• 제목/요약/키워드: sample pretreatment

검색결과 229건 처리시간 0.027초

다채널 액상 미세 추출 시스템 설계 및 제작 (Multichannel Liquid Phase Microextraction System)

  • 장신걸;정석;박상범
    • 한국기계가공학회지
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    • 제19권10호
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    • pp.1-7
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    • 2020
  • In this study, a multichannel gas-liquid microextraction system is designed by integrating the automatic elution of extraction line and multichannel gas-purging liquid phase microextraction. The system uses an injection pump and inert gas to push the extraction solvent to a sample bottle of a gas-phase color autosampler and then implements multichannel gas-liquid microextraction and gas chromatography-mass spectrometry. The system also employs a three-way integrated micro-high-temperature heater, syringe pump, and microflow controller to realize the simultaneous processing of multiple groups of samples, thus improving the sample pretreatment speed and reproducibility and reducing human error. Autoinjection experiments were implemented with polycyclic aromatic hydrocarbon standard samples. The experiments show that the average recovery rate of the system exceeds 70%, and the relative standard among the channels is less than 15%.

저식염 속성 멸치 발효액화물 가공에 관한 연구(III) - 숙성 중 ATP관련화합물, TMAO, TMA, creatine 및 creatinine 함량변화 - (Studies on the Processing of Rapid- and low Salt-Fermented Liquefaction of Anchovy(Engrulis japonica)(III) - Changes in ATP-related compounds, TMAO, TMA, Creatine, and Creatinine during Fermentation -)

  • 박춘규
    • 한국식생활문화학회지
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    • 제17권4호
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    • pp.482-495
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    • 2002
  • Changes in ATP and related compounds, TMAO, TMA, creatine and creatinine were analyzed to establish the processing conditions for rapid- and low salt-fermented liquefaction of anchovy(Engrulis japonica) extracts during fermentation. Experimental sample A: chopped whole anchovy, adding 20% water, heating at $50^{\circ}C$ for 9 hrs and then adding 10% NaCl. Sample B: chopped whole anchovy, adding 20% water, heating at $50^{\circ}C$ for 9 hrs and then adding 13% NaCl. Sample C: chopped whole anchovy adding 13% NaCl. Sample D: whole anchovy adding 17% NaCl. ATP, ADP, AMP and IMP were broken down during fermentation period, while inosine and hypoxanthine or hypoxanthine were detected in each fermented liquefaction of anchovy. However the amounts of them were varied from collection to collection according to the pretreatment methods. Possibly ATP and their related compounds will not make a great contribution to the umami taste in fermented liquefaction of anchovy. The contents of TMAO were decreased during fermentation period, ranging from 3 to 15 mg/100g in the fermented liquefaction of anchovy after 180 days. The TMA contents were increased slowly during fermentation period, ranging from 60 to 114 mg/100g in the 180 days specimens, however their contents were varied from sample to sample. The contents of creatine and creatinine were increased during early fermentation period, and then they were decreased in the last period. As for distribution of nitrogen in the anchovy extracts, the contribution of creatine and creatinine to the extractive nitrogen was occupying 6.8, 5.7, 4.6 and 5.7% in the experimental sample A, B, C and D, respectively. The contribution of ATP and related compounds to the extractive nitrogen was occupying 2.1, 2.4, 2.2 and 2.7% in the experimental sample A, B, C and D, respectively. The contribution of TMAO and TMA to the extractive nitrogen was very low as they are occupying $0.7{\sim}1.2%$ in the four experimental samples.

몬테카를로 전산해석을 이용한 콘크리트 코어시료의 직경과 밀도에 따른 보정인자 계산 (Calculation of the Correction Factors related to the Diameter and Density of the Concrete Core Samples using a Monte Carlo Simulation)

  • 이규영;강보선
    • 한국방사선학회논문지
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    • 제14권5호
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    • pp.503-510
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    • 2020
  • 콘크리트는 원자력 시설의 차폐용 구조물로 광범위하게 사용되고 있는 재료이다. 하지만, 시설의 해체 시 양적으로 가장 많이 발생하는 방사성 폐기물이기도하다. 콘크리트는 중성자를 포획하여 다양한 방사성 핵종을 생성하기 때문에 해체 전에 시료를 채취하여 방사능 측정 및 평가를 수행해야 한다. 측정은 주로 HPGe 검출기를 이용하는데 시료의 정확한 방사능 판정을 위해는 기하학적 보정인자, 자가흡수 보정인자, 계측기의 절대효율 등 효과적인 보정인자를 측정치에 반영해야 한다. 보정인자는 기하학적 및 화학적 상태가 실제 시료와 동일한 표준시료를 이용해서 동일한 측정조건 하에서 획득한다. 하지만, 콘크리트는 다양한 구성물질과 높은 밀도로 전처리가 제한적이므로 콘크리트 표준시료를 제작하는 것은 매우 어렵다. 또한 코어드릴(core drill)을 사용하여 채취되는 콘크리트 시료는 체적선원이므로 직경에 대한 기하학적 보정과 밀도에 대한 자가흡수에 대한 보정이 필수적이다. 따라서, 최근에는 많은 연구자들이 표준선원을 제작 후 측정하는 대신 몬테카를로 전산모사(Monte Carlo simulation)을 이용하여 효과적인 보정인자들을 계산하는 연구를 수행하고 있다. 본 연구에서는 Monte Carlo code 중 하나인 Geant4를 이용하여 방사화 콘크리트에서 가장 많이 생성되는 핵종인 152Eu, 60Co에서 방출되는 감마선 에너지에 대한 콘크리트 코어시료의 직경과 밀도에 따른 보정인자를 산출하였다.

CE-AD기반의 Microfluidic chip을 이용한 Simazine과 Atrazine 그리고 Ametryn Herbicides의 검출 (Detection of Simazine, Atrazine and Ametryn Herbicides on a Microfluidic Chip Based on CE-AD)

  • ;장유철;;;김용상
    • 대한전기학회:학술대회논문집
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    • 대한전기학회 2011년도 제42회 하계학술대회
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    • pp.1688-1689
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    • 2011
  • A simple and rapid capillary electrophoresis method was developed for the quantitative analysis of common triazine herbicides. Cyclic voltammetry was employed to clarify the detection voltage which showed characteristic irreversible cathodic peaks. For the analysis, the mixture of triazine herbicides was applied in a microfluidic chip to determine the CE-separated peaks. Soil sample extracts were analyzed directly after drying and redissolution with the supporting electrolyte but without other pretreatment. The results were comparable to those obtained by HPLC with UV detection. Therefore, this method can be used in the rapid determination of pesticide/herbicide residues.

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후추중의 Piperine 정량법에 관한 연구 (A Study on Quantitative Method of Piperine in Pure Ground Black Pepper)

  • 고종명
    • 한국식품위생안전성학회지
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    • 제10권3호
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    • pp.169-174
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    • 1995
  • Piperine, component of pure ground black pepper, has strong stimulative and hot. Analytical method for piperine was developed by high performance liquid chromatography. Analytical conditions are as follows, mobile phase is 70% methanol, detector UV 343 nm (0.05 AuFs), column is Novapak 5 C18 (15 cm $\times$ 4.6mm), flow rate is 1.0ml/min, chart speed is 0.25 cm/min and injection volume is 20 ul. Analytical results are as follows that relative standard deviation is 1.15%, calibration curve is y=170473.1x-7848.5 (R2=0.999) that shows good linearity. Standard solution of piperine is stable up to 10 hr and content of piperine in pureground black pepper is 4.97$\pm$0.86% Retention time of piperine in HPLC method is about 7 min. Therefore, the developed HPLC method including simple pretreatment of sample will be contribute to quality mangement.

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MasterSizer와 SediGraph에 의한 입도분석 결과의 비교 및 문제점 (Comparison of Two Methods in Grain-size analysis: SediGraph and Master Sizer)

  • 정회수;김광신
    • 한국해양학회지
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    • 제28권1호
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    • pp.72-78
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    • 1993
  • MasterSizer와 SediGraph를 이용하여 표준입자와 여러 종유의 퇴적물을 분석하고 그 결과를 비교하였다. SediGraph에 의해 분석된 퇴적물 시료의 입도분석 결과는 MasterSizer에 의한 결과보다 세립하게 나타나는 데, 특히 심해저의 규질연니 퇴적물 에서 그 차이가 크다. 이러한 차이는 시료의 전처리 과정, 기기에 도입되는 시료 농 도, 세립한 입자(약 1um 이하) 감지 능력, 그리고 비구형 입자가 두 기기에 인지되는 방식 등 두 방법상의 여러 가지 다른 점에 기인할 가능성이 있다.

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HPLC를 이용한 식품 보존료의 동시분석에 관한 연구 (Studies on Simultaneous Analysis of Preservatives by High Pressure Liquid Chromatography in Foods)

  • 김우성;임복규;백종민;박인원;박인원;임연하;지영애;조경종
    • 한국식품위생안전성학회지
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    • 제7권1호
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    • pp.49-52
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    • 1992
  • 식품에 잔류하는 보존료를 동시에 정성 및 정량 분석하고자 수증기 증류법에 의한 전처리한 용액을 HPLC주입하여 Chromatogram을 얻었다. cosmosil $5C_{18}$ HPLC column을 상용하였고, 이동상 용매로서는 1% phosphotic acid와 acetonitrile(60 : 40) 혼합용매를 사용하였고 220 nm의 검출 파장 조건에서 실험해 본 결과 분리도가 좋은 chromatogram을 얻었다. 따라서 수증기 증류법에 의해 단 한번의 전처리 과정을 거쳐 HPLC를 이용하여 보존료를 동시 분석, 정성 및 정량이 가능하였다.

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모세관 전기영동 분석법의 복합약물제제의 품질관리 분석에 응용을 위한 연구 (Application of Capillary Electrophoresis for Quality Control Analysis of Complex Medicine)

  • 허유정;이공주
    • 약학회지
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    • 제41권5호
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    • pp.539-546
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    • 1997
  • Capillary electrophoresis (CE) is perceived as an attractive tool for the analysis of pharmaceuticals and biological materials because of their high separation efficiency, easy separation and low running cost. New concept of micellar electrokinetic capillary chromatography (MECC) expanded the application of CE to the separation of neutral molecules. Validation of CE as an analytical technique for quality control of pharmaceuticals should be confirmed by quantitative analysis and the peak confirmation. In this study, the quantitative analyses of various types of neutral, acidic and basic components (acetaminophen, caffeine, ascorbic acid, riboflavin, thiamine, chlorpheniramine, phenylpropanolamine, dl-methylephedrine and dextromethorphan) in complex cold medicines have been accomplished using CE. Combined methods of MECC using SDS and capillary zone electrophoresis lowering the pH of running buffer were adopted to determine the ingredients in capsule type or liquid formula complex medicines without particular sample pretreatment. The results indicate that CE is a promising technique for quality control analysis of pharmaceuticals as a validation method.

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크롬계 이중도금층 제조 및 특성평가 (Fabrication of Chromium-based Double Layered Deposit)

  • 박상언;김동수;김만;장도연;권식철
    • 연구논문집
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    • 통권31호
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    • pp.127-133
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    • 2001
  • In chromium electrodeposition, crack is inevitably accompanied by chromium layer. Behavior of crack formation and crack density were different from the plating conditions such as current density, temperature, waveform of applied current and so on. And cracks have an influence on the corrosion resistance of chromium deposit, because corrosion occurs through the network of cracks between deposit and substrate. Therefore, many researches have been achieved in order to remove the cracks in chromium deposit. Formation of double layers, Cr/Cr and Ni/Cr were investigated to increase corrosion resistance of chromium deposit in this study. As pretreatment prior to outer chromium coating, acid pickling and current control method were examined. Cracks in cross-section of each sample were observed with SEM and CASS(Copper modified acetic acid salt spray) test was performed to evaluate corrosion resistance. It was found that corrosion resistance of Cr/Cr and Ni/Cr double layers were superior to Cr or Ni single layer from the results of CASS test.

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A Synthesis of Optically Active cis and trans 2-(5-Hydroxypoperidin-2-yl)acetates

  • P.N. Reddy;한상수;정교현
    • Bulletin of the Korean Chemical Society
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    • 제19권6호
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    • pp.617-618
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    • 1998
  • A simple and reproducible pretreatment method was developed for the determination of dioxins in milk sample. Liquid-liquid extraction (LLE) was used for the initial extraction of the analyte from milk. For the elimination of interferences coextracted from milk, acid treatment followed by multilayer silica gel, and then alumina column clean-up were performed. The clean extract could be obtained without carbon column or high performance liquid chromatographic (HPLC) clean-up procedure. Polychlorinated biphenyles (PCBs) and dioxins were separated on neutral alumina activated at 180 ℃ for 12 hours. The final extract was analyzed by HPLC and high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS). The recovery of dioxins spiked in milk at 75-300 ppt level was 83.3-98.9% and their relative standard deviation was 4.1-14%.