• Title/Summary/Keyword: solid phase method

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Comparison Solid Phase Microextraction with Purge & Trap on the GC/MS Analysis of Volatile Organic Compounds in Biota Samples (Solid Phase Microextraction 및 Purge & Trap을 이용한 생물시료 중 휘발성 유기화합물의 GC/MS 분석비교)

  • Ahn, Yun-Gyong;Seo, Jong-Bok;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.392-399
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    • 2001
  • The analysis of n-butylbenzene and 1,2-dibromo-3-chloropropane (DBCP) as volatile organic compounds in biota samples was performed by gas chromatography/mass spectrometry-selected ion monitoring mode. The target compounds, n-butylbenzene and DBCP, in biota samples were extracted by headspace solid phase microextraction (SPME) with $100{\mu}m$ polydimethyl siloxane (PDMS) fiber and purge & trap method. The extraction recoveries of these compounds obtained by SPME was 85.8% for n-butylbenzene and 92.4% for DBCP, respectively. Each value of method detection limit were $0.15{\mu}g/kg$ and $0.05{\mu}g/kg$, respectively. While in the case of purge & trap method, the extraction recovery was 115.2% for n-butylbenzene, 80.9% for DBCP and method detection limit were $0.04{\mu}g/kg$ and $0.70{\mu}g/kg$, respectively. The extraction yields and detection limits of these compounds obtained by purge & trap were equivalent to those by SPME.

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Analysis of oligosaccharides from Panax ginseng by using solid-phase permethylation method combined with ultra-high-performance liquid chromatography-Q-Orbitrap/mass spectrometry

  • Li, Lele;Ma, Li;Guo, Yunlong;Liu, Wenlong;Wang, Yang;Liu, Shuying
    • Journal of Ginseng Research
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    • v.44 no.6
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    • pp.775-783
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    • 2020
  • Background: The reports about valuable oligosaccharides in ginseng are quite limited. There is an urgent need to develop a practical procedure to detect and analyze ginseng oligosaccharides. Methods: The oligosaccharide extracts from ginseng were permethylated by solid-phase methylation method and then were analyzed by ultra-high-performance liquid chromatography-Q-Orbitrap/MS. The sequence, linkage, and configuration information of oligosaccharides were determined by using accurate m/z value and tandem mass information. Several standard references were used to further confirm the identification. The oligosaccharide composition in white ginseng and red ginseng was compared using a multivariate statistical analysis method. Results: The nonreducing oligosaccharide erlose among 12 oligosaccharides identified was reported for the first time in ginseng. In the comparison of the oligosaccharide extracts from white ginseng and red ginseng, a clear separation was observed in the partial least squares-discriminate analysis score plot, indicating the sugar differences in these two kinds of ginseng samples. The glycans with variable importance in the projection value large than 1.0 were considered to contribute most to the classification. The contents of oligosaccharides in red ginseng were lower than those in white ginseng, and the contents of maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose, maltoheptaose, maltooctaose, maltononaose, sucrose, and erlose decreased significantly (p < 0.05) in red ginseng. Conclusion: A solid-phase methylation method combined with liquid chromatography-tandem mass spectrometry was successfully applied to analyze the oligosaccharides in ginseng extracts, which provides the possibility for holistic evaluation of ginseng oligosaccharides. The comparison of oligosaccharide composition of white ginseng and red ginseng could help understand the differences in pharmacological activities between these two kinds of ginseng samples from the perspective of glycans.

Preparation and Controlled Release of Microcapsules Containing $Ketoprofen-{\beta}-Cyclodextrin$ Solid Dispersion (케토프로펜-${\beta}$-시클로덱스트린 고체분산체의 마이크로캅셀화 및 제어 방출)

  • Chun, In-Koo;Park, Jung-Hwa
    • Journal of Pharmaceutical Investigation
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    • v.22 no.1
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    • pp.33-40
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    • 1992
  • This study was aimed to control the release characteristics of ketoprofen by microencapsulating $ketoprofen-{\beta}-cyclodextrin\;(KF-{\beta}-CyD)$ solid dispersion with Eudragit RS by the phase separation method using a nonaqueous vehicle. KF alone was also microencapsulated with Eudragit RS by the evaporation process in water phase. The results obtained showed that it was not possible to microencapsulate KF alone by phase separation in a chloroform-cyclohexane system while it was easy to microencapsulate $(KF-{\beta}-CyD)$ solid dispersion system. For the microcapsules, the release test was performed in the first fluid (pH 1.2) and the second fluid (pH 6.8) of K.P.V disintegration medium at $37^{\circ}C$. The release of KF from $(KF-{\beta}-CyD)$ solid dispersion microcapsules (1:1 core wall ratio) was more sustained than that from KF microcapsules, and followed zero-order kinetics. Especially, solid dispersion microcapsules showed pH-independent release patterns with higher wall to core ratio (1:1 w/w).

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Effects of Chemical Inhomogeneity on Phase Coexistence in Pb(Zr, Ti))$O_3$ Ceramics at Morphotropic Tetragonal and Rhombohedral Phase Boundary (정방정상과 능면체상의 경계조성 Pb(Zr, Ti)$O_3$ 세라믹스에서 화학조성의 불균일성이 상공존에 미치는 영향)

  • 천채일;김호기
    • Journal of the Korean Ceramic Society
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    • v.27 no.8
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    • pp.1027-1033
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    • 1990
  • In order to identify the origin of phase coexistence at morphotropic tetragonal and rhombohedral boundary in PZT ceramics, the effect of chemical inhomogeneity on phase coexistence region was investigated. Two kinds of PZT ceramics with different chemical homogeneity were prepared by conventional solid state reaction and co-precipitation method. There was coexistence of tetragonal and rhombohedral phase over a wide composition range in PZT ceramics calcined by solid state reaction, and there was also phase coexistence of which region was reduced considerably in sintered samples. And phase coexistence region was not observed in co-precipitated PZT ceramics(within 1 mole%). Therefore compositional fluctuation is considered to be major origin of the phase coexistence at morphotropic phae boundary in PZT ceramics.

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Development of Light Transmission Fluctuation for Particle Measurement in Solid-Gas Two Phase Flows

  • YANG, Bin;WANG, Zhan-ping;HE, Yuan;CAI, Xiao-Shu
    • Particle and aerosol research
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    • v.12 no.1
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    • pp.21-26
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    • 2016
  • In order to realize In-line and convenient measurement for solid-gas two phase flows, Light Transmission Fluctuation (LTF) based on the random variation of transmitted light intensity, light scattering theory and cross-correlation method was presented for online measurement of particle size, concentration and velocity. The statistical relationship among transmitted light intensity, particle size and particle number in measurement zone was described by Beer-Lambert Law. Accordingly, the particle size and concentration were determined from the fluctuation signal of transmitted light intensity. Simultaneously, the particle velocity was calculated by cross-correlation analysis of two neighboring light beams. By considering the influence of concentration variation in industrial applications, the improved algorithm based on spectral analysis of transmitted light intensity was proposed to improve measurement accuracy and stability. Therefore, the online measurement system based on LTF was developed and applied to measure pulverized coal in power station and raw material in cement plant. The particle size, concentration and velocity of powder were monitored in real-time. It can provide important references for optimal control, energy saving and emission reduction of energy-intensive industries.

Research of liquid-solid two phase flow in centrifugal pump with crystallization phenomenon

  • Liu, Dong;Wang, Ya-Yun;Wang, Ying-Ze;Wang, Chun-Lin;Yang, Min-Guan
    • International Journal of Fluid Machinery and Systems
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    • v.7 no.2
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    • pp.54-59
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    • 2014
  • Particle Image Velocimetry combined with developed image processing method is adopted to study the liquid-solid two phase flow in the centrifugal pump impeller with crystallization phenomenon. The tracer particle is used to follow the liquid phase, which has the diameter between 8 to $12{\mu}m$. The crystal particle precipitates from the sodium sulfate solution does change the wavelength of the laser, and which has great laser scattering characteristics. The diameter of the crystal particle is larger than $20{\mu}m$. Through calculating the diameter of the particles in the image, the tracer particle and the crystal particle can be distinguished. By analyzing the experimental result, the following conclusion has been obtained. During the delay period, there is not any crystal particle and the pump performance has not been changed. As the crystallization process begins, the crystal nuclei appears from the supersaturation solution and grows larger with temperature decreasing, which has the tendency of moving towards the pressure side. The characteristics of liquid-solid two phase flow with crystallization phenomenon in the pump are obtained according to analysis of experimental results, and some guiding advices are presented to mitigate the crystallization phenomenon in pump impeller.

TRANSIENT SIMULATION OF SOLID PARTICLE DISTRIBUTION WITH VARIOUS DESIGN PARAMETERS OF THE BAFFLE IN A STIRRED TANK (배플 형상에 따른 교반기 내부 고체입자 분포의 비정상상태 해석)

  • Kim, Chi-Gyeom;Lee, Seung-Jae;Won, Chan-Shik;Hur, Nahm-Keon
    • Journal of computational fluids engineering
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    • v.14 no.4
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    • pp.1-6
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    • 2009
  • In the present study, numerical simulations were performed in a stirred solid/liquid system by using Eulerian multi-phase model. The transient flow field of liquid and distribution of solid particles were predicted in the stirred tank with pitched paddle impeller and baffles. The Frozen rotor method is adopted to consider the rotating motion of the impeller. The effects of number and width of baffles on the mixing time and the quality of solid suspension in the stirred tank are presented numerically. The result shows that the mixing time decreases as the width and number of baffles increase. The present numerical methodology can be applied to optimizing mixing condition of industrial mixer.

Determination of Grayanotoxin I and Grayanotoxin III in mad honey from Nepal using liquid chromatography-tandem mass spectrometry

  • Ahn, Su Youn;Kim, Suncheun;Cho, Hwangeui
    • Analytical Science and Technology
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    • v.35 no.2
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    • pp.82-91
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    • 2022
  • Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquid-chromatography-tandem-mass-spectrometric method (LC-MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 ㎍/g. The intra- and inter-day deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 - 64.86 ㎍/g and 0.25 - 63.99 ㎍/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.

Densification of Cu-50%Cr Powder Compacts and Properties of the Sintered Compacts (Cu-50%Cr 분말성형체의 치밀화 및 소결체 물성)

  • 김미진;정재필;도정만;박종구;홍경태
    • Journal of Powder Materials
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    • v.7 no.4
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    • pp.218-227
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    • 2000
  • It is well known that the Cu-Cr alloys are very difficult to be made by conventional sintering methods. This difficulty originates both from limited solubility of Cr in the Cu matrix and from limited sintering temperature due to high vapor pressures of Cr and Cu components at the high temperature. Densification of Cu-50%Cr Powder compacts by conventional Powder metallurgy Process has been studied. Three kinds of sintering methods were tested in order to obtain high-density sintered compacts. Completely densified Cu-Cr compacts could be obtained neither by solid state sintering method nor by liquid phase sintering method. Both low degree of shrinkage and evolution of large pores in the Cu matrix during the solid state sintering are attributed to the anchoring effect of large Cr particles, which inhibits homogeneous densification of Cu matrix and induces pore generation in the Cu matrix. In addition, the effect of undiffusible gas coming from the reduction of Cu-oxide and Cr-oxide was observed during liquid phase sintering. A two-step sintering method, solid state sintering followed by liquid phase sintering, was proved to have beneficial effect on the fabrication of high-dendsity Cu-Cr sintered compacts. The sintered compacts have properties similar to those of commercial products.

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Spectrometric Determination of Rhodamine B in Chili Powder After Molecularly Imprinted Solid Phase Extraction

  • Liu, Xiuying;Zhang, Xuan;Zhou, Qian;Bai, Bing;Ji, Shujuan
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3381-3386
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    • 2013
  • This paper reports a method using molecularly imprinted polymers that are grafted onto the surface of carboxyl-modified multi-walled carbon nanotubes as the solid-phase extraction adsorbents to detect Rhodamine B in chili powder samples. The polymers were characterized by FTIR and TGA. Various parameters which probably influence efficiency of extraction were optimized. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions. And the proposed method was applied to analysis of Rhodamine B in chili powder samples. The limits of detection and quantification were 2.57 and 8.56 ${\mu}g/g$, respectively. The recoveries for analytes were higher than 95% and relative standard deviation values were found to be in the range of 0.83-4.15%. This method was successfully applied for the determination of Rhodamine B.