• 제목/요약/키워드: Chemical detection methods

검색결과 245건 처리시간 0.023초

Chemical Derivatization of Catecholamines for Gas Chromatography-Mass Spectrometry

  • Park, Sun-Young;Kang, Bo-Xin;Li, Quing;Kim, Hoon-Sik;Lee, Jun-Gae;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • 제30권7호
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    • pp.1497-1504
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    • 2009
  • GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

Combined Isobutoxycarbonylation and tert-Butyldimethylsilylation for the GC/MS-SIM Detection of Alkylphenols, Chlorophenols and Bisphenol A in Mackerel Samples

  • Kim, Hyub;Hong, Jong-Ki;Kim, Yong-Hwa;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • 제26권9호
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    • pp.697-705
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    • 2003
  • The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization and tert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 6$0^{\circ}C$ for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3∼150.6% and 93.8∼108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 $\mu$ g/kg and 0.010 $\mu$ g/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755∼0.9981 and 0.9908∼0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.

Development of Continuous Flow Microwave Digestion Procedures for Analysis of Trace Metal in Water Using Ion Chromatography

  • Youn Doo Kim;Gae Ho Lee;Hyung Seung Kim;Dong Soo Kim;Kwang Kyu Park
    • Bulletin of the Korean Chemical Society
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    • 제15권9호
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    • pp.786-791
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    • 1994
  • A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

수질 시료 중의 Pesticide Priority Pollutants 동시분석에 관한 연구 (Simultaneous Analysis of Pesticide Priority Pollutants in Water Samples)

  • 김계영;김종혁;이석근
    • 대한화학회지
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    • 제37권6호
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    • pp.590-598
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    • 1993
  • 미국의 환경청이 지정한 129종의 priority pollutants 중 16종의 유기살충제를 대상물질로 선정하여 수질시료 중의 극미량 분석방법을 연구하였다. 분석방법으로는 기체크로마토그래프-전자포획 및 기체크로마토그래프/질량분석기-SIM(selected ion moitoring)법을 검출방법으로 정하고, 시료용액의 추출 및 농축방법으로는 용매추출법(liquid-liquid extraction)과 고체상 추출법(solid-phase extraction)을 비교 연구하였다. 각 화합물들의 회수율, 상대표준편차 및 검출한계 등을 측정하여 EPA 분석법을 대체할 수 있는지의 가능성을 조사하였다.

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발효유제품에서 박테리오파지의 특성, 검출과 제어 (The Characteristics, Detection and Control of Bacteriophage in Fermented Dairy Products)

  • 안성일;리합 아조니;트란 티 탄 후옌;곽해수
    • 한국축산식품학회지
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    • 제29권1호
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    • pp.1-14
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    • 2009
  • This study was to review the classification, detection and control of bacteriophage in fermented dairy products. Bacteriophage has lytic and/or lysogenic life cycles. Epidemiologically speaking, detected major phages are c2, 936 and p335. Among them p335 has been the largest concern in dairy industry. Traditionally, various analytical technologies, such as spot, starter activity, indicator test, ATP measurement and conductimetric analysis, have been used for the phage detection. In recent years, advanced methods such as flow cytometric method, petrifilm, enzyme linked immunosorbent assay (ELISA) and multiflex PCR diagnostic kit have been deveoloped. The phage contamination has been controlled by using heat, high-pressure treatment, and the combinations of heat and pressure, and/or chemical. Also some starter cultures with phage-resistant character have been developed to minimize the concentration of phages in dairy product. Bacteriophage inhibition media such as calcium medium was also mentioned. To prevent the contamination of bacteriophage in dairy industry, further researches on the detection and control of phage, and phage resistant starters are necessary in the future.

미세유체 기반의 플랫폼을 이용한 미지의 백색가루 간이식별 탐지방안 (Simple Identification Methods for Unknown Suspicious White Powders using Microfluidic-based Platform)

  • 박재우;송지영;나상철;변기식;전누리
    • 한국군사과학기술학회지
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    • 제20권6호
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    • pp.853-859
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    • 2017
  • Terrorists always threats the global security with the possibility of using prohibited warfare, NBCs(Nuclear, Biological and Chemical Warfare). Compared to other prohibited warfares, most of biological warfare agents (BWAs) have no physical properties and time delays from spread to affect. Therefore the early detection is important to protect and decontaminate from BWAs. On the preliminary detection stage for suspicious material, most of detection kits only serve to know weather the BWAs exists or not. Due to this reason, simple field confirmation testing for suspicious substances have been used to identify materials which show negative result on detection kits. Considering the current Lab on a Chip(LOC) technologies, we suggest simple identification platform for unknown suspicious substances based on paper fluidics. We hope that our research will envision the future direction for the specific point-of-view for LOC technologies on detection strategy of BWAs.

머신러닝 기법을 활용한 LDPE 공정의 이상 감지 (Fault Detection in LDPE Process using Machine Learning Techniques)

  • 이창송;이규황;이호경
    • Korean Chemical Engineering Research
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    • 제58권2호
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    • pp.224-229
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    • 2020
  • 머신러닝 기법을 활용하여 LDPE (Low Density Polyethylene) 공정의 이상을 사전 감지하고, 설비의 수명을 예측할 수 있는 기술을 소개한다. 안전성과 생산성 극대화를 위해, 화학 공정의 예상치 못한 이상을 사전에 감지하고 예방하는 것은 매우 중요하다. LDPE 공정은 3,000 kg/㎠g 이상까지 승압되는 고압 공정이기 때문에, ESD (Emergency Shutdown)가 발생하면 예상치 못한 부동이 발생하고, 그에 따른 보수 기간 증가로 인한 생산성 손실이 발생한다. 고압 공정의 주요 변수들의 운전 데이터를 수집하고, 비지도학습 머신러닝 기술을 활용하여, ESD의 사전 감지 모형을 개발하였다. 4회의 ESD를 2.4일 전에 감지하는 결과를 얻을 수 있었다. 더불어, 물리적으로 의미 있는 핵심 변수들을 활용하면, 고압 설비의 수명을 예측할 수 있음을 확인할 수 있었다.

Body fluid identification in forensics

  • An, Ja-Hyun;Shin, Kyoung-Jin;Yang, Woo-Ick;Lee, Hwan-Young
    • BMB Reports
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    • 제45권10호
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    • pp.545-553
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    • 2012
  • Determination of the type and origin of the body fluids found at a crime scene can give important insights into crime scene reconstruction by supporting a link between sample donors and actual criminal acts. For more than a century, numerous types of body fluid identification methods have been developed, such as chemical tests, immunological tests, protein catalytic activity tests, spectroscopic methods and microscopy. However, these conventional body fluid identification methods are mostly presumptive, and are carried out for only one body fluid at a time. Therefore, the use of a molecular genetics-based approach using RNA profiling or DNA methylation detection has been recently proposed to supplant conventional body fluid identification methods. Several RNA markers and tDMRs (tissue-specific differentially methylated regions) which are specific to forensically relevant body fluids have been identified, and their specificities and sensitivities have been tested using various samples. In this review, we provide an overview of the present knowledge and the most recent developments in forensic body fluid identification and discuss its possible practical application to forensic casework.

용융아연 도금강판의 도금층에 잔류한 드로스 검출에 관한 연구 (A Study on Detecting Dross in Coating Layer on Hot-dip Galvanizing Steels)

  • 김유철;이호종
    • 한국표면공학회지
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    • 제36권6호
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    • pp.466-474
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    • 2003
  • To develop a method of detecting dross in coating layer on hot-dip galvanizing steel, chemical etching behavior of the artificial coating layers with top and bottom dross were investigated. After chemical etching with the mixture of picric acid and sodium thiosulfate, each of the top and bottom dross take its distinct color, and alloy layer in coating is also observed. Defects in the coating layers of HGI(hot rolled galvanized iron), CGI(continuous galvanized steel sheet) and GA(galvannealed steel) were analysed, and methods of dross detection which can be applied to inspection process in manufacture were suggested.

Photo-induced inter-protein interaction changes in the time domain; a blue light sensor protein PixD

  • Terazima, Masahide
    • Rapid Communication in Photoscience
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    • 제4권1호
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    • pp.1-8
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    • 2015
  • For understanding molecular mechanisms of photochemical reactions, in particular reactions of proteins with biological functions, it is important to elucidate both the initial reactions from the photoexcited states and the series of subsequent chemical reactions, e.g., conformation, intermolecular interactions (hydrogen bonding, hydrophobic interactions), and inter-protein interactions (oligomer formation, dissociation reactions). Although time-resolved detection of such dynamics is essential, these dynamics have been very difficult to track by traditional spectroscopic techniques. Here, relatively new approaches for probing the dynamics of protein photochemical reactions using time-resolved transient grating (TG) are reviewed. By using this method, a variety of spectrally silent dynamics can be detected and such data provide a valuable description about the reaction scheme. Herein, a blue light sensor protein TePixD is the exemplar. The initial photochemistry for TePixD occurs around the chromophore and is detected readily by light absorption, but subsequent reactions are spectrally silent. The TG experiments revealed conformational changes and changes in inter-protein interactions, which are essential for TePixD function. The TG experiments also showed the importance of fluctuations of the intermediates as the driving force of the reaction. This technique is complementary to optical absorption detection methods. The TG signal contains a variety of unique information, which is difficult to obtain by other methods. The advantages and methods for signal analyses are described in detail in this review.