• Title/Summary/Keyword: 가스크로마토그라피 질량분석

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Determination of Polycyclic Aromatic Hydrocarbons in Chinmey Soot Extract by High-Resolution Gas Chromatography (고분리능 기체크로마토그라피에 의한 굴뚝재추출물안의 다환방향족 탄화수소의 정량에 관한 연구)

  • 서영화;이광우;허귀석
    • Journal of Korean Society for Atmospheric Environment
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    • v.4 no.2
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    • pp.11-19
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    • 1988
  • 대기오염물질 속에 함유되어 있는 다환방향족 탄화수소 (PAHs)는 분자식 구조가 비슷한 수십개의 이성질체가 여러 종류의 유기화합물과 혼합되어 존재한다. 본 연구에서는 환경오염 시료중의 PAHs를 분석하는데 있어서 분석방법과 결과를 비교하기 위하여 지침이 될 수 있는 환경표준 기준물을 개발할 목적으로 굴뚝 안쪽벽에서 긁어 채취한 검댕을 시료로 선책하여 액체/액체 용매 추출방법에 의해 PAHs 분류부분을 얻었다. Phenanthrene 이외의 30여종의 PAHs 화합물을 가스크로마토그라피의 머무른시간과 가스크로마토그라피/질량분석기에 의하여 분리, 판명하였고 5종의 주 PAHs 화합물을 정확하게 정량 분석하였다. 정량분석 결과의 신뢰도, 정확도, 정밀도는 미국 NBS의 표준기준물 1647을 분석하여 검정치와 비교함으로써 평가하였다.

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Analysis of the Degradation Products of Turmeric using GC-MS (GC-MS법을 이용한 울금의 퇴화물 분석)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.31 no.6 s.165
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    • pp.859-868
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    • 2007
  • Degradation products of the dye extracted from turmeric and the turmeric dyed textiles were examined by using GC-MS after 100 oven (OV) and $H_2O_2/UV/O_2$(PER) treatments for up to 28 days. Throughout the OV degradation times, 2-propenoic acid, 3-(2-hydroxyphenyl)- was found consistently, while isovanillin, and vanillic acid were newly detected. In 28 day PER degradation sample, feruloylmethane, 2-propenoic acid, 3-(2-hydroxyphenyl)-, benzoic acid, and vanillic acid were detected as well as isovanillin. Feruloylrnethane, and 2-propenoic acid, 3-(2-hydroxyphenyl)- were detected from the degraded fabric samples. With the absence of curcuminoids in the GC-MS result, the decreasing pattern of 2-propenoic acid, 3-(2-hydrokyphenyl)- reflect the degradation of curcuminoids in turmeric extraction with the progression of OV degradation times. It is suggested that isovanillin, feruloylmethane, 2-propenoic acid,3-(2-hydroxyphenyl)-, and vanillic acid are the probable fingerprint products for determining the turmeric dye from the badly faded archaeological textiles.

Comparison of TLC and GC-MS Method in the Analysis of Dye Extracted from Madder Plant (꼭두서니 추출염료에 대한 TLC와 GC-MS 분석법의 비교 연구)

  • ;S. Kay Obendorf
    • The Research Journal of the Costume Culture
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    • v.12 no.4
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    • pp.579-590
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    • 2004
  • This research was aimed to investigate and compare the effectiveness of TLC and GC-MS methods in the analysis of chromophoric substances extracted from madder plant. Alizarin and purpurin 0.3% solution were used as comparative standards; madder extraction was prepared by heating the solution of powdered madder at 80℃, pH 1.5, for 90 min. Best elution solvent for TLC in silica gel plate was toluene:ethyl acetate=9:1, which resulted in red and yellow spots from madder extraction each of which showed R/sub f/ values 0.32-0.43 and 0.07-0.11. Although the red spot in particular exhibited similar characteristics as standard purpurin in color, shape, and R/sub f/ values, the result was inconsistent throughout different TLC trials. GC-MS analysis showed only small amount of alizarin and no purpurin in the madder extraction. Other chromophoric substance such as 2-furancarboxaldehyde, 5-(hydroxymethyl)-, anthralin, and danthron were also detected in small amounts. The result indicated that TLC was less sensitive to detecting and identifying the natural dyestuff which is generally constituted with a number of similar but chemically different chromophoric substances.

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Production of T-2 Toxin and Its Metabolites by Fusarium sporotrichioides Isolates from the Corn Producing Area in Korea (우리나라 옥수수산지에서 분리한 Fusarium sporotrichioides 균주들에 의한 T-2 독소 및 관련 대사물의 생성)

  • Lee, Yin-Won;Kim, Kook-Hyung;Chung, Hoo-Sup
    • The Korean Journal of Mycology
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    • v.18 no.1
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    • pp.13-19
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    • 1990
  • Four isolates of Fusarium sporotrichioides obtained from the corn producing area were tested for their toxicities by feeding the crude cultures to rats. Three out of four isolates were highly toxic and killed all rats within 3-4 days after feeding. The chemical analyses of toxic cultures by thin layer chromatography and gas chromatography-mass spectrometry revealed that two isolates from Jeongsun district produced T-2 toxin and its related trichothecenes. This is the first report that F. sporotrichioides isolates produce T-2 toxin in Korea.

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Separation of Chromophoric Substance from Sappanwood under Different Extraction Conditions (염료 추출조건에 따른 소목의 색소성분 분리 거동)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.31 no.12
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    • pp.1653-1661
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    • 2007
  • The research aimed to establish the standard extraction procedure for examining brazilin, the major chromophoric substance of Sappanwood, using GC-MS with the ultimate goal of identifying the sappanwood dye in severely faded archaeological textiles. The amount of brazilin represented by the GC abundance was the largest when acetone was used as the extraction medium, followed by methanol. Shaking plate operated at room temperature was more effective than the waterbath shaker which was operated at $30^{\circ}C$. In both cases, the extraction method which incorporated one hour pre-soaking before the 12 hours of actual extraction resulted in a larger amount of brazilin detection than the extraction procedure without the one hour pre-soaking. In case of water extraction, pH 5 resulted in the most effective pH level for the extraction of brazilin, The best GC-MS parameter for detecting brazilin was to set the column temperature initially at $50^{\circ}C$. gradually increase to $210^{\circ}C$ at a $23^{\circ}C/min$ rate, finally increase to $305^{\circ}C$ at $30^{\circ}C/min$ rate, and hold for 14 minutes, and the MSD scan range at $75{\sim}400m/z$.

Analysis of Degradation Products in Madder Dyed Fabrics in Selective Degradation Conditions (퇴화조건에 따른 꼭두서니 염색물의 퇴화물 연구)

  • Ahn, Cheun-Soon;Obendorf, S.-Kay
    • Journal of the Korean Society of Clothing and Textiles
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    • v.29 no.12 s.148
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    • pp.1608-1618
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    • 2005
  • The purpose of this investigation was to investigate the degradation products of the dye component extracted from madder dyed fabrics using the GC-MS analysis and to evaluate the change of color due to degradation treatment. Four different degradation protocols were used in this study,; refrigeration at $7^{\circ}C$ (LT), room temperature (RT), oven treatment at $100^{\circ}C$ (OV), and $H_2O_2/UV(PER)$ method. Degradation times for each thermal system were 6 hour, 24 hour, 48 hour, 1 week, 2 week, 4 week. Alizarin was detected from the control and degraded samples of both alizarin dyed and madder dyed fabrics. Benzoic acid, 2, 4-di-tert-butylphenol, phthalic anhydride were detected as the degradation products for both alizarin dyed and madder dyed fabrics. The result suggest that these products can be used as the fingerprints of GC-MS analysis for the identification of madder dye in archaeological textiles. Both alizarin dyed and madder dyed samples became less red and less yellow after degradation. In the PER degradation system madder dyed sample showed the greatest color difference even after 1 week of degradation treatment. Further research is necessary for investigating the color change in the exhumed textiles, which is caused by the dual action of dye fading and the staining of organic matters in the soil.

Separation of Chromophoric Substance from Amur Cork Tree Using GC-MS (GC-MS를 이용한 황벽의 색소 성분 분리 거동)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.33 no.6
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    • pp.980-989
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    • 2009
  • Amur cork tree was extracted in methanol with the purpose of investigating the most effective extraction procedure for detecting the chromophore using the GC-MS analysis. Different procedures of waterbath and hotplate extractions were carried out and five different GC-MS instrument parameters including the operating temperatures in the GC capillary column and the MSD scan range were tested for their efficiencies. Berberine was determined by the detection of dihydroberberine at 15.0 min r.t. Hotplate was a better device for extracting amur cork tree than waterbath shaker either with or without presoaking in the room temperature. Water was not an adequate extraction medium for the berberine detection. The most effective GC-MS parameter was Method 4; the initial temperature at $50^{\circ}C$ followed by the temperature increase of $23^{\circ}C$/min until $210^{\circ}C$, then increase of $30^{\circ}C$/min until the final temperature reach at $305^{\circ}C$, then hold for 14 minutes to maintain the total run time 24.12 minutes. The MSD scan range for Method 4 was $35\sim400$m/z.

Evaluation of Exposure to Pyrethroid Pesticides according to Sprayer Type using Biological Monitoring (생물학적 모니터링을 이용한 분무기 형태에 따른 피레스로이드 농약 노출량 평가)

  • Song, Jae Seok;Choi, Hong Soon;Yu, Ho Young;Park, Byung Gon;Kwon, Daeho
    • The Korean Journal of Pesticide Science
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    • v.20 no.4
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    • pp.300-304
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    • 2016
  • The aim of this study were to evaluate the exposure level of pyrethroid pesticide according to spraying machine type. The urinary metabolites of pyrethroid pesticide in apple farmers were analyzed to determine the exposure level of pyrethroid pesticide. The result shows that, the spraying volume was greater in SS sprayer group than in power sprayer group. But multi variate analysis which adjust spraying volume and field area, there were no difference of urinary metabolites between two sprayer machine. To make more accurate model of pesticide exposure, the factors influencing pesticide exposure should be determined and further study should be done.

Analysis of $\triangle^9$-Tetrahydrocannabinol and 11-nor-9-carboxytetrahydrocannabinol in Hair by Gas Chromatography/Mass Spectrometry (가스크로마토그라피/질량분석기에 의한 모발중 대마성분 분석)

  • 양원경;한은영;박용훈;임미애;정희선
    • YAKHAK HOEJI
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    • v.48 no.3
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    • pp.207-212
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    • 2004
  • An analytic method was developed for the quantitation of $\Delta$$^{9}-$ tetrahydrocannabinol (THC) and 11-nor-9-carboxy THC (THC-COOH) in human hair. After hair samples were pulverized using Freezer Mill, deuterated internal standards were added and digested in 1 N NaOH at $100^{\circ}C$ water bath for 30 min. Digest solutions were extracted by 5 ml hexane:ethyl acetate (90:10) after acidification with acetic acid. The organic phase was evaporated under N 2 and derivatized by BSTFA (with 1% TMCS) at $85^{\circ}C$ for 45 min. The derivatized solution was separated on HP-5MS column ($30m{\times}0.25mm{\times}0.25mm$) and detected using EI-GC-MS with selective ion monitoring mode. The assay of calibration was ranged from 5 to 100 ng/50 mg hair ($r^2$>0.99) for THC and THC-COOH. Within and between-run precision were calculated at 6, 30, 60 ng/50 mg hair with coefficients of variation less than 11%. Within and between run accuracies at the same concentrations were$\pm$14% and $\pm$30% of target for both analytes, respectively. Absolute and relative recovery at 10 and 100 ng were 60∼91%. The method was used to detect and quantify THC and THC-COOH in cannabis abuser's hairs (N = 16) and SRM (N=5, THC 1 ng/mg, NIST). We detected THC and THC-COOH in only one hair sample. In SRM, % accuracy was 93% (range 86∼103%) and precision (% CV) was 8.14. We began to set up a quantitative analysis of THC and THC-COOH using EI-GC-MS. Continuously, we need to modify and develop this method in order to apply for identification in cannanbis users' hair.