• Title/Summary/Keyword: Chromatographic methods

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A Review on the Sampling and Analytical Methods for Ammonia in Air

  • Das, Piw;Kim, K.H.;Sa, J.H.;Kim, J.C.;Lee, S.R.;Jeon, E.C.
    • Journal of the Korean earth science society
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    • v.28 no.5
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    • pp.572-584
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    • 2007
  • The quantification of ammonia concentrations has received a lot of scientific attention. Numerous devices for the quantification of $NH_3$ in the ambient air have been developed to provide more technical possibilities for research in abating $NH_3$ emission from various source processes. For the proper quantification of $NH_3$, a number of sampling methods have been discussed by grouping them into different categories based on the principle of functioning. In general, active samplers employ pumps to draw air in, while passive samplers are exposed to air over a certain period of time to obtain integrated signature of $NH_3$. In case of the former, impingers and absorption flasks can be employed simultaneously with suitable absorbents to capture $NH_3$ passing through them. The methods of analysis include both in-situ and laboratory determination. In the laboratory, colorimetric or ion chromatographic methods are generally used for its quantification. In the field, a number of real time analyzers have been proven to be useful. These real time analyzers can be grouped according to their principle of operation. These analyzers may use the principle of spectroscopy (e.g. DOAS), photoacousticics (e.g. photoacoustic monitor) or Chemiluminescence ($NO_x$ analyzer). The automated annular denuder sampling system with on-line analyzer is also suitable for continuous monitoring of ammonia in air.

A Study on the Prediction of the Octane Number of Gasolines from the Carbon Type Structural Compositions by 13C-Nuclear Magnetic Resonance Spectroscopy (13C-NMR에 의해 결정된 탄소 유형별 구조적 조성으로부터 가솔린 옥탄가의 예측에 관한 연구)

  • Choi, Ju-Hwan;Chun, Yong-Jin;Choi, Ung-Su;Choi, Young-Sang;Kwon, Oh-Kwan
    • Applied Chemistry for Engineering
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    • v.4 no.4
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    • pp.753-759
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    • 1993
  • The research and motor octane numbers (RON & MON, respectively) of a gasoline are dynamic measures of its quality of performance as a fuel. ASTM standard engine test methods (RON:ASTM D-2699, MON:ASTM D-2700) have been used for determining the octane numbers (RON,MON)of gasolines. But these methods have been widely criticized because their repeatability and reproducibility of the test method are very poor. In addition to these objections, the cost and operation time involved in measuring by the standard method led to searches for "non -engine" methods (Gas Chromatographic method, Nuclear Magnetic Resonance Spectroscopic method). In this study, we determined the carbon type structural compositions of the gasolines by $^{13}C-NMR$ spectroscopy and predicted the octane number (RON & MON) with good accuracy. we presented an assessment of the effects of molecular structural composition on octane numbers.

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DETECTION OF PHYSIOLOGICAL PROCESSES IN WHEAT BY NIR

  • Salgo, A.;Gergely, Sz.;Scholz, E.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1158-1158
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    • 2001
  • Fast and dynamic biochemical, enzymatic and morphological changes occur during the so-called generative development and during the vegetative processes in seeds. The most characteristic biochemical and compositional changes of this period are the formation and decline of storage components or their precursors, the change of their degree in polymerization and an extensive change in water content. The aim of the present study was to detect the maturation processes in seed nondestructively and to verify the applicability of near infrared spectroscopic methods in the measurement of physiological, chemical and biochemical changes in wheat seed. The amount and variation of different water “species” has been changed intensively during maturation. Characteristic changes of three water absorption bands (1920, 1420 and 1150 nm) during maturation were analysed. It was concluded that the free/bound transition of water molecules could be followed sensitively in different region of NIR spectra. Kinetic changes of carbohydrate reserves were characteristic during maturation. An intensive formation and decline of carbohydrate reserves were observed during early stage of maturation (0 -13 days, high energy demand). An accelerated formation of storage carbohydrates (starch) was detected in the second phase of maturation. Five characteristic absorption bands were analysed which were sensitive indicators the changes of carbohydrates occurred during maturation. Precursors of protein synthesis and the synthesis of reserve proteins and their kinetic changes during maturation were followed from NIR spectra qualitative and qualitatively. Dynamic formation of amino acids and the changes of N forms were detected by spectroscopic, chromatographic and by capillary electrophoresis methods. Calibration equations were developed and validated in order to measure the optimal maturation time protein and moisture content of developing wheat seeds. The spectroscopic methods are offering chance and measurement potential in order to detect fine details of physiological processes. The spectra have many hidden details, which can help to understand the biochemical background of processes.

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A Comparison of Sonication and Microwave-assisted Extraction Method for Speciation of Arsenic in Fish Tissue, DORM-2 (어류중 비소의 종분화 분석을 위한 초음파 추출법과 마이크로파 추출법의 비교)

  • Yoon, Cheol-Ho;Park, Yong-Chul;Hong, Jong-Ki
    • Analytical Science and Technology
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    • v.16 no.2
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    • pp.134-142
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    • 2003
  • Comparison of a microwave-assisted extraction with sonication extraction was performed for arsenic speciation in fish tissue with chromatographic separation and inductively coupled plasma mass spectrometry detection. The detection limits of arsenicals with ultrasonic nebulizerand cross-flow nebulizer were shown to be similar. The arsenicals investigated were arsenobetaine (AsB), arsenite [As(III)], dimethylarsine acid (DMA), monomethylarsonic acid (MMA), arsenate [As(v)], and phenylarsonic acid (PAA). Quantitative extraction of arsenicals from dogfish muscle, DORM-2, standard reference material of NRCC (National Research Council of Canada) was achieved using 50% (v/v) methanol-water in both extraction methods. Extraction efficiency of arsenobetaine in both methods is greater than 82% with RSDs on replicates of less than 5%. The concentrations of AsB determined in extract of microwave assisted extraction and sonication methods were $14.18{\pm}0.42mg\;kg^{-1}$ and $13.54 {\pm}0.84mg\;kg^{-1}$, respectively. And the concentrations of DMA were $0.45{\pm}0.06mg\;kg^{-1}$ and $0.44{\pm}0.06mg\;kg^{-1}$, respectively.

A Study on the Analysis of Isothiazolinone Components by High Performance Liquid Chromatography (고성능액체크로마토그래피에 의한 Isothiazolinone Components의 분석에 관한 연구)

  • 김종규;이덕희
    • Journal of Environmental Health Sciences
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    • v.18 no.2
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    • pp.102-105
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    • 1992
  • Introduction : Isothiazolinone product is one of new preservatives used in cooling tower, paper mill, and general industrial waters.l) It is also effective in controlling bacteria and fungi in the manufacture and storage of dispersed pigments, such as kaolin clays, titanium dioxide, calcium carbonate and others\ulcorner Its broad-spectrum activity, excellent physical and chemical compatibility with anionic, nonionic and cationic surfactants and most organic and inorganic compounds and low toxicity at recommended use levels provide formulators with an effective, economical, and environmentally acceptable alternative to other commercial biocides. It dose not contain or generate formaldehyde and is easy to formulate (1.5% solution is supplied as an aqueous solution), so that it gains advantage over the other preservatives. The active ingredients of the isothiazolinone product are unchlorinated compound (2-methyl-4-isothiazolin-3-one) and chlorinated one (5-chloro-2-methyl-4-isothiazolin-3-one). Methods preferred for the analysis of preservatives are chromatographic methods, especially high performance liquid chromatograph (HPLC). Although several methods were satisfactory in respect to separation, no offical method has been published for the isothiazolinone components. This study was performed to search for an alternative method in order to show flexible operating conditions of HPLC and to reduce assay time.

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Impurity profiling and chemometric analysis of methamphetamine seizures in Korea

  • Shin, Dong Won;Ko, Beom Jun;Cheong, Jae Chul;Lee, Wonho;Kim, Suhkmann;Kim, Jin Young
    • Analytical Science and Technology
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    • v.33 no.2
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    • pp.98-107
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    • 2020
  • Methamphetamine (MA) is currently the most abused illicit drug in Korea. MA is produced by chemical synthesis, and the final target drug that is produced contains small amounts of the precursor chemicals, intermediates, and by-products. To identify and quantify these trace compounds in MA seizures, a practical and feasible approach for conducting chromatographic fingerprinting with a suite of traditional chemometric methods and recently introduced machine learning approaches was examined. This was achieved using gas chromatography (GC) coupled with a flame ionization detector (FID) and mass spectrometry (MS). Following appropriate examination of all the peaks in 71 samples, 166 impurities were selected as the characteristic components. Unsupervised (principal component analysis (PCA), hierarchical cluster analysis (HCA), and K-means clustering) and supervised (partial least squares-discriminant analysis (PLS-DA), orthogonal partial least squares-discriminant analysis (OPLS-DA), support vector machines (SVM), and deep neural network (DNN) with Keras) chemometric techniques were employed for classifying the 71 MA seizures. The results of the PCA, HCA, K-means clustering, PLS-DA, OPLS-DA, SVM, and DNN methods for quality evaluation were in good agreement. However, the tested MA seizures possessed distinct features, such as chirality, cutting agents, and boiling points. The study indicated that the established qualitative and semi-quantitative methods will be practical and useful analytical tools for characterizing trace compounds in illicit MA seizures. Moreover, they will provide a statistical basis for identifying the synthesis route, sources of supply, trafficking routes, and connections between seizures, which will support drug law enforcement agencies in their effort to eliminate organized MA crime.

Determination of oxymatrine in Sophora Radix by High Performance Liquid Chromatography (고성능 액체 크로마토그래피를 이용한 고삼 중의 oxymatrine 분석에 관한 연구)

  • Yang, Seung Kwon;Yun, Young Ja;Namgung, Mi Ok
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.289-294
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    • 2004
  • A high performance liquid chromatographic method was designed for the quantitative analysis of oxymatrine in Sophora Radix. The separation of oxymatrine was performed by reversed-phase chromatography with a $C_{18}$ column and a buffered aqueous solution containing acetonitrile, and monitored by UV absorption at 215 nm. Extraction of oxymatrine in Sophora Radix was carried out using various solvents and extraction methods. The optimum extraction efficiency for the crushed Sophora Radix was achieved by reflux at $80^{\circ}C$ in 50% ethanol for five hours. Most extraction methods used to complicate pretreatments. In this study, sublimation was employed for a extraction method without going through complicate pretreatments. Sublimation was carried out under high vacuum ($1{\times}10^{-3}$ torr) and at high temperature ($200^{\circ}C$). Extraction efficiency using Sublimation was found to be inferior to other extraction methods.

Headspace Analysis for Residual Hexane in Vegetable Oil

  • Oh, Chang-Hwan;Kwon, Yong-Kwan;Jang, Young-Mi;Lee, Dal-Su;Park, Jong-Sei
    • Food Science and Biotechnology
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    • v.14 no.4
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    • pp.456-460
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    • 2005
  • To enforce the maximum residue limit for residual hexane (0.005 g/kg) in commercially available Korean vegetable oil, convenient and accurate quantification methods were investigated. Using dual surrogate standards, pentane and heptane were dissolved in ethanol, and then added to hexane-tree sunflower oil for setting up the calibration curve. Gas Chromatograph-Flame Ionization Detector with a porous layer open tubular column, indicated good chromatographic separation of hexane from other inhibiting matrix components. The lowest calibration level was $0.5\;{\mu}g/g$, not exceeding a relative standard deviation of 10% (RSD%), and 1.0\;{\mu}g/g$ not exceeding a deviation of 22% RSD% using heptane as an internal standard for the Static headspace analysis by using a headspace auto-sampler and manual injection, respectively. The residual hexane was detected in nine of the samples among 87 vegetable oil samples purchased on the local market.

Analysis of Nodakenetin from Samultangs Fermented by Lactose Bactera Strains (유산균 발효에 의한 사물탕들부터 노다케네틴의 분리 및 함량분석)

  • Kim, Dong-Seon;Roh, Joo-Hwan;Cho, Chang-Won;Ma, Jin-Yeul
    • The Korea Journal of Herbology
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    • v.27 no.1
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    • pp.35-39
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    • 2012
  • Objectives : The purpose of this study was to investigate the changes in the contents of constituents in Samultang and its fermentations with 10 species of lactic acid bacteria. Methods : Ten strains of lactic acid bacteria, Lactobacillus casei, L. acidophilus, L. casei, L. plantarum, L. amylophilus, L. curvatus, L. delbruekil subsp. lactis, L. casei, B. breve, and B. thermophilum, were used for the fermentation of Samultang. The increased and decreased constituents were identified using HPLC/DAD and various liquid chromatographic techniques, and the structure was elucidated using NMR and MS. These compounds were quantitatively analyzed using an HPLC/DAD system. Results : A remarkably increased component was identified to be nodakenetin and a decreased component was determined to be nodakenin. The fermentation of the ten lactic acid bacteria demonstrated that the decomposable rate of these two compounds in fermented Samultang were different. Samultang fermented by L. plantarum showed the most remarkable changes. Conclusion : Nodakenetin was identified as bioconversion component after fermentation and L. plantarum was discovered the best bacteria to increase the component.

Inhibitory Effects of Quinoline Isolated from Ruta chalepensis and Its Structurally Related Derivatives against α-Amylase or α-Glucosidase

  • Park, Jun-Hwan;Lee, Hoi-Seon
    • Journal of Applied Biological Chemistry
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    • v.58 no.1
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    • pp.5-8
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    • 2015
  • This study was to isolate an active component of the chloroform fraction from the methanol extract of Ruta chalepensis leaves and to measure inhibitory effects against ${\alpha}$-glucosidase or ${\alpha}$-amylase. The inhibitory compound of R. chalepensis leaves was isolated using chromatographic methods and identified as quinoline. Quinoline and its structurally related derivatives were tested for their inhibitory activities by evaluating the $IC_{50}$ values against ${\alpha}$-amylase or ${\alpha}$-glucosidase and were compared with that of acarbose. Based on the $IC_{50}$ values, quinazoline exhibited the greatest inhibitory activity ($20.5{\mu}g/mL$), followed by acarbose ($66.5{\mu}g/mL$), and quinoline ($80.3{\mu}g/mL$) against ${\alpha}$-glucosidase. In case of ${\alpha}$-amylase, quinazoline had potent inhibitory activity, followed by quinoline ($179.5{\mu}g/mL$) and acarbose ($180.6{\mu}g/mL$). These results indicate that R. chalepensis extract, quinoline, and quinazoline could be useful for inhibiting ${\alpha}$-glucosidase or ${\alpha}$-amylase.