• 제목/요약/키워드: GC-determination

검색결과 479건 처리시간 0.036초

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

  • 오보영;배준현;강준길;김연두
    • 대한화학회지
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    • 제43권6호
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    • pp.663-669
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    • 1999
  • HPLC/UV 및 GC/FPD 법을 사용하여 환경수에 존재하는 Diazinon, EPN, Fenitrothion, Phosalon 및 Phosmet 등 5종의 유기인계 잔류농약을 분석하였다. 전처리 과정으로 고체상추출법(SPE)과 용매추출법(LLE)을 각각 적용한 결과, 회수율과 재현성에 있어, HPLC/UV에서는 용매추출법(LLE)보다 고체상추출법(SPE)이 더 우수하였고, GC/FPD에서는 고체상추출법(SPE)보다 용매추출법(LLE)이 더 우수하였다. 또 수돗물 및 하천수(와룡천)에 일정량의 유기인계 농약을 가하여 만든 합성시료중 각 성분을 분석한 결과, SPE-HPLC/UV 법에서는 회수율이 101%, % RSD는 4.3∼8.7이었고, LLE-GC/FPD 법에서는 회수율이 100%, % RSD는 3.2∼9.5이었다. 이 결과는 두 방법 모두 유기인계 잔류농약 분석에 이용할 수 있는 우수한 방법임을 제시하고 있다.

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고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법 (The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque)

  • 안상우;이시진;장순웅
    • 한국환경과학회지
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    • 제13권10호
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.

Electrochemical Determination of Dopamine Based on Carbon Nanotube-Sol-Gel Titania-Nafion Composite Film Modified Electrode

  • Park, Ji-Ae;Kim, Byung-Kun;Choi, Han-Nim;Lee, Won-Yong
    • Bulletin of the Korean Chemical Society
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    • 제31권11호
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    • pp.3123-3127
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    • 2010
  • A highly sensitive electrochemical detection method for dopamine (DA) has been developed by relying on a multiwalled carbon nanotube (CNT)-sol-gel titania-Nafion composite film modified glassy carbon (GC) electrode. The CNT-titania-Nafion/GC electrode exhibited excellent electrocatalytic activity towards DA. Therefore, the CNT-titania-Nafion/GC electrode showed improved voltammetric and amperometric responses for DA compared to those obtained with both titania-Nafion/GC and Nafion/GC electrodes. The CNT-titania-Nafion/GC electrode gave a linear response ($R^2$ = 0.999) for DA from $0.5\;{\mu}M$ to 0.5 mM with a detection limit (S/N = 3) of $0.1\;{\mu}M$ and a good sensitivity of 150 mA/M while other electrodes such as CNT-Nafion/GC, titania-Nafion/GC, and a bare GC gave a sensitivity of 89, 39, and 36 mA/M, respectively. Besides, the CNT-titania-Nafion/GC electrode displayed very fast response time within 2 s. The modified electrode showed good selectivity against ascorbic acid. The modified electrode showed good stability and reproducibility. The CNT-titania-Nafion/GC electrode was applied to the determination of DA in urine and serum samples.

Studies on Determination of Aliphatic Carbamates -Quantitative Analysis of Carisoprodol-

  • Kim, Jeoung-Sook;Kim, Bak-Kwang
    • Journal of Pharmaceutical Investigation
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    • 제15권3호
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    • pp.151-159
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    • 1985
  • For the determination of aliphatic carbamates, the quantitative analysis of carisoprodol was investigated by gab chromatography (GC) and spectrophotometry. All the methods studied were found to be very quantitative. The minimum experimental amounts of GC method, spectrophotometric method I and II were approximately $10^{-9},\;10^{-5}$ and $10^{-8}$ mole, respectively. The obtained results showed that GC method I was much more sensitive and rapid than spectrophotometric method II.

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GC 및 GC/MSD를 이용한 주요 분변 부패산물 신속분석법 (Rapid Analysis of Major Putrefactive Metabolites by GC and GC/MSD)

  • 박규용;김민철;우강융;이나경;백현동
    • KSBB Journal
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    • 제18권1호
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    • pp.74-77
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    • 2003
  • 대표적인 부패산물들로 잘 알려진 indole, skatole, 그리고 $\rho$-cresol 등을 측정하기 위한 방법으로 HPLC, spectrophotometric 법, 그리고 GC 및 GC/MSD 방법 등이 있으며, 수십년 간에 걸쳐 이러한 물질들의 분석이 이루어져 왔다. 본 연구에서는 많은 전처리 과정을 생략하여 분석물의 손실을 최소화하면서 GC 및 GC/MSD를 이용하여 쉽고 빠르게 측정할 수 있는 조건과 방법을 확립하였다. 측정사료는 건강한 성인 남녀의 분변이었으며, 내부 표준물질로 4-isopropylphenol을 사용하였으며, 분변 중 indole의 함량은 10~90 ppm 수준이었으며, skatole의 경우에는 약 40 ppm 정도로 검출되었다. 또한, $\rho$-cresol은 30~300 ppm 수준으로 그 분포 범위가 아주 넓게 나타났었다. GC/MSD를 이용하여 시료 중상기 물질들을 정성적으로 정확히 확인할 수 있었다. DB-17 capillary 컬럼을 이용하여 시료의 전처리 과정을 생략하여도 분석하려던 부패산물의 정성 및 정량에 방해되는 불순 peak는 없었고, 분리능도 매우 우수하였으므로 보다 빠르고 신속하게 상기 물질들을 확인할 수 있었다. 향후 본 연구를 통해 개발된 신속분석법이 분변에 존재하는 주요 부패산물들의 정량에 유용하게 사용되리라 판단된다.

Validation of an analytical method for cyanide determination in blood, urine, lung, and skin tissues of rats using gas chromatography mass spectrometry (GC-MS)

  • Shin, Min-Chul;Kwon, Young Sang;Kim, Jong-Hwan;Hwang, Kyunghwa;Seo, Jong-Su
    • 분석과학
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    • 제32권3호
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    • pp.88-95
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    • 2019
  • This study was conducted to establish the analytical method for the determination of cyanide in blood, urine, lung and skin tissues in rats. In order to detect or quantify the sodium cyanide in above biological matrixes, it was derivatized to Pentafluorobenzyl cyanide (PFB-CN) using pentafluorobenzyl bromide (PFB-Br) and then reaction substance was analyzed using gas chromatography mass spectrometer (GC/MS)-SIM (selected ion monitoring) mode. The analytical method for cyanide determination was validated with respect to parameters such as selectivity, system suitability, linearity, accuracy and precision. No interference peak was observed for the determination of cyanide in blank samples, zero samples and lower limit of quantification (LLOQ) samples. The lowest limit detection (LOD) for cyanide was $10{\mu}M$. The linear dynamic range was from 10 to $200{\mu}M$ for cyanide with correlation coefficients higher than 0.99. For quality control samples at four different concentrations including LLOQ that were analyzed in quintuplicate, on six separate occasions, the accuracy and precision range from -14.1 % to 14.5% and 2.7 % to 18.3 %, respectively. The GC/MS-based method of analysis established in this study could be applied to the toxicokinetic study of cyanide on biological matrix substrates such as blood, urine, lung and skin tissues.

가스크로마토그라피-염광광도 검출기에 의한 혈장중 카르복실기 함유 약물의 정량 (Determination of Carboxyl Drugs by Gas Chromatography-Flame Photometric Detector)

  • 박만기;조영현;유무영;강탁림
    • 약학회지
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    • 제30권4호
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    • pp.180-184
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    • 1986
  • Such carboxyl drugs as mefenamic acid, alclofenac, ketoprofen, cicloxilic acid and tolfenainic acid in rat plasma were determined by the gas chromatography flame photometric detector (GC-FPD). After methylthiomethyl (MTM) esterification with MTM-chloride in 1, 8-diazabicyclo [5.4.0] undec-7-ene (DBU) catalyst, determination of these drugs by this method was tried and compared with that by the GC-flame ionization detector (FID) method in respect to sensitivity and effect of inteferences. The results showed it was possible to analyze with accuracy by this method because of specificity of the FPD, although these drugs were not separated from interferences in plasma on GC column. The GC-FPD method was more sensitive than GC-FID method and the minimum detectable amount of monocarboxylic drugs on 3%, QF-1 column was about 15fmol/injection.

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Determination of N. N-dimethylaniline in penicillins by GC-MS

  • Choi, Jung-Kap;Park, Man-Ki
    • Archives of Pharmacal Research
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    • 제4권2호
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    • pp.85-90
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    • 1981
  • A quantitative GC-MS spectrometric assay was used for the determination of residual N, N-dimethylaniline as a contaminant in commercial penicillin derivatives from various sources. The assay utilizes selective ion focusing to monitor in a GC effluent the molecular ions of DMA generated by electron impact ionization. This method includes dissolution of the sample in alkaline solution, extraction of organic base with cyclohexane and injection into GC-MS with a 3% OV-17 column. Levels of 50 ppb of DMA were easily measured with a coeffecient of varation less than 5 % and recoveries from spiked samples exceeded 97 %. The results of the determinations of DMA in various commercial penicillins were relatively free of this contaminant.

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KGS GC101을 통한 가스시설 폭발위험장소의 설정 (Area Classification of Hazardous Gas Facility According to KGS GC101 Code)

  • 김정환;이민경;길성희;김영규;고영규
    • 한국가스학회지
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    • 제23권4호
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    • pp.46-64
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    • 2019
  • 폭발위험장소의 선정과 거리계산에 대한 상세기술기준 KGS GC101 2018(가스시설의 폭발위험장소 종류 구분 및 범위 산정에 관한 기준)이 제정되어, 2018년 7월 12일부터 시행되었다. IEC60079-10-1 2015 (Explosive atmospheres Part 10-1: Classification of areas - Explosive gas atmospheres)에 대한 전수 내용을 정리하고, 모호한 기준의 해석이나 기준에 대한 가이드라인을 추가하여 제정하였다. KGS GC101은 폭발위험장소 종류의 구분을 위한 방법으로 (1)누출등급의 결정 (2)누출 홀 크기의 결정 (3)누출유량의 결정 (4)희석등급의 결정 (5)환기유효성의 결정을 통하여 최종적으로 (6)위험장소의 결정 (7) 폭발위험장소 범위의 산정을 할 수 있다. 이 과정을 쉽게 계산하기 위하여 Visual Basic for Application (Excel) 언어로 구성한 프로그램(KGS-HAC, C-2018-020632)을 한국가스안전공사에서 제작하였고, 현재 시범 사용 중(2019년 4월 1일 현재 v1.14)에 있다. 그럼에도 불구하고 현장에서 어려워하여, 본 논문을 통하여 코드 및 프로그램의 사용법을 설명하는 것으로 해결코자 한다.