• Title/Summary/Keyword: 고체상 추출

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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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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).

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.

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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Determination of fungicides in wines by solid-phase extraction and gas chromatography with mass selective detection (고체상 추출법과 GC/MS를 이용한 포도주 중의 fungicides 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.438-442
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    • 2003
  • The fungicides, used for grape growth and remained in the wine products from domestic and foreign countries such as vinclozolin, dichlofluanid, penconazole, procymidone were quantitatively analyzed after solid-phase extraction using a GC/MS-SIM method. The results obtained were as follows: for all the samples, the content of procymidone was in the range from 2.2 to $76.1{\mu}g/L$, recoveries 81.3-93.1 %, and standard deviation 1.4-3.4 %.

Determination of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) in human urine by solid-phase extraction and GC/MS (고체상 추출과 GC/MS를 이용한 소변 중 대마 대사체 (THCCOOH) 분석)

  • Cheong, Jae Chul;Kim, Jin Young;In, Moon Kyo;Cheong, Won Jo
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.441-448
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    • 2006
  • 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH) is the major metabolite of tetrahydrocannabinol (THC) which is the primary psychoactive component of marijuana. It is also the target analyte for the discrimination marijuana use. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of THCCOOH in human urine. Urine samples (3 mL) were extracted by SPE column with a cation exchange cartridge after basic hydrolysis. The eluents were then evaporated, derivatized, and injected into the GC/MS. The limits of detection (LOD) and quantitation (LOQ) were 0.4 and 1.2 ng/mL, respectively. The response was linear with a correlation coefficient of 0.999 within the concentration range of 1.2 (LLE 1.3)~50.0 ng/mL. The precision and accuracy were stable within 1.20% and the recovery was 83.6~90.7%. The recovery of SPE method was lower than that of liquid-liquid extraction (LLE), but there were no apparent differences in LOD, LOQ, precision and accuracy between the two methods. While SPE method is used as a very effective and rapid procedure for sample pretreatment, and clean extracts, LLE method was not suitable for the extraction procedure of THCCOOH in urine. The applicability of the method was proven by analyzing a urine samples from a marijuana abusers.