• 제목/요약/키워드: HPLC/SPE/HPLC

검색결과 103건 처리시간 0.025초

HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구 (Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC)

  • 오보영;배준현;강준길;김연두
    • 대한화학회지
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    • 제43권6호
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    • pp.663-669
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    • 1999
  • HPLC/UV 및 GC/FPD 법을 사용하여 환경수에 존재하는 Diazinon, EPN, Fenitrothion, Phosalon 및 Phosmet 등 5종의 유기인계 잔류농약을 분석하였다. 전처리 과정으로 고체상추출법(SPE)과 용매추출법(LLE)을 각각 적용한 결과, 회수율과 재현성에 있어, HPLC/UV에서는 용매추출법(LLE)보다 고체상추출법(SPE)이 더 우수하였고, GC/FPD에서는 고체상추출법(SPE)보다 용매추출법(LLE)이 더 우수하였다. 또 수돗물 및 하천수(와룡천)에 일정량의 유기인계 농약을 가하여 만든 합성시료중 각 성분을 분석한 결과, SPE-HPLC/UV 법에서는 회수율이 101%, % RSD는 4.3∼8.7이었고, LLE-GC/FPD 법에서는 회수율이 100%, % RSD는 3.2∼9.5이었다. 이 결과는 두 방법 모두 유기인계 잔류농약 분석에 이용할 수 있는 우수한 방법임을 제시하고 있다.

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Determination of Pesticide Residues in Water using On-line SPE-HPLC Coupling System

  • Lee, Dai Woon;Lee, Sung Kwang;Park, Young Hun;Paeng, Ki-Jung
    • 분석과학
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    • 제8권4호
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    • pp.539-543
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    • 1995
  • The on-line SPE-HPLC coupling system was developed for the efficient separation and determination of trace pesticides, such as phenoxyacetic acids and esters, and triazines in aqueous solutions. By using the developed SPE-HPLC on-line system, the band broadening usually observed in single precolumn switching mode was greatly reduced, consequently, the quantitative determination of trace pesticides could be achieved, Besides, since most of the analytes preconcentrated by SPE column could be injected directly into HPLC system, the limit of detection can be improved down to ppt level.

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HPLC를 이용한 석유제품 중의 식별제 Unimark 1494DB 분석 (Determination of Unimark 1494DB in Petroleum using HPLC)

  • 임영관;김동길;임의순;신성철
    • Korean Chemical Engineering Research
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    • 제47권5호
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    • pp.593-598
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    • 2009
  • 정상경유에 등유 및 부생연료유를 인위적으로 혼합한 후, SPE 전처리 과정과 HPLC 분석을 통해 석유제품 내에 함유되어 있는 식별제의 정성 정량분석방법에 관해 연구하였다. SPE 전처리 과정에서 시료주입 후 15분에 분취된 시료에서 가장 높은 농도의 식별제가 분석되었다. 경유제품에 1 mg/L의 식별제를 혼입시킨 후, 전처리를 거쳐 HPLC로 분석한 결과 9.8분의 머무름시간에서 $1626.92mV{\cdot}sec$ 의 감도로 식별제가 분석되었으며, 또한 기존의 UV-Spectroscopy법으로 분석이 힘들었던 산성조건의 석유제품에서 식별제 분석이 가능하였다.

On-line SPE-HPLC Method using Alumina Filtering to Selectively Extract Phenolic Compounds from Environmental Water

  • Lee, Sung-Kwang
    • Bulletin of the Korean Chemical Society
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    • 제31권12호
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    • pp.3755-3759
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    • 2010
  • A on-line SPE (solid phase extraction)-HPLC preconcentration method was developed for the determination of phenolic compounds at trace levels in environmental water sample. XAD-4 and Dowex 1-X8 were used as sorbent in the on-line SPE-HPLC method for the selective enrichment of nine phenolic compounds, which are included in the priority pollutants list of the US EPA. Also alumina prefiltering considerably reduced the amount of interfering peaks due to humic substances that could accumulated due to the preconcentration step and prevent quantification of polar phenolic compounds in environmental water samples. This method was used to determine the phenolic compounds in tap and river water and superiority to the US EPA 625 method in its enrichment factor, pretreatment time, recoveries, and detection limit. The limits of detection were in the range of $0.3-0.9\;{\mu}g/L$ in tap water sample.

고체상추출법과 HPLC/MSD/FLD를 이용한 수질중의 페놀 분석 (Determination of phenol using solid-phase extraction and HPLC/MSD/FLD in water)

  • 이태준;박근영;표동진
    • 분석과학
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    • 제28권6호
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    • pp.370-376
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    • 2015
  • Priority pollutant이며 페놀성화합물의 전구체인 페놀을 고체상추출법을 이용하여 추출 정제하여 형광검출기와 질량분석기가 각각 장착된 고속액체크로마토그래프를 이용하여 분석하는 방법을 설정하여 보았다. 고체상추출은 고분자성물질이 충진된 Oasis HLB cartridge를 이용하여 최적의 조건을 확립하였으며 이때의 평균회수율은 87.0% 이었다. 형광검출기를 이용한 경우가 질량분석기를 이용한 경우보다 검출한계가 낮았으나 선택성의 측면에서 질량분석기가 우수하였다.

Rapid Identification of Bioactive Compounds Reducing the Production of Amyloid β-Peptide (Aβ) from South African Plants Using an Automated HPLC/SPE/HPLC Coupling System

  • Kwon, Hak-Cheol;Cha, Jin-Wook;Park, Jin-Soo;Chun, Yoon-Sun;Moodley, Nivan;Maharaj, Vinesh J.;Youn, Sung-Hee;Chung, Sung-Kwon;Yang, Hyun-Ok
    • Biomolecules & Therapeutics
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    • 제19권1호
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    • pp.90-96
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    • 2011
  • Automated HPLC/SPE/HPLC coupling experiments using the Sepbox system allowed the rapid identification of four bioactive principles reducing the production of amyloid $\beta$-peptide ($A{\beta}$) from two South African plants, Euclea crispa subsp. crispa and Crinum macowanii. The structures of biologically active compounds isolated from the methanol extract of Euclea crispa subsp. crispa were assigned as 3-oxo-oleanolic acid (1) and natalenone (2) based on their NMR and MS data, while lycorine (3) and hamayne (4) were isolated from the dichloromethane-methanol (1:1) extract of Crinum macowanii. These compounds were shown to inhibit the production of $A{\beta}$ from HeLa cells stably expressing Swedish mutant form of amyloid precursor protein (APPsw).

Simultaneous determination of bisphenol A, chlorophenols and alkylphenols by solid-phase extraction and HPLC

  • Lee, Taejoon;Park, Keun-Young;Pyo, Dongjin
    • 분석과학
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    • 제30권1호
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    • pp.20-25
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    • 2017
  • An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

자동화 HPLC/SPE/HPLC 시스템(Sepbox system)을 활용한 고추 잎 (leaf of Capsicum annuum L.) 추출물 분리 및 α-glucosidase 억제 활성 물질 탐색 (Rapid separation of Capsicum annuum L. leaf extract using automated HPLC/SPE/HPLC coupling system (Sepbox system) and identification of α-glucosidase inhibitory active substances)

  • 김민선;진종범;이정환;안혜숙;판철호;박진수
    • Journal of Applied Biological Chemistry
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    • 제64권1호
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    • pp.25-32
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    • 2021
  • 식물 유래 화합물은 다양한 생리활성과 구조 다양성으로 많은 연구자에게 관심을 받고 있으나 화합물 분리는 많은 시간 소요, 과량의 유기용매 소모와 분리과정 중의 활성성분의 유실 등의 어려움을 겪게 된다. 이러한 점을 극복하기 위하여 HPLC/SPE/HPLC를 결합한 Sepbox 분리시스템을 이용하여 고추잎 추출물에서 288개 분획물을 획득하였고 이 중에서 alpha-glucosidase 저해효능을 가지는 화합물인 luteolin 7-O-glucoside를 효과적으로 확인할 수 있었다. 또한 고추잎에 풍부한 플라보노이드 다당체를 가수분해함에 따라 해당 활성이 증가함을 검증하였다. 그러므로 본 연구결과는 Sepbox 시스템이 생리활성 평가와 결합할 경우 식물 내 유용물질 탐색에 효과적임을 보여주었다.

테트라싸이클린계 잔류항생물질 분석을 위한 전처리방법 비교 (Comparison of pretreatment methods for tetracyclines analysis by HPLC)

  • 김동언;황래홍;윤은선;함희진;양윤모;김창기;기노준;이정학
    • 한국동물위생학회지
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    • 제26권3호
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    • pp.199-202
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    • 2003
  • Solid phase extraction(SPE) and matrix solid phase dispersion(MSPD) have been studied as preparation procedures for tetracyclines analysis by high-performance liquid chromatography(HPLC) in meat. The recovery range was 74${\sim}$98% for SPE, and 72${\sim}$93% for MSPD at spiked levels of 100ng/g for oxytetracycline(OTC), tetracycline(TC), chlortetracycline(CTC), and doxycycline(DC). The detection limits were 15${\sim}$78ng/g for SPE and 25${\sim}$84ng/g for MSPD, respectively. Analytical method was HPLC with UV detector. The purpose of this study was developing a practical, accurate and precise method for rapid extraction and quantitation of tetracycline residues in meat.

Preconcentration and Detection of Herbicides in Water by Using the On-line SPE-HPLC System and Photochemical Reaction

  • 이승호;이성광;박영훈;김현주;이대운
    • Bulletin of the Korean Chemical Society
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    • 제20권10호
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    • pp.1165-1171
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    • 1999
  • The analysis of trace herbicides using the on-line SPE-HPLC system and a photochemical reaction was studied. 18 compounds of herbicides including eight triazines, six phenoxy acids and esters, and four other herbicides were examined. The on-line SPE-HPLC system developed for selection of eluting solvent improved chromatographic efficiency. The recoveries of herbicides were higher than 77%. With 100 mL tap water samples, the detection limits for all analytes were in the 0.1-2.3×10-10 M range. Detection was done by a UV or fluorescence spectrometer after photochemical reaction at the end of the column with 2W or 450W mercury lamp. Without a photochemical reaction, all compounds responded to 230 nm UV detector, but phenoxy acids and esters were weakly detected. However, with a photochemical reaction, these compounds were selectively detected at 320 nm wavelength of UV absorption and 400 nm emission of the fluorescence detectors. This method can be used for the analysis of environmental water containing herbicides at trace levels.