• Title/Summary/Keyword: Solid phase cartridge

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Efficiency of Silver Ion-Silica Solid Phase Extraction for Elimination of Sulfur Compounds during Pesticide Multiresidue Analysis in Allium Species (파속류의 잔류농약분석과정에서 silver ion-silica solid phase extraction에 의한 황화합물의 제거 효율성)

  • Park, Jin-Woo;Moon, Kyung-Mi;Choi, Young-Whan;Lee, Young-Guen
    • Journal of Life Science
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    • v.20 no.1
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    • pp.60-65
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    • 2010
  • Since organic sulfur compounds respond to GC/ECD sensitively, they interfere with quantitative separation of pesticides during residual pesticide analysis of Allium species. In this study, it was intended to develop a rapid and simple method for pesticide multi-residues analysis through clean-up and interferences by a solid-phase extraction (SPE). An SPE method employing silver nitrate impregnated Florosil cartridge was developed and evaluated for the elimination of sulfur compounds from the test solution of Allium species during pesticide residues analysis. The silver nitrate impregnated Florosil cartridge was prepared by efflux of 3 ml of 20% silver nitrate solution through Florosil cartridge (1 g packing, 6 ml tube). The extracts equivalent to 2, 4 6, and 10 g of each sample were loaded onto the cartridge and allowed to exude, and then the exudations were analyzed by GC/ECD. More than 95% of sulfur compounds were removed from the loaded extracts equivalent, up to 6 g in onion, 4 g in spring onion and 4 g in shallot, respectively. 40 pesticides were spiked in the Allium species and loaded onto the cartridge to determine the recoveries; from this, the recoveries of 34 pesticides were within 70~120%.

Simultaneous detection of residual fungicide in Bean Sprouts by Solid-phase Extraction (고체상 추출법에 의한 콩나물 중의 잔류농약 동시 검출)

  • Lee, Myunghwoon;Lee, Taejoon;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.509-514
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    • 1993
  • Benomyl, topsin-M and thiram been known as one of the seed disinfectant. For these studies benomyl, topsin-M and thiram simultaneously had been analyzed by high performance liquid chromatographic method using ODS cartridge, benomyl, topsin-M and thiram was chromatographed using an ODS column and eluent 40% Acetonitrile at a flow rate of 1ml/min. The UV Detector responses at 276nm.

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Study on Solid Phase Extraction and Spectrophotometric Determination of Vanadium with 2-(2-Quinolylazo)-5-Diethylaminophenol

  • Hu, Qiu-Fen;Yang, Guan-Gyu;Huang, Zhang-Jie;Yin, Jia-Yuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.263-266
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    • 2004
  • A sensitive, selective and rapid method has been developed for the determination ${\mu}$g/L level of vanadium ion based on the rapid reaction of vanadium(V) with 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) and the solid phase extraction of the colored chelate with $C_{18}$ cartridge. The QADEAP reacts with V(V) in the presence of citric acid-sodium hydroxide buffer solution (pH = 3.5) and cetyl trimethylammonium bromide (CTMAB) medium to form a violet chelate of a molar ratio 1 : 2 (V(V) to QADEAP). This chelate was enriched by solid phase extraction with $C_{18}$cartridge and the enrichment factor of 50 was obtained by elution of the chelates from the cartridge with ethanol. The molar absorptivity of the chelate is $1.28 {\times}10^5L\;mol^{-1}cm^{-1}$ at 590 nm in the measured solution. Beer's law is obeyed in the range of 0.01-0.6 ${\mu}$g/mL. The detection limit is 0.04 ${\mu}$g/L in the original samples. This method was applied to the determination of vanadium(V) in water and biological samples with good results.

Simple and Highly Efficient Synthesis of [$^{11}C$]methionine Using Solid-Phase Extraction Method (고정상 추출법을 이용한 효율적인 [$^{11}C$]methionine의 합성)

  • Lim, Sung-Jae;Moon, Woo-Yeon;Choi, Jae-Chil;Cho, Shee-Man;Oh, Seung-Jun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.12 no.3
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    • pp.181-183
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    • 2008
  • We developed simple and highly efficient synthesis method for [$^{11}C$]methionine using solid-phase extraction method. For synthesis, we used C18 cartridge. [$^{11}C$]methionine was synthesized on C18 cartridge according to the solid-phase [$^{11}C$]methylation of precursor L-homocysteine thiolactone hydrochloride. The radiochemical yields of [$^{11}C$]methionine was $48.9{\pm}7.93%$ decay corrected (results of 30 syntheses, mean$\pm$SD), with average production higher than 180 mCi. This procedure showed high yield and simple synthesis of [$^{11}C$]methionine.

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Analysis of Aromatic Amines in Mainstream Cigarette Smoke Using Solid-Phase Extraction (Solid-Phase Extraction을 이용한 담배연기 중 Aromatic Amino의 분석)

  • Kim, Ick-Joong;Lee, John-Tae;Lee, Jeong-Min;Min, Hye-Jeong;Jang, Gi-Chul;Kim, Hyo-Keun;Hwang, Keon-Joong;Min, Young-Keun
    • Journal of the Korean Society of Tobacco Science
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    • v.28 no.2
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    • pp.152-157
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    • 2006
  • A new procedure has been developed for the quantitation of aromatic amines in mainstream cigarette smoke. Two solid-phase extraction (SPE) clean up steps, using a different retention mechanisms, are required to process the samples. The first step used a cation-exchange cartridge, followed by a second step that used a cartridge with a hydrophobic retention character. The aromatic amines eluted from the second SPE cartridge are derivatized with pentafluoropropionic anhydride. This new method have advantages over other reported techniques, being sensitive, robust, and easily automated. The detection limits were ranged from 0.12 ng/mL for 1-aminonaphthalene to 0.16 ng/mL for 3-aminobiphenyl and the recoveries were from 97 to 106%. Compared with other reports for analysis of 2R4F reference cigarette, this method shows a close analytical data and good repeatability.

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.

Solid-Phase Extraction of Caffeine and Catechin Compounds from Green Tea by Caffeine Molecular Imprinted Polymer

  • Jin, Yinzhe;Row, Kyung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.28 no.2
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    • pp.276-280
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    • 2007
  • In this work, caffeine and some catechin compounds + C, EC, EGC, and EGCG were extracted from green tea by using molecular imprinted polymers (MIP) as sorbent materials in a solid-phase extraction (SPE) process known as MISPE (molecular imprinted solid-phase extraction). For synthesis of MIP, caffeine was employed as the template, MAA as the monomer, EGDMA as the crosslinker, and AIBN as the initiator. A solution of caffeine (0.2 mg/mL in methanol) was utilized in the solid extraction cartridges following loading, washing, and elution procedures with acetonitrile, methanol, and methanol-acetic acid (90/10, %v/v) as the solvents, respectively. This solid-phase extraction protocol was applied for the extraction of caffeine and some catechin compounds from green tea. A comparison was made between the results obtained with the MIP cartridges and a traditional C18 reversed-phase cartridge. It was thereupon found that the recovery of caffeine by the MIPbased sorbent used in this work was almost two and four times greater than that by a commercially available C18 material. A quantitative analysis was conducted by high performance liquid chromatography (HPLC) using a C18 column (5 μm, 250 × 4.6 mm) with methanol/water (40/60, %v/v) as the mobile phase at a flow rate of 0.5 mL/min.

Solid-Phase Extraction of Sulfamerazine from Shrimp Residue and Determination by Reversed Phase High Performance Liquid Chromatography

  • Jang, Won-Cheoul;Heo, Gang-Joon
    • Toxicological Research
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    • v.12 no.2
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    • pp.163-169
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    • 1996
  • The focus of this study was to investigate the suitable analytical methods for measurement of sulfamerazine and its metabolite in shrimp hepatopancreas and tail tissue, in addition to the methods for the optimization of solid-phase extraction cartridge conditions and the elucidation of sulfamerazine concentrations in aqueous buffer using HPLC with UV and EC detectors. Compared with UV detector the EC detector appears to be 10 times more sensitive than that of the UV detector. After the shrimp was exposed to 10 ppm sulfamerazine, the accumulation levels of sulfamerazine and its metabolite in tail tissue, which is edible portion, were considerably lower than 0.1 ppm. The data indicate that sulfamerazine continues to be a candidate for use at levels of sulfamerazine concentration used in aquaculture of shrimp.

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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.

Simultaneous Liquid Chromatography Tandem Mass Spectrometric Determination of 35 Prohibited Substances in Equine Plasma for Doping Control

  • Kwak, Young Beom;Yu, Jundong;Yoo, Hye Hyun
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.158-165
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    • 2022
  • Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.