• Title/Summary/Keyword: 고체상추출

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The Analysis on VOCs That Occurs in Leather Cultural Heritage with SPME (고체상미세추출법(SPME)을 이용한 피혁 재질로부터 발생된 휘발성 유기화합물 분석기술 연구)

  • Chung, Yong-Jae
    • Journal of Conservation Science
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    • v.28 no.2
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    • pp.113-118
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    • 2012
  • Cultural heritages emit volatile organic compounds(VOCs) during degradation as chemical, biological factors. These VOCs in the atmosphere are degradation factors for another materials. But non-destructive organic analysis methods are uncommon, and have difficulties for field application. In this study, solid phase micro-extraction(SPME) and gas chromatography( GC) are carried out for analysis of VOCs which are emitted from leather, and prove SPME field holder's efficiency. I analize leather archival objects at The National Archives of Korea by cross-checking GC and SPME methods. It could be confirmed that the compounds are (E)-2-nonenal, butyl hydroxy toluene emitted itself from leather.

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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Comparison of Liquid-Liquid Extraction and Solid-Phase Extraction Coupled with GC/MS for Determination of Priority Pollutants in Water (액체 추출법과 고체상 추출법에 의한 수질 중 유해물질 농축법 비교)

  • Yook, Keun-Sung;Hong, Sa-Moon;Kim, Jong-Ho
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.441-453
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    • 1994
  • Two extraction methods, liquid-liquid extraction(LLE) and solid-phase extraction(SPE), coupled with GC/MS were compared as preconcentration procedures for priority pollutants in water. Among the semi-volatile priority pollutants, 11 acid and 44 base/neutral compounds were spiked in reagent water. With LLE, which is a modification of EPA Method 625, the overall mean recovery of the 54 compounds was 91% with a mean relative standard deviation(RSD) of 4.6%. With SPE, the overall mean recovery of the 52 compounds was 53% with a mean RSD of 8.9%. The detection limits of both methods were in the range of $1{\sim}5{\mu}g/l$.

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Solid Phase Extraction(SPE) of Curcuminoids from Turmeric by Optimization Analytical Condition (최적 분석조건에 의한 강황으로부터 Curcuminoids의 고체상추출(SPE))

  • Lee, Kwang Jin;Ma, Jin Yeul;Kim, Young Jun;Kim, Young Sik
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.13 no.10
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    • pp.4927-4935
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    • 2012
  • Turmeric is a medicinal herb with various pharmacological activities. Curcumin, demethoxycurcumin(DMC) and bisdemethoxycurcumin(BDMC) were extracted from turmeric by dipping and ultrasonic wave method. And extraction efficiency was identified using solid phase extraction(SPE). The extracted sample were simultaneously separated and analyzed from three kinds of commercial $C_{18}$ reversed-phase high performance liquid chromatography using water and acetonitrile as mobile phase with isocratic elution mode. Flow rate 1.0mL/min, injection volume $10{\mu}L$ and column oven temperature $40^{\circ}C$ at 425nm wavelength has been conducted. From the experimental results, the optimum mobile phase composition of water/acetonitrile 50/50vol% using RS tech column. It is evident that the amount of curcuminoids extracted(extraction time 4h) by 100% MeOH was higher than any aqueous MeOH composition. Finally, in 100% water extraction, the amount(mAU${\times}$mim) of curcuminoids extracted by SPE was 14.3 and 24.5 times respectively higher than ultrasonic wave and dipping method. The shown results can be applied as sources for pharmaceuticals and functional material.

Determination of thyroid hormones by solid-phase extraction using high performance liquid chromatograph/diode array detector/electro-spray ionization mass spectrometry in urine samples (HPLC/DAD/ESI-MS 및 고체상 추출법을 이용한 뇨시료중 갑상선 호르몬 분석)

  • Kwak, Sun Young;Moon, Myeong Hee;Pyo, Heesoo
    • Analytical Science and Technology
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    • v.19 no.6
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    • pp.519-528
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    • 2006
  • An analytical method for the determination of thyroid hormones in urine samples has been studied by using solid-phase extraction and high-performance liquid chromatography/diode array detector/electro-spray mass spectrometry. Seven thyroid hormones were successfully separated by gradient elution on the reverse phase Hypersil ODS column (4.6 mm I.D., 100 mm length, particle size $5{\mu}m$) with ammonium formate buffer and acetonitrile, and UV spectra and mass fragment could be confirmed. The extraction recoveries of thyroid hormones in the urine samples (pH 3) were in the range of 89.0-113.1% with solid-phase extraction by C18, followed by elution with 4 ml of methanol/ammonium hydroxide (9 : 1). The calibration curves showed good linearity with the correlation coefficients ($r^2$) varying from 0.992 to 0.998 and the detection limits of all analytes were obtained in the range of 2-4 ng/ml (3.8-13.0 pmol/ml).

Development of Analytical Method for Fipronil and Fipronil-Sulfone in Animal Serum by LC-MS/MS (LC-MS/MS에 의한 동물 혈청 내 피프로닐 및 피프로닐 설폰 분석법 개발)

  • Lee, Jeongsun;Park, Na-Youn;Jung, Woong;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.63 no.6
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    • pp.415-419
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    • 2019
  • Fipronil is an insecticide that belongs to the N-phenylpytazole and has been used mainly for an insect pest control. However, it is known that acute poisoning of the human body causes various symptoms such as dizziness, muscle weakness, dyspnea, skin irritation, and increased heart rate. Lately, eggs containing fipronil have been distributed and toxic problems are spreading around the world. In this study, we tried to develop analytical methods to evaluate the exposure of fipronil and fipronil sulfone in animal serum samples. The differences according to mobile phase and the results of liquid - liquid extraction and solid phase extraction pretreatment method were compared. Distilled water (A) and acetonitrile (B) were selected for the mobile phase, and the pretreatment method was determined by solid phase extraction. As a result of the method validation, the intra-day / inter-day accuracies were 82.2~114.1% and the precisions were less than 20%. The detection limit was 0.027 ng/ml for fipronil and 0.087 ng/ml for fipronil sulfone. The linearity obtained was satisfying, with a coefficient of determination (r2) higher than 0.99. The concentrations in some animal sera were determined using the methods of analysis for fipronil and fipronil sulfone in animal sera developed in this study. Using the method developed in this study, it could be used as an analytical method for human bio-monitoring of fipronil and fipronil sulfone as well as animal serum.

Monitoring and Development of Pretreatment Method for Perfluorinated Compounds in Fish Samples (어류에서의 과불화합물 분석을 위한 전처리법 확립 및 모니터링)

  • Heo, Jin-Ju;Lee, Ji-Woo;Kim, Seung-Kyu;Oh, Jeong-Eun
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.7
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    • pp.485-494
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    • 2013
  • An efficient extraction method was developed for the analysis of 16 perfluorinated compounds (PFCs) in fish samples. We compared the recoveries from the Ion-Pairing Extraction (IPE), Liquid-Liquid Extraction (LLE), Solid-Phase Extraction (SPE), IPE + SPE method with varying the injection time of the internal standard. As a result, IPE method with the internal standard before extraction was evaluated as the most effective pretreatment method. The RPM (Revolution Per Munite) and pH in IPE-before method were additionally adjusted and the more efficient pretreatment method was established. The total 33 fish samples including liver and gut samples were collected from Korean markets and analyzed PFCs with developed pretreatment method of this study. Total 16 PFC levels in fish samples ranged from ND to 1.67 ng/g with 100% detection frequency. The average PFCs concentrations of muscle, liver and gut samples from fish were compared and showed the following trend: liver (17.8 ng/g) > gut (13.3 ng/g) > muscle (1.67 ng/g). The PFC levels in fish samples were similar or lower than other available previous results of foreign studies.

Analysis of 1,3-dichloro-2-propanol and 3-chloro-1,2-propanediol by Solid Phase Extraction (고체상 추출에 의한 1,3-dichloro-2-propanol과 3-chloro-1,2-propanediol의 분석)

  • Chae, Hee-Jeong;In, Man-Jin;Kim, Min-Hong;Han, Keum-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.1
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    • pp.183-187
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    • 1997
  • The analytical conditions of 1,3-dichloro-2-propanol (DCP) and 3-chloro-1,2-propanediol (MCPD) by solid phase extraction were optimized to improve recovery. Selected-ion monitoring technique which was used for GC-MS analysis of both compounds gave substantially higher sensitivity. The detection limits of DCP and MCPD were 25 and 50 ppb, respectively. The effects of extraction column type, elution solvent and salt concentration on recovery were examined. A normal phase column was better than a reverse phase column in solid phase extraction of DCP and MCPD. It was explained in terms of polarity relationship of solvent-solute-solid phase. A maximum recovery was obtained at the salt concentration of 20% (w/v). Water-immiscible and chloropropanol-soluble solvents such as chloroform, diethyl ether, hexane and ethyl acetate were tested for elution solvent. Hexane and ethyl acetate were the most suitable solvents for the extraction of DCP and MCPD, respectively. High recovery better than 95% was obtained with the selected solvents.

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A Study on the Separation and Extraction of Polycyclic Aromatic Hydrocarbons in Water Sample by Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법에 의한 물시료 중 Polycyclic Aromatic Hydrocarbons의 분리 및 추출에 관한 연구)

  • Lee, Won;Hong, Jee-Eun;Park, Song-Ja;Pyo, Hee Soo;Kim, In-Whan
    • Analytical Science and Technology
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    • v.11 no.5
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    • pp.321-331
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    • 1998
  • The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHs) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some extraction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range $80{\sim}310^{\circ}C$. Extraction procedures of PAHs in water samples were somewhat modified and compared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3~109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7~94.9%) were obtained in case of $C_{18}$ disk extraction method by filtration. And extraction recoveries of PAHs by $C_{18}$ solid-phase were in the range of 51.8~77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25~6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05~1.25 ppb by disk extraction methods.

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