• Title/Summary/Keyword: HPLC/SPE/HPLC

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

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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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
    • Analytical Science and Technology
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    • v.8 no.4
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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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Determination of Unimark 1494DB in Petroleum using HPLC (HPLC를 이용한 석유제품 중의 식별제 Unimark 1494DB 분석)

  • Lim, Young-Kwan;Kim, DongKil;Yim, Eui Soon;Shin, Seong-Cheol
    • Korean Chemical Engineering Research
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    • v.47 no.5
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    • pp.593-598
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    • 2009
  • In this study, the qualitative and quantitative analytical method for petroleum marker(Unimark 1494DB) in common diesel involved kerosene and byproduct fuel was developed using SPE pretreatment and high performance liquid chromatography. In SPE pretreatment process, the highest concentrated marker was obtained 15 minutes after addition of petroleum sample. The petroleum marker was detected with $1626.92mV{\cdot}sec$ intensity at 9.8 minutes retention time in 1 mg/L content in petrodiesel after pretreatment. Also petroleum marker was selectively identified in an acidic petroleum product which was previously difficult to be analyzed by UV-Vis Spectroscopy.

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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    • v.31 no.12
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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.

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

  • Lee, Taejoon;Park, Keun-Young;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.28 no.6
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    • pp.370-376
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    • 2015
  • An analytical method for determining phenol considered priority pollutants of the US EPA and precursor of toxic phenolic compounds by solid-phase extraction (SPE) and high performance liquid chromatographic systems (HPLC) equipped with fluorescence and mass selective detectors have been developed. The SPE process for sample preconcentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of pH, elution solvent, and elution volume on the recoveries of the analytes were investigated with HPLC/FLD. Average recovery of >87.0% was achieved with 60 mg sorbents using 5 mL of methanol as an elution solvent at pH=3.

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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    • v.19 no.1
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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
    • Analytical Science and Technology
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    • v.30 no.1
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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.

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 (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)

  • Kim, Min-Seon;Jin, Jong Beom;Lee, Jung Hwan;An, Hye Suck;Pan, Cheol-Ho;Park, Jin-Soo
    • Journal of Applied Biological Chemistry
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    • v.64 no.1
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    • pp.25-32
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    • 2021
  • Phytochemicals include plant-derived natural products that promote and improve the human metabolism and physiological activity, and there is a lot of research to find the value of the molecules is in progress. Likewise, we obtained 288 fractions of Capsicum annuum L. extract in less than 20 h using HPLC/SPE/HPLC coupling experiment through Sepbox system, an effective separation system to search for active substances in natural resources and ensure efficacy and reliability. Therefore, this experiment allowed rapid identification of biologically active molecules from the extract compared to traditional separation processes. Of the above fractions, eight fractions showed the α-glucosidase inhibitory (AGI) activity and subsequent LC-MS analysis revealed one of the active molecules as luteolin 7-O-glucoside. In addition, we proved the increase in AGI activity according to deglycosylation of flavonoid glycoside. Therefore, this study suggests that the Sepbox system can quickly separate and identify active components from plant extract, and is an effective technique for finding new active substances.

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

  • Kim, Dong-Eon;Hwang, Lae-Hwong;Yun, En-Sun;Ham, Hee-Jin;Yang, Yoon-Mo;Kim, Chang-Gi;Ki, No-Jun;Lee, Jung-Hark
    • Korean Journal of Veterinary Service
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    • v.26 no.3
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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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    • v.20 no.10
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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.