• 제목/요약/키워드: On-column injection

검색결과 165건 처리시간 0.021초

새로운 HPLC용 형광유도체화제인 1-(N,N-dimethylamino) pyrene-6-sulfonyl chloride를 이용한 아민화합물의 분석 (Determination of Amine Compounds Using 1-(N,N-Dimethylamino) pyrene-6-sulfonyl chloride as a New Fluorescent Derivatizing Reagent for HPLC)

  • 이윤중;김용희;조정길
    • 약학회지
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    • 제35권4호
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    • pp.288-294
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    • 1991
  • A new fluorescent derivatizing reagent was developed to be used in HPLC for the trace determination of primary and secondary amines. This new reagent, 1-(N,N-dimethylamino)pyrene-6-sulfonyl chloride, was synthesized by the chlorination of sodium 1-(N,N-dimethylamino)pyrene-6-sulfonate which was obtained from 1-(N,N-dimethylamino)pyrene after sulfonation. Ephedrine and norephedrine were derivatized quantitatively by this reagent. The optimum conditions for the derivatization such as pH, reagent concentration, reaction time and reaction temperature ware examined. The structures of derivatives were identified by IR, $^{1}$H-NMR and MS methods. The fluorescence properties and the stability of the derivatives were examined. The derivatives were separated on silica column with an isocratic elution using the mixture of n-hexane and ethylacetate and monitored by fluorescene detector. Linear calibration curves were obtained and detection limits in a 10 $\mu$l injection volume were 5 picomole for ephedrine and norephedrine.

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액체 크로마토그래프법에 의한 대기시료중 미량 알데히드류의 정량 (Determination of Trace Aldehydes in Ambient Air by Liquid Chromatography)

  • 이용근;정태우
    • 한국대기환경학회지
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    • 제11권4호
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    • pp.339-349
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    • 1995
  • The purpose on this study is to optimize the chromatographic determination method of trace aldehydes in ambient air. Carbonyl compounds in urban air were trapped at $C_{18}$ DNPH-coated cartridges, and generated hydrazone derivatives were separated by HPLC and detected by UV-vis spectroscopic detector at 360nm. Formaldehyde and acetaldehyde compounds could be isolated from urban(Seoul) air with more than 95% collection efficiency. The analytical detection limits for formaldehyde and acetaldehyde are 0.06pp $b_{v}$, 0.08pp $b_{v}$ for 108 L air samples, respectively. The precision of this method are 3 .sim. 4%(RSD) for mutiple injection of hydrazone standards. Separation of seven dinitrophenylhydrazones could be achieved in appoximately 20 minutes operation time using $C_{18}$ column with apprepriate eluent. The method was applied to the analysis of aldehydes and ketone in Seoul ambient air. The 24-h ambient levels of formaldehyde, acetaldehyde reached up to 6 .sim. 14 and 3 .sim. 8ppbv, respectively. The daily average concentration ratio were 0.60 for acetaldehyde/formaldehyde.yde.

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친화성 막모듈에 의한 단백질 크로마토그래픽 특성 (Characteristics of Protein Chromatography by Affinity Membrane Mudule)

  • 이광진;염경호
    • KSBB Journal
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    • 제13권2호
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    • pp.125-132
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    • 1998
  • Protein affinity membrane was prepared via the coating of chitosan gel on the porous flat polysulfone membrane surface, followed by the immobilization f the reactive dye (Cibacron Blue 3GA) to the chitonsan gel. The maximum protein binding capacity of affinity membrane was about 70${\mu}g/cm^2$ determined by the batch adsorption experiments of human serum albumin (HSA). Using module of this membrane, the characteristics of protein chromatography were investigated through the experiments of elution and frontal chromatography of HSA. This membrane module promises as a chromatography column, since it represented a lower pressure drop and a greater reproducibility. The protein separation ratio was significantly influenced by the flow rate of mobile phase and the injection quantity of HSA. The dynamic protein binding capacity of module decreased from the equilibrium binding capacity with increasing flow rate and approached the value of 15 - 20 ${\mu}g/cm^2$ for flow rates above 6 mL/min.

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Enantioseparation of Racemic 1,1'Binaphthyl-2,2'diamine by Preparative Liquid Chromatography

  • Ryoo, Jae-Jeong;Kwon, Woo-Jeong;Kim, Tae-Hyuk;Lee, Kwang-Pill;Choi, Seong-Ho
    • Bulletin of the Korean Chemical Society
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    • 제25권9호
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    • pp.1336-1340
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    • 2004
  • The same kind of chiral stationary phase with a commercialized chiral column was used to make preparative chiral columns and was applied to resolve racemic N-acetyl-1-naphthylethylamide (3) by preparative liquid chromatography. An improved chromatographic condition to resolve racemic 3 on the CSP was examined by changing flow rate and kind of the mobile phase and the sample injection volume. The optimized separation conditions were applied to resolve racemic 1,1'-Binaphthyl-2,2'-diamine(4).

A New Trend of In-situ Electron Microscopy with Ion and Electron Beam Nano-Fabrication

  • Furuya, Kazuo;Tanaka, Miyoko
    • Applied Microscopy
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    • 제36권spc1호
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    • pp.25-33
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    • 2006
  • Nanofabrication with finely focused ion and electron beams is reviewed, and position and size controlled fabrication of nano-metals and -semiconductors is demonstrated. A focused ion beam (FIB) interface attached to a column of 200keV transmission electron microscope (TEM) was developed. Parallel lines and dots arrays were patterned on GaAs, Si and $SiO_2$ substrates with a 25keV $Ga^+-FIB$ of 200nm beam diameter at room temperature. FIB nanofabrication to semiconductor specimens caused amorphization and Ga injection. For the electron beam induced chemical vapor deposition (EBI-CVD), we have discovered that nano-metal dots are formed depending upon the beam diameter and the exposure time when decomposable gases such as $W(CO)_6$ were introduced at the beam irradiated areas. The diameter of the dots was reduced to less than 2.0nm with the UHV-FE-TEM, while those were limited to about 15nm in diameter with the FE-SEM. Self-standing 3D nanostructures were also successfully fabricated.

Study on Retardation Effect of a Heavy Metal in Sandy Soils

  • Kim, Dong-Ju;Sung, Baek-Doo
    • 한국지하수토양환경학회:학술대회논문집
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    • 한국지하수토양환경학회 1998년도 총회 및 춘계 학술발표회 논문집
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    • pp.43-49
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    • 1998
  • Retardation effect of heavy metals in soils caused by adsorption onto the surfaces of solids particles is well known phenomena. The adsorption of metal ions has been recognized more strong in clay mineral and organic matter contents rather than sands and gravels. In this study, we investigated the retardation effect in two sandy soils by conducting batch and column tests. The column tests were conducted to obtain the relationship between concentration and time known as breakthrough curve (BTC). We applied pulse type injection of ZnCl$_2$solution on the inlet boundary and monitored the effluent concentration at the exit boundary under steady state condition using EC-meter and ICP-AES. Batch test consisted of an equilibrium procedure for fine fractions collected from two sandy soils for various initial ZnCl$_2$concentrations, and analysis of Zn ions in equilibrated solution using ICP-AES. The results of column test showed that i) the peak concentration of Zn analyzed by ICP was far less than that detected by EC-meter for both soils and ii) travel times for peak concentration were more less identical for two different monitoring techniques. The first result can be explained by ion exchange between Zn and other cations initially present in the soil particles since ICP analysis showed a significant amount of Ca, Mg ions in the effluent. From the second result, we found that retardation effect was not present in these soils due to strong cation exchange capacity of Zn ion over other cations since we did not apply a solution containing more adsorptive cations such as Al. The result of batch test also showed high distribution coefficients (K$_{d}$) for two soils supporting the dominant ion exchange phenomena. Based on the retardation factor obtained from the Kd, we predicted the BTC using CDE model and compared with the BTC of Zn concentration obtained from ICP The predicted BTC, however, disagreed with the monitored in terms of travel time and magnitude of the peak concentrations. The only way to describe the prominent decrease of Zn ion was to introduce decay or sink coefficient in the CDE model to account for irreversible decrease of Zn ions in liquid phase.e.

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지하수 부존지역에서 최적 지열에너지 활용방식 수치 모의 (Numerical Simulations for Optimal Utilization of Geothermal Energy under Groundwater-bearing Conditions)

  • 김진성;차장환;송성호;정교철
    • 지질공학
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    • 제24권4호
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    • pp.487-499
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    • 2014
  • 최근 지열에너지 활용 증가 추세와 더불어 지하수 부존량이 풍부한 지역에서 수직개방형의 효율이 더 높다는 연구결과가 제시됨에도 불구하고, 국내 지열냉난방시스템의 열교환 방식은 수직밀폐형 방식이 주를 이루고 있다. 따라서, 본 연구에서는 지하수 부존량이 풍부한 지역에서 수직개방형 방식의 효율성을 검증하기 위하여, 수리지질 및 열적 특성을 반영한 최적의 지열에너지 활용 방식을 수치 모의하였다. 1차 모의 결과, 지하수 부존량이 풍부한 지역에서 지열냉난방시스템을 활용하는 경우 수직밀폐형보다 지하수를 직접 이용하는 수직개방형이 더욱 효과적인 것으로 분석되었으며, 수직개방형 중에서는 SCW (standing column well)형 보다는 주입정과 추출정이 분리된 복수관정형에서 지반과 열교환을 통해 얻을 수 있는 주입수와 추출수의 온도차 (${\Delta}$)가 커 더욱 효율적인 것으로 나타났다. 2차 모의에서는 수직개방형 지열에너지 공급방식인 단일관정형, SCW형, 복수관정형을 대상으로 열 이송, 이격거리 및 유량, 지하수 수리경사 등을 고려한 최적의 활용 방식을 검토하였으며, 이를 바탕으로 지열냉난방시스템의 지중 열교환 방식 선정 시 활용할 수 있는 흐름도를 제시하였다. 본 연구결과 제시된 다양한 선정 기준을 기초로 실제 선정 시에는 전체 지열냉난방 시스템에 대한 COP (coefficient of performance) 계산 및 세부적인 타당성 검토가 필요할 것으로 판단된다.

구미강활탕의 성분 분석 및 LDL 산화억제 효능 연구 (Simultaneous Determination of Gumiganghwal-tang and Its Anti-atherosclerotic Effect)

  • 김온순;서창섭;신현규
    • 대한예방한의학회지
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    • 제17권3호
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    • pp.165-176
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    • 2013
  • Objective : The purpose of this study was to establish the simultaneous analysis for six compounds in Gumiganghwal-tang (GMGHT, Jiuweiqianghuo-tang) and to investigate the anti-atherosclerotic effects of GMGHT in vitro. Methods : The column for separation of six compounds was used Luna $C_{18}$ column and maintained at $40^{\circ}C$. The mobile phase for gradient elution consisted of two solvent systems, 1.0% acetic acid in water and 1.0% acetic acid in acetonitrile. The analysis was carried out at a flow rate of 1.0 mL/min with pothodiode array (PDA) detection at 254, 280, and 320 nm. The injection volume was 10 ${\mu}L$. The antioxidant activities of GMGHT were evaluated by measuring free radical scavenging activities on 2,2'-Azinobis-3-ethyl-benzothiazoline-6-sulfonic acid (ABTS) and 1-1-diphenyl-2-picrylhydrazyl (DPPH). The inhibitory effects on low-density lipoprotein (LDL) oxidation were evaluated by the formation of thiobarbituric acid relative substances (TBARS), relative electrophoretic mobility (REM), and fragmentation of apolipoprotein B (ApoB)-100. Results : Calibration curves were acquired with $r^2{\geq}0.9998$. The contents of liquiritin, ferulic acid, baicalin, baicalein, glycyrrhizin, and wogonin in GMGHT were 1.784, 1.693, 37.899, 0.258, 1.869, and 0.034 mg/g, respectively. The GMGHT showed the radical scavenging activity in a dose-dependent manner. The concentration required for 50% reduction ($RC_{50}$) against ABTS and DPPH radicals were 72.51 ${\mu}g/mL$ and 128.49 ${\mu}g/mL$. Furthermore, GMGHT reduced the oxidation properties of LDL induced by $CuSO_4$. Conclusion : HPLC-PDA is considered as an available and convenient method for quality control and standardization of GMGH and GMGHT has potentials on anti-atherosclerosis by anti-oxidative effect and suppressive effect on LDL oxidation.

지질매질체내에서 계면활성제가 박테리아 이동 증진에 미치는 영향 (Influence of Surfactants on Enhancing Transport of Bacteria in Geological Materials)

  • 최낙철;박성직;김성배;김동주;이성재
    • 대한환경공학회지
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    • 제32권11호
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    • pp.1017-1023
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    • 2010
  • 본 연구에서는 지질매질체내에서 계면활성제(비이온성 계면활성제(Tween 20), 생계면활성제)가 박테리아(Bacillus subtilis ATCC 6633)의 이동 증진에 미치는 영향을 분석하였다. 계면활성제가 존재하는 다양한 실험조건에서 석영모래(입경분포: 0.5~2.0 mm, 평균입경: 1.0 mm)로 충진된 칼럼을 이용하여 박테리아의 이동에 관한 칼럼실험을 수행하였고, 박테리아 파과곡선으로부터 질량회수율과 부착효율 등을 정량화하였다. 실험결과, MSM(박테리아 성장에 필요한 무기물 배지)의 존재 하에서 매질체 표면에 박테리아의 부착이 상당히 증가하였는데(특히, 주입부분에), 이는 MSM으로 인한 이온강도의 증가 때문이다. 계면활성제가 존재할 경우에는, 계면활성제로 인하여 매질체내에서 박테리아 이동이 증진됨을 관찰할 수 있었다. 또한, MSM과 생계면활성제 주입방법에 따른 박테리아의 이동을 비교한 결과, 박테리아의 이동 증진을 위한 주입조건은 박테리아를 함유한 MSM용액보다 계면활성제를 선주입하거나, 또는 MSM용액과 계면활성제를 동시주입하는 것이 효과적임을 알 수 있었다. 본 연구를 통해 계면활성제의 존재와 주입방법이 박테리아의 이동에 영향을 미칠 수 있음을 알 수 있었다.

Qualitative Analysis of the Major Constituents in Traditional Oriental Prescription Bang-poong-tong-sung-san by Liquid Chromatography/Ultraviolet Detector/Ion-Trap Time-of-Flight Mass Spectrometry

  • Eom, Han Young;Kim, Hyung-Seung;Han, Sang Beom
    • Mass Spectrometry Letters
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    • 제5권1호
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    • pp.24-29
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    • 2014
  • An advanced and reliable high performance liquid chromatography (HPLC)/ultraviolet detector (UV)/ion-trap time-of-flight (IT-TOF) mass spectrometry was developed for the simultaneous quantification of 19 marker compounds in Bang-poong-tong-sung-san (BPTS), a traditional oriental prescription. Various parameters affecting HPLC separation and IT-TOF detection were investigated, and optimized conditions were identified. The separation was achieved on a Capcell PAK C18 column ($1.5mm{\times}250mm$, $5{\mu}m$ particle size) using a gradient elution of acetonitrile and water containing 0.1% formic acid at a flow rate of 0.1 mL/min. The column temperature was maintained at $40^{\circ}C$ and the injection volume was $2{\mu}L$. IT-TOF system was equipped with an electrospray ion source (ESI) operating in positive or negative ion mode. The optimized electrospray ionization parameters were as follows: ion spray voltage, +4.5 kV (positive ion mode), or -3.5 kV (negative ion mode); drying gas ($N_2$), 1.5 L/min; heat block temperature, $200^{\circ}C$. Automatic $MS^n$ (n = 1~3) analyses were carried out to obtain structural information of analytes. Elemental compositions and their mass errors were calculated based on their accurate masses obtained from a formula predictor software. The marker compounds in BPTS were identified by comparisons between $MS^n$ spectra from standards and those from extracts. Moreover, the libraries of $MS^2$ and $MS^3$ spectra and accurate masses of parent and fragment ions for marker compounds were constructed. The developed method was successfully applied to the BPTS extracts and identified 17 out of 19 marker compounds in the BPTS extracts.