• Title, Summary, Keyword: Solid phase extraction (SPE)

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Optimization of Solid Phase Extraction Method for Quantitative Analysis of Perfluorooctanoic Acid in Serum using Liquid Chromatography-Tandem Mass Spectrometry

  • Lee, Hyun-Seok;Yim, Yong-Hyeon
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.30-33
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    • 2014
  • A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

A Solid-Phase Extraction Method for Analyzing Trace Amounts of Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans in Waste Water

  • Park, Deok-Hie;Youn, Yeu-Young;Choi, Jae-Won;Lim, Young-Hee;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • v.2 no.1
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    • pp.12-15
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    • 2011
  • The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001.0.25 and 0.015.4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.

Mulberry Paper Bag μ-Solid Phase Extraction for the Analysis of Five Spice Flavors by Gas Chromatography-Mass Spectrometry

  • Yoon, Ok-Kyung;Lee, Dong-Sun
    • Bulletin of the Korean Chemical Society
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    • v.30 no.1
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    • pp.35-42
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    • 2009
  • Headspace micro solid phase extraction using mulberry paper bag (HS-MPB-$\mu$-SPE) has been developed and validated for the analysis of volatile flavor compounds from five spice by gas chromatography-mass spectrometry (GC/MS). HS-MPB-$\mu$-SPE was performed with adsorbent particles enclosed inside a mulberry paper bag. Four different kinds of adsorbents such as Tenax TA, Porapack Q, dimethylpolysiloxane and polyethylene glycol were tested. The extraction solvents compared were petroleum ether, methylene chloride, and chloroform. Better results were obtained when Tenax TA and petroleum ether were used. The limit of detection (LOD) and the limit of quantitation (LOQ) were in the range of 1.3 ng/mL and 4.3 ng/mL, respectively, for o-cymene as a model compound of monoterpene. Proposed method showed good reproducibility (3.3%, RSD) and good recoveries (94.0%). The HS-MPB- μ-SPE is very simple to use, inexpensive, rapid, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume (0.6 mL), there is minimal waste or exposure to toxic organic solvent and no further concentration step. This method allows successful characterization of the headspace in contact with the five spice sample. Strong trans-anethole from star anise or fennel is a characteristic flavor of five spice powders. HS-MPB-$\mu$-SPE combined with GC/MS can be a promising technique for the broad spectrum measurement of volatile aroma compounds from solid spices.

On-Channel Micro-Solid Phase Extraction Bed Based on 1-Dodecanethiol Self-Assembly on Gold-Deposited Colloidal Silica Packing on a Capillary Electrochromatographic Microchip

  • Park, Jongman;Kim, Shinseon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.45-50
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    • 2014
  • A fully packed capillary electrochromatographic (CEC) microchip with an on-column micro-solid phase extraction (SPE) bed for the preconcentration and separation of organic analytes was prepared. A linear microchannel with monodisperse colloidal silica packing was formed on a cyclic olefinic copolymer microchip with two reservoirs on both ends. Silver-cemented silica packing frit structure was formed at the entrance of the microchannel by electroless plating treatment as a base layer. A gold coating was formed on it by reducing $Au^{3+}$ to gold with hydroxylamine. Finally micro-SPE bed was formed by self-assembly adsorption of 1-dodecanethiol on it. Micro-SPE beds were about 100-150 ${\mu}m$ long. Approximately $10^3$ fold sensitivity enhancements for Sulforhodamine B, and Fluorescein in nM concentration levels were possible with 80 s preconcentration. Basic extraction characteristics were studied.

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.

Molecularly Imprinted Polymers for Solid-Phase Extraction of Sarcosine as Prostate Cancer Biomarker from Human Urine

  • Hashemi-Moghaddam, Hamid;Rahimian, Majid;Niromand, Bahman
    • Bulletin of the Korean Chemical Society
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    • v.34 no.8
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    • pp.2330-2334
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    • 2013
  • A highly selective molecularly imprinted polymer (MIP) for sarcosine, a cancer marker, was prepared and its use as solid-phase extraction (SPE) sorbent material was demonstrated. The MIP was prepared by a very simple procedure using methacrylic acid as functional monomer and a mixture acetonitrile/water (4/1, v/v) as porogen, overcoming in this way the problems usually related to the imprinting of biological polar compounds. The MIP was tested in batch experiments in order to evaluate its binding properties and then used as SPE sorbent for the selective clean-up and pre-concentration of sarcosine. The extraction protocol was successfully applied to the direct extraction of sarcosine from spiked human urine indicating that the MIP allowed sarcosine to be pre-concentrated while simultaneously interfering compounds were removed from the matrix.

A Study on the Analytical Methods Using Solid-phase Extraction for the Determination of Phenols in Water

  • Jeon, Chi-Wan;Lee, Jung-Hwa;Lee, Sang-Hak
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • pp.135-138
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    • 2003
  • Based on solid phase extraction, gas chromatography and mass spectrometry procedure for determining phenol and its derivatives in natural water was presented. In solid phase extraction, three types of techniques using solid phase adsorption material were treated with acid and salt, and converted second portion of acetyl derivatives. Under the these condition, extraction efficiency and detection ability dependent on extraction methods were discussed. Obtained results using optimized solid phase extraction techniques showed more convenience, simplifier and lower cost than the conventional analytical methods with holding wide dynamic range and lower detection limits.

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Application of Reversed-Phase Solid Phase Extraction for the HPLC Analysis of Microcystins in Water (다량 시료중 마이크로시스틴의 농축 및 분석)

  • Kim, Myeong-Hee;Kim, Tae-Seung;Kim, Tae-Keun;Park, Sun Ku
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.399-402
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    • 2000
  • To determine the concentrations of microcystins present in lake water or in tap water using high performance liquid chromatography, it is necessary to concentrate a large volume of water samples (about 20 L) into very small volume (0.1-0.3 mL). Concentration can be conveniently done when disc type solid phase extraction (SPE) apparatus is used. Using this apparatus we have investigated the recovery rates of three kinds of microcystins, RR, YR, LR. The recovery rates were relatively low and the reproducibilities were not good either. It is expected, however, that the appropriate selection of the disc conditioning and eluting solvents and reproducible reconcentration process after SPE will improve both the recovery rates and the reproducibilities.

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The Study on the Rapid Screening of Schedule Chemicals in Aqueous Solution Using SPE-ACF (수용액에서 SPE-ACF를 이용한 특정화학물질의 신속 스크리닝 기법 연구)

  • Park, Hoon;Jung, Chang-Hee;Lee, Yong-Han;Hong, Dea-Sik
    • Journal of the Korean Chemical Society
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    • v.52 no.3
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    • pp.239-248
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    • 2008
  • study of the solid phase extraction (SPE) technique using activated carbon fiber (ACF) as a sorbent was carried out on the schedule chemicals in water. 14 different schedule chemicals, which are the hydrolysis products and simulants of chemical agents such as alkylphosphonate, thiodiglycol etc. were selected for the study. Pyridine was used as a promoter to increase the derivatization efficiency, especially to improve silylation of 3-quinuclidinol. To improve the recovery efficiency of amines in the water solution, 1 mL of 5% Et3N/MeOH was introduced into SPE-ACF before the water sample loading. Throughout this study, the optimum condition was established to detect rapidly above chemicals in water.