스플레이용 적색 형광체 (Y,Gd)$_2$O$_3$: Eu의 발광특성)

  • 김유혁;김좌연
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.10 no.6
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    • pp.400-406
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    • 2000
  • The fired Precursor (Y,Gd,Eu)(OH)$CO_3$.$H_2O$$900^{\circ}C$ was used to synthesize the red phosphor $(Y,Gd)_2O_3$: Eu for plasma display panel. Rounded and ~l $\mu\textrm{m}$ diameter phosphor $(Y,Gd)_2O_3$: Eu can be obtained by the reaction of aformentioned powder with a small amount addition of flux at $1350^{\circ}C$ for 2 hours. Emission spectra of these phosphors were measured under excitation wavelength at 254 nm and 147 nm and the optimum concentrations of activator ion were determined at around 15 mo1e % and 10 mole % under these conditions, respectively. $BaCO_3$flux had the best property in emission intensity among the prepared $BaCO_3AlF_3$and $Li_3PO_4$phosphors. The properties of optimized sample were improved in terms of relative luminance and color coordinate comparing with commercial phosphor such as $Y_2O_3$: Eu.

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Development of Analysis Method of Caffeine and Content Survey in Commercial Foods by HPLC (HPLC를 이용한 카페인의 분석법 개발 및 시판 식품중 함유량 조사)

  • Kim, Hee-Yun;Lee, Young-Ja;Hong, Ki-Hyoung;Lee, Chul-Won;Kim, Kil-Saeng;Ha, Sang-Chul
    • Korean Journal of Food Science and Technology
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    • v.31 no.6
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    • pp.1471-1476
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    • 1999
  • A simple and practical method for determination of caffeine in foods was developed. The analysis of caffeine was performed by reverse phase high performance liquid chromatography using a ${\mu}-Bondapak\;C_{18}$ column at isocratic condition with methanol-acetic acid-water(20 : 1 : 79) on UV detector at 280 nm. The clean-up and extraction of caffeine in samples were based on a simple pretreatment using a Sep-Pak $C_{18}$ cartridge. Recovery rates obtained with this method for cider, candy, cookie, milk, ice cream and persimmon leaf tea were 99.23%, 99.50%, 99.17%, 99.37%, 98.93% and 99.10% respectively. And the detection limit of caffeine was $0.1\;{\mu}g/mL$. With this method, the range of caffeine contents extracted from coffee, green tea, black tea, Oolong tea(tea bag), soft drinks, ice cream, milk and commercial confectionery were $3.38{\sim}37.50\;mg/g,\;16.30{\sim}26.10\;mg/g,\;10.80{\sim}16.65\;mg/g,\;11.25\;mg/g,\;0.06{\sim}0.11\;mg/g,\;0.04{\sim}0.44\;mg/g,\;0.04{\sim}0.39\;mg/g\;and\;0.10{\sim}1.80\;mg/g$, respectively. But caffeine was not detected in the other tea such as Acanthopanax sessiliflorum tea, Angelica gigas tea, Angelica tea, Arrow root tea, Duchu'ng tea, Dunggulle tea, Ganoerma lucidum tea, Ginger tea powder, Persimmon leaf tea, Ssanghwa tea and Cocoa mix powder.

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Comparison of Non-desructive Method to Detect Nitrogen Deficient Cucumber (질소결핍 오이의 비파괴 진단법 비교)

  • 성제훈;서상룡;류육성;정갑채
    • Journal of Biosystems Engineering
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    • v.24 no.6
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    • pp.539-546
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    • 1999
  • Some stress for a plant could be detected to a certain degree by plant physiological measuring technique of the state of the art. The capability of early detection of my measuring system depends on kind of plant and kind and level of stress. The objectives of this study were to evaluate the capability of several fast and intact type plant stress detection systems to detect nitrogen deficiency of cucumber in the field. A series of experiment was carried out with four kinds of intact type measuring devices - a chlorophyll content meter, a chlorophyll fluorescence measurement system, an infrared thermometer and an optical spectrometer. The experiments resulted that the chlorophyll content meter could detect the stress of N deficiency at a confidence level higher than 95% on 3rd day for the earliest case and the detection of high precision was possible from 7th day after the stress was applied. The chlorophyll fluorescence measurement system detected the stress at a confidence level higher than 95% on 3rd day for the earliest case but the detection was not as much precise as the chlorophyll content meter. Leaf temperature measurement noted very poor results to detect the stress. Using the spectrometer, sensitive wavelength regions to detect the stress were searched and found out as 562∼564 nm, 700∼724 nm and 1,886∼1,894 nm. With the spectrometer using any of wavelength within the sensitive wavelength region, detection of the stress at a confidence level higher than 95% was possible from 3rd or 4th day after the stress was applied.

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Vegetation Cover Type Mapping Over The Korean Peninsula Using Multitemporal AVHRR Data (시계열(時系列) AVHRR 위성자료(衛星資料)를 이용한 한반도 식생분포(植生分布) 구분(區分))

  • Lee, Kyu-Sung
    • Journal of Korean Society of Forest Science
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    • v.83 no.4
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    • pp.441-449
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    • 1994
  • The two reflective channels(red and near infrared spectrum) of advanced very high resolution radiometer(AVHRR) data were used to classify primary vegetation cover types in the Korean Peninsula. From the NOAA-11 satellite data archive of 1991, 27 daytime scenes of relatively minimum cloud coverage were obtained. After the initial radiometric calibration, normalized difference vegetation index(NDVI) was calculated for each of the 27 data sets. Four or five daily NDVI data were then overlaid for each of the six months starting from February to November and the maximum value of NDVI was retained for every pixel location to make a monthly composite. The six bands of monthly NDVI composite were nearly cloud free and used for the computer classification of vegetation cover. Based on the temporal signatures of different vegetation cover types, which were generated by an unsupervised block clustering algorithm, every pixel was classified into one of the six cover type categories. The classification result was evaluated by both qualitative interpretation and quantitative comparison with existing forest statistics. Considering frequent data acquisition, low data cost and volume, and large area coverage, it is believed that AVHRR data are effective for vegetation cover type mapping at regional scale.

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Properties of Nano-sized Au Particle Doped ZrO2 Thin Film Prepared by the Sol-gel Method (졸-겔법에 의한 나노 사이즈 Au 미립자 분산 ZrO2 박막의 특성)

  • 이승민;문종수
    • Journal of the Korean Ceramic Society
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    • v.40 no.12
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    • pp.1197-1201
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    • 2003
  • Thin film on SiO$_2$ glass was synthesized by a dip-coating method from the ZrO$_2$ sol which had dispersed nanosize Au particle under ambient atmosphere. After heat treatment of the prepared thin film, the characteristics were investigated by X-ray diffraction, UV-VIS spectrometer, Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM). It was found that ZrO$_2$ thin film with 100 nm thickness was crystallized to tetragonal phase at 50$0^{\circ}C$. The size of dispersed Au particle was 15∼40nm and the film had a smooth surface with a roughness of 0.84 nm. The film showed nonlinearity characteristics with absorption peaks at 630∼670nm visible region because of the plasma resonance of Au metallic particles.

Development and Validation of Analytical Method for Determination of Biphenyl Analysis in Foods (식품 중 비페닐 분석법 개발 및 유효성 검증)

  • Kim, Jung-Bok;Kim, Myung-Chul;Song, Sung-Woan;Shin, Jae-Wook
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.4
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    • pp.459-464
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    • 2017
  • Biphenyl is used as an intermediate in the production of crop protection products, a solvent in pharmaceutical production, and as a component in the preservation of citrus fruits in many countries. Biphenyl is not authorized for use and also does not have standards or specifications as a food additive in Korea. National and imported food products are likely to contain biphenyl. Therefore, control and management of these products is required. In this study, a simple analytical method was developed and validated using HPLC to determine biphenyl in food. These methods are validated by assessing certain performance parameters: linearity, accuracy, precision, recovery, limit of detection (LOD), and limit of quantitation (LOQ). The calibration curve was obtained from 1.0 to $100.0{\mu}g/mL$ with satisfactory relative standard deviations (RSD) of 0.999 in the representative sample (orange). In the measurement of quality control (QC) samples, accuracy was in the range of 95.8~104.0% within normal values. The inter-day and inter-day precision values were less than 2.4% RSD in the measurement of QC samples. Recoveries of biphenyl from spiked orange samples ranged from 92.7 to 99.4% with RSD between 0.7 and 1.7% at levels of 10, 50, and $100{\mu}g/mL$. The LOD and LOQ were determined to be 0.04 and $0.13{\mu}g/mL$, respectively. These results show that the developed method is appropriate for biphenyl identification and can be used to examine the safety of citrus fruits and surface treatments containing biphenyl residues.

A Study of Roughness Measurement of Rock Discontinuities Using a Confocal Laser Scanning Microscope (콘포컬 레이저 현미경을 이용한 불연속면의 거칠기 측정 연구)

  • Byung Gon Chae;Jae Yong Song;Gyo Cheol Jeong
    • The Journal of Engineering Geology
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    • v.12 no.4
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    • pp.405-419
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    • 2002
  • Fracture roughness of rock specimens is observed by a new confocal laser scanning microscope (CLSM; Olympus OLS1100). The wave length of laser is 488 nm, and the laser scanning is managed by a light polarization method using two galvano-meter scanner mirrors. The function of laser reflection auto-focusing enables us to measure line data fast and precisely. The system improves resolution in the light axis (namely z) direction because of the confocal optics. Using the CLSM, it is Possible to measure a specimen of the size up to $10{\;}{\times}{\;}10{\;}cm$ which is fixed on a specially designed stage. A sampling is managed in a spacing $2.5{\;}\mu\textrm{m}$ along x and y directions. The highest measurement resolution of z direction is $10{\;}\mu\textrm{m}$, which is more accurate than other methods. Core specimens of coarse and fine grained granite are provided. Fractures are artificially maneuvered by a Brazilian test method. Measurements are performed along three scan lines on each fracture surface. The measured data are represented as 2-D and 3-D digital images showing detailed features of roughness. Line profiles of the coarse granites represent more frequent change of undulation than those of the fine granite. Spectral analyses by the fast Fourier transform (FFT) are performed to characterize the roughness data quantitatively and to identify influential frequency of roughness. The FFT results suggest that a specimen loaded by large and low frequency energy tends to have high values of undulation change and large wave length of fracture roughness.

Direct determination of gadolinium in urania-gadolinia nuclear fuels by inductively coupled plasma atomic emission spectrometry (유도결합플라스마 원자방출분광법을 이용한 UO2-Gd2O3 핵연료 중 가돌리늄 분석)

  • Choi, Kwang-Soon;Suh, Moo-Yul;Lee, Chang-Heon;Han, Sun-Ho;Jee, Kwang-Yong
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.131-137
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    • 2007
  • The urania-gadolinia fuels were dissolved with nitric acid. The analytical conditions of ICP-AES for the direct determinations of gadolinium in the uranium matrices without separation process were investigated. Based on the effect of uranium on gadolinium intensity, the best wavelength for gadolinium was 336.223 nm. The relative deviation of two methods, direct and indirect measurements with anion exchange chromatography, was less than 5 %. Therefore it was possible for this procedure directly to measure 5~10 wt.% of gadolinium in urania-gadolinia fuels without separation by ICP-AES.