• Title/Summary/Keyword: mobile phase

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Comparison of Anthocyanin Content in Seed Coats of Black Soybean [Glycine max(L.) Merr.] Cultivars Using Liquid Chromatography Coupled to Tandem Mass Spectrometry

  • Shin, Sung-Chul;Lee, Soo-Jung;Lee, Sung-Joong;Chung, Jong-Il;Bae, Dong-Won;Kim, Soo-Taek;Sung, Nak-Ju
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1470-1475
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    • 2009
  • The seed coat of the black soybean contains 3 main anthocyanins such as delphinidin-3-O-$\beta$-glucoside, cyanidin-3-O-$\beta$-glucoside, and petunidin-3-O-$\beta$-glucoside. As a part of our effort on discovering and breeding new black soybean cultivars which possesses specific anthocyanin component rich, we determined the anthocyanin profiles of the 2 cultivars recently developed soybean cv. Gaechuck #1 and cv. Gyeongsang #1, using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and compared their content and identity with those of previously known 10 cultivar controls. The Cosmosil-$5C_{18}$-AR-II column were selected for the analysis because of the best peak separation. The column temperature was set up at $35^{\circ}C$. The mobile phase consisting of water containing 0.5%(v/v) formic acid and methanol gave good separation between the 3 anthocyanin analytes and internal standard (quercetin 3-O-$\beta$-rutinoside) and peaks with suppressed tail. The MS/MS spectra of each individual anthocyanin standard were detected in positive electron spray ionization (ESI) modes. It was disclosed that the anthocyanin contents of the soybean cv. Gaechuck#1 and cv. Gyeongsang#1 are roughly higher than those of the 10 controls.

HPLC를 이용한 축육(Pork Muscle)내의 Dihydrostreptomycin 검출법

  • Choe, Ji-Hyeon;Han, Eun-Yeong;Park, Jin-Gwan;Lee, Su-Yeon;Choe, Dong-Mi;Sin, Ho-Cheol;Lee, Chi-Ho
    • Proceedings of the Korean Society for Food Science of Animal Resources Conference
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    • 2005.10a
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    • pp.196-203
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    • 2005
  • 축산식품 고기내의 잔류항생물질을 신속하고 간편하고 정확하게 분석하기 위한 시험법 개발 을 목적으로 하였다. 축산식품내의 일반적인 잔류항생물질에 대한 지금까지의 분석법으로는 Bioassay법, TLC법, ELISA법, GC법 및 HPLC법 등이 있지만 Streptomycin/Dihydro streptomycin, Neomycin에 대한 HPLC법은 거의 확립되어 있지 않은 실정이다. 우리나라의 공인 검사법으로는 Bioassay법 및 HPLC법 등이 있지만 그러나 지금까지의 방법으로는 검출감도가 낮은 것이 큰 문제점으로 되어 왔다. 본 연구에서는 DST에 대한 HPLC법에 대한 보고한 P. Edder 방법 중에 clean-up과정 및 이동상 조건을 대폭 수정하여 DST의 분리 및 검출감도를 낮추려고 시도하였다. 본 연구에 사용된 유도체화 장치 Post-Column Derivatization Instrument PCX 5100 (Pickering Laboratories, Inc.)의 컬럼온도는 $40^{\circ}C$, 오븐온도 $55^{\circ}C$, reagent 유속 0.6ml/min mobile phase 유속 0.8ml/min으로 검출기는 형광검출기를 이용하여 DST 검출에 대해 만족할 만한 결과를 얻었다. 이때의 분석소요시간은 약 15분이었다. 표준시료 DST의 검량선은 넓은 농도범위(0.02${\sim}$1.0ppm)에서 양호한 직선성을 나타냈다. 본 시험법에 의한 검출한계는 limit of detection (LOD)은 0.02ppm이었으며, 적어도 고기에서의 MRL이 0.6ppm임을 감안하면 DST를 정량적으로 정도 좋게 측정할 수 있다는 것을 확인했다. 상기의 조건하에서 실제시료인 고기에 표준 DST를 1ppm을 spiking한 후 SPE상에서 SCX(Strong cation exchange column)을 통한 clean-up과정을 거친 후의 DST의 limit of quantification(LOQ)는 약 0.47ppm이었으며, 이에 대한 회수율은 97.7%(n= 8)를 나타냈다. 실제 codex에서 권장한 고기의 MRL이 0.6ppm인 점을 감안하면 codex 권고치에 도달할 수 있는 것으로 판단되었다. 따라서 본 연구에서 개발된 시험법은 지금까지 국내적으로 DST에 대한 시험법이 확립되어 있지 않은 것으로 이와 아울러 간편한 parallux와 병용해 DST에 대한 정량 및 정성 분석을 유도체화 장치 및 형광검출기를 이용해 잔류항생물질 DST에 대한 분석시험법의 개발이 가능하다고 여겨진다.

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Separation Characteristics of Ibuprofen in Kromasil HPLC Column (Kromasil HPLC 칼럼을 이용한 Ibuprofen의 분리특성 연구)

  • Park Joon Sub;Kim Byung Lip;Yoon Tae Ho;Kim In Ho
    • KSBB Journal
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    • v.20 no.3
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    • pp.244-249
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    • 2005
  • Chiral separation of racemic ibuprofen was achieved on a Kromasil KR100-5CHI-TBB column. Some chromatographic parameters (resolution, number of theoretical plates, HETP, capacity factor) are calculated under different separation conditions such as change of mobile phase compositions (hexane / t-BME : 85 / 15, 75 / 15, 65 / 35, 55 /45) as well as acetic acid concentrations for adjusting pH (0.1 to 1 $v/v\%$). Flow rate versus number of theoretical plates and HETP were compared to evaluate column efficiency. To determine the adsorption isotherms, PIM (Pulsed Input Method) was carried out. At concentrations of racemic ibuprofen between 0.1 and 0.3 mg/ml, S- and R-ibuprofen have the same retention time of 4.48 and 5.81 min. Ibuprofen isotherms show a linear form under concentrations of 0.3 mg/ml with eluent (hexane / t-BME = 55 / 45).

Epidemic Reliable Multicast by Peer Collaborations in Wireless Tactical Networks (무선 전술 네트워크에서 단말의 협력을 통한 전염 기반의 신뢰성 있는 멀티캐스트)

  • Hong, Min-Ki;Kang, Kyung-Ran;Cho, Young-Jong
    • The Journal of Korean Institute of Communications and Information Sciences
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    • v.33 no.10B
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    • pp.865-875
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    • 2008
  • In this paper, we propose a reliable multicast scheme for the tactical wireless ad hoc network where the members share the situation and operation data. Our scheme consists of two phases to guarantee the reliability. During the dissemination phase, we utilizes an epidemic approach similar to gossip-based ad hoc routing. Then the group members interchange the message reception state information periodically so that they are able to recover missing packets from the other members. We evaluate the performance of our scheme through extensive simulations using the network simulator in comparison with other existing reliable multicast schemes in mobile ad hoc network. Our scheme shows higher packet delivery ratio regardless of the mobility and imposes much lower control overhead to the non-group members compared with the existing schemes.

A Study on Adaptive Linear MMSE Detector for DS-CDMA Reverse Link in Rayleigh Fading Environment (레일리 페이딩 환경하에서 DS-CDMA 역방향 링크에 적용 가능한 적응 선형 MMSE 수신기의 연구)

  • 안태기;이병섭;김성락;이정구
    • The Journal of Korean Institute of Electromagnetic Engineering and Science
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    • v.9 no.2
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    • pp.131-140
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    • 1998
  • MAI(Multi-Access Interference) and fast channel variation due to the fading environment are the major problems in the mobile CDMA communication systems. Recently, interest has been increasing in applying the Adaptive Linear MMSE Detector to MAI cancellation in the CDMA reverse link. In this paper, we propose a modified Adaptive Linear MMSE Detector structure which can be used in Long-duration code CDMA system in the presence of independent Rayleigh fading. We use independent multiple tap-weight vector structure to cope with the variation of spreading sequence pattern between neighbor symbols because of the Long-duration code. In this case, more exact channel parameter estimation is required. To solve this problem, we use coherent CDMA structure which can track the channel parameters like amplitude and phase by employing the low power pilot channel in the CDMA reverse link.

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Stabilization of Nickel-Rich Layered Cathode Materials of High Energy Density by Ca Doping (칼슘 도핑을 통한 고 에너지 밀도를 가지는 Ni-rich 층상 구조형 양극 소재의 안정화)

  • Kang, Beomhee;Hong, Soonhyun;Yoon, Hongkwan;Kim, Dojin;Kim, Chunjoong
    • Korean Journal of Materials Research
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    • v.28 no.5
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    • pp.273-278
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    • 2018
  • Lithium-ion batteries have been considered the most important devices to power mobile or small-sized devices due to their high energy density. $LixCoO_2$ has been studied as a cathode material for the Li-ion battery. However, the limitation of its capacity impedes the development of high capacity cathode materials with Ni, Mn, etc. in them. The substitution of Mn and Ni for Co leads to the formation of solid solution phase $LiNi_xMn_yCo_{1-x-y}O_2$ (NMC, both x and y < 1), which shows better battery performance than unsubstituted $LiCoO_2$. However, despite a high discharge capacity in the Ni-rich compound (Ni > 0.8 in the metal site), poor cycle retention capability still remains to be overcome. In this study, aiming to improve the stability of the physical and chemical bonding, we investigate the stabilization effect of Ca in the Ni-rich layered compound $Li(Ni_{0.83}Co_{0.12}Mn_{0.05})O_2$, and then Ca is added to the modified secondary particles to lower the degree of cationic mixing of the final particles. For the optimization of the final grains added with Ca, the Ca content (x = 0, 2.5, 5.0, 10.0 at.%) versus Li is analyzed.

Computation of Ionic Conductivity at NASICON Solid Electrolytes (II) Effects of mid-Na Sites on Na1-Na2 Conduction Paths (NASICON 고체 전해질의 이온 전도도 계산 (II) Na1-Na2 전도 경로에 미치는 mid-Na의 영향)

  • 최진삼;서양곤;강은태
    • Journal of the Korean Ceramic Society
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    • v.32 no.11
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    • pp.1292-1300
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    • 1995
  • The ionic conductivity of NASICON solid electrolytes was simulated by using Monte Carlo Method (MCM). There were included two conduction paths: (1) Na1-Na2 and (2) Na1-Na2 including Na2-Na2. We assumed that mid-Na ions provde an additional driving force for Na mobile ions due to the interionic repulsion between Na1 and Na2 ions. The inflection point of vacancy availability factor, V has been shown at nearby x=2, the maximum mid-Na ions. The inflection point of vacancy availability factor, V has been shown at nearby x=2, the maximum mid-Na sites are occupied. The effective jump frequency factor, V has been shown at nearby x=2, the maximum mid-Na sites are occupied. The effective jump frequency factor, W increased rapidly with the composition at low temperature, but decreased at high temperature region. On Na1-Na2 conduction path, the minimum of charge correlation factor, fc and the maximum of $\sigma$T were appeared at x=2.0. this indicated that mid-Na ions affect on the high ionic conductivity behavior. At the whole range of NASICON composition, 1n $\sigma$T vs. 1/T* plots have been shown Arrhenius behavior but 1n (VWFc) vs. 1/T* have been shown the Arrhenius type tendency at x=2, which mid-Na is being the maximum. The results of MCM agreed with the experimental one when the chosen saddle point value was 6$\varepsilon$ : 3$\varepsilon$. Here the calculated characteristic parameter of materials, K and the phase transition temperature were -4.001$\times$103 and 178$^{\circ}C$ (1/T*=1.92, 1000/T=2.22), respectively.

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Quantitative Analysis of the Eleven Marker Components in Traditional Korean Formula, Jakyakgamcho-Tang Decoction Using an Ultra-Performance Liquid Chromatography Coupled to Electrospray Ionization Tandem Mass Spectrometry (UPLC-MS/MS를 이용한 작약감초탕 물 추출물 중 11종 성분의 함량분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • YAKHAK HOEJI
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    • v.60 no.2
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    • pp.64-72
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    • 2016
  • Jakyakgamcho-tang is a well-known traditional herbal medicine and has been used for the treatment of mainly pains in oriental medicine. In this study, analytical method for the quantitative determination of the eleven marker components, gallic acid (1), oxypaeoniflorin (2), paeoniflorin (3), albiflorin (4), liquiritin (5), isoliquiritin (6), ononin (7), liquiritigenin (8), benzoylpaeoniflorin (9), paeonol (10), and glycyrrhizin (11) in Jakyakgamcho-tang decoction was performed using an ultra-performance liquid chromatography-electrospray ionization-mass spectrometer. The analytical column for separation of the compounds 1~11 was used an UPLC BEH $C_{18}$ ($100{\times}2.1mm$, $1.7{\mu}m$) column and column oven temperature was maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid (A) and acetonitrile (B) by gradient elution. The flow rate was 0.3 ml/min and injection volume was $2.0{\mu}l$. Correlation coefficient in the calibration curves of the compounds 1~11 were showed a good linearity with more than 0.99. The limit of detection and limit of quantification values of the compounds 1~13 were detected in the ranges 0.06~18.43 ng/ml and 0.18~58.29 ng/ml, respectively. Among the compounds 1~11, the compounds 10 were not detected in this sample, while the ten compounds, 1~9 and 11, were detected $44.05{\sim}19,289.05{\mu}g/g$ in Jakyakgamcho-tang extract.

Rapid Determination of Caffeine in Forensic Aqueous Sample by Dilute and Shoot LC-MS/MS (시료 희석 직접 주입 LC-MS/MS를 이용한 법화학 수용액 시료 중 카페인 신속 분석)

  • Choi, Yun Jeong;Kim, Hee Seung;In, Moon Kyo;Kim, Jin Young
    • YAKHAK HOEJI
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    • v.60 no.3
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    • pp.112-117
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    • 2016
  • A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of caffeine in forensic aqueous sample. The centrifuged sample ($100{\mu}l$) was diluted 50-fold with distilled water. The diluted sample ($400{\mu}l$) was then diluted further with $200{\mu}l$ of 0.1% formic acid solution and $400{\mu}l$ of acetonitrile containing 500 ng of caffeine-(3-methyl-$^{13}C_3$) prior to LC-MS/MS analysis. The mobile phase was composed of 0.1% formic acid in distilled water (A) and acetonitrile (B). Chromatographic separation was performed by using a Zorbax SB-C18 ($100mm{\times}2.1mm$ i.d., $3.5{\mu}m$) column and caffeine was eluted within 1.1 min. Linear least-squares regression with a 1/x weighting factor was used to generate a calibration curve with the coefficients of determination ($r^2=0.9983$). The lower limit of quantification was $25ng/ml$ for the analyte. The process efficiency was 98.6~100.1%. Intra- and inter-day precisions were not more than 2.1% and 1.7%, while intra- and inter-day accuracies were ranged from -6.8 to 4.5%, respectively. The suitability of the method was examined by analyzing unknown forensic aqueous samples.

Simultaneous Analysis of Bioactive Metabolites from Caulis Lonicera japonica by HPLC-DAD-ion trap-MS (HPLC-DAD-ion trap-MS를 이용한 인동 생리활성 물질의 동시분석)

  • Ryu, Sung-Kwang;Won, Tae-Hyung;Kang, Sam-Sik;Shin, Jong-Heon
    • YAKHAK HOEJI
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    • v.54 no.3
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    • pp.157-163
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    • 2010
  • A high-performance liquid chromatography (HPLC) with DAD detector and electrospray ionization mass spectrometry (ESI-MS) was established for the simultaneous determination of coniferin (1), loganic acid (2), demethylsecologanol (3), sweroside (4) and loganin (5) from caulis Lonicera joponica. The optimal chromatographic conditions were obtained on an ODS column ($5{\mu}m$, $4.6{\times}150mm$) with the column temperature $35^{\circ}C$. The mobile phase was composed of (A) water with 0.1% formic acid and (B) methanol with 0.1% formic acid using a gradient elution, the flow rate was 0.3 ml/min. Detection wavelength was set at 254 nm. All calibration curves showed good linear regression ($r^2$>0.998) within test ranges. The developed method provided satisfactory precision and accuracy with overall intra-day and interday variations of 0.16~3.28% and 0.14~1.99%, respectively, and the overall recoveries of 99.39~105.89% for the five compounds analyzed. The verified method was successfully applied to quantitative determination of the two types (phenolic compounds and iridoids) of bioactive compounds in 24 commercial caulis L. japonica samples from different markets in Korea and China. The analytical results demonstrated that the contents of the five analytes vary significantly with sources.