• 제목/요약/키워드: GC and GC-MS method

검색결과 832건 처리시간 0.034초

Identification of Higenamine nad its Metabolites in Rat by Gas Chromatography/Mass Spectrometry

  • Ryu, Jae-chun;Song, Yun-Seon;Kim, Myung-Soo;Cho, Jung-Hyuck;Yunchoi, Hye-Sook
    • Archives of Pharmacal Research
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    • 제16권3호
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    • pp.213-218
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    • 1993
  • ($\pm$)-Higenamine is known as a cardiotonic principle of aconite root (root of Aconitum spp., Ranunculaceae). A simple and sensitive detection method for higenamine was developed by using gas chromatography-mass spectrometry (GC/MS). The recovery of higenamine after extraction and concentration with XAD-2 resin column was around 95% from rat biological fluids such as bile, plasma and urine. The limits of detection of higenamine in these biological fluids were approximately 0.1 ng/ml each. It has well been suggested that tetrahydroisoquinolines possessing catechol moiety such as higenamine should be subjected to the catechol-O-methyl transferase (COMT) activity in vivo. We detected two major peaks of presumed metabolites of higenamine in the total ion chromatogram obtained from the rat urine sample after the oral adminstration of ($\pm$)-higenamine. The scan mass spectrum of one of the metabolties coincided with those obtained from coclaurine $(C_6$-O-methyl higenamine) and those of the other metabolite are suggestive of isococlaurine $(C_7$-O-methyl higenamine).

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Increasing Sulforaphane Formation in Broccoli Sprouts by Radish Sprouts Additions

  • Gi-Chang Kim;Mi Jang;Hab-Hwa Beak;In-Guk Hwang;Hae-Ju Kang;Byung-Soon Hwang;Ji-Young Kim;Chan-Mi Park
    • 한국자원식물학회:학술대회논문집
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    • 한국자원식물학회 2020년도 추계국제학술대회
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    • pp.78-78
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    • 2020
  • Cruciferous plants such as broccoli and radish contain glucosinolate, which is a bioactive precursor that is most often used in Korean foods and is unique as a food ingredient. In addition, it contains various other phytochemicals and is promising as a health-oriented food material. In particular, Sulforaphane is a hydrolyzate of the glucosinolate, which has a more beneficial effect on the human body. Glucosinolate may be hydrolyzed by enzymes called myrosinase, which is voluntarily possessed by cruciferous plants. However, the ESP(Epithiospecifier protein) in broccoli sprouts could acts competitively with myrosinase, and convert to the less bioactive sulforaphane nitrile form. Therefore, we improved the yielding of sulforaphane in broccoli sprouts with a new method. We induce inactivation of the ESP protein by heat treatment. At this time, a myrosinase was introduced from the radish sprout because myrosinase in broccoli sprouts is also denatured by heat treatment. According to the results, we have confirmed by GC / MS that formation of sulforaphane increases more than 7 fold using set heating and mixing conditions.

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제품담배의 공기희석율에 따른 주류연중 휘발성 유기화합물의 이행특성 (A Study on the Delivery of Volatile Organic Compounds in Cigarette Mainstream Smoke with a Different Ventilation Rate)

  • 지상운;황건중;이문수;신창호;김수호;김종열;김미주
    • 한국연초학회지
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    • 제26권2호
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    • pp.179-185
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    • 2004
  • This study was conducted to investigate the delivery pattern of volatile organic compounds(VOCs) in mainstream smoke generated by the combustion of a different ventilated cigarette. To compare the delivery pattern and the concentration of VOCs in mainstream smoke, the six different ventilated cigarette was manufactured and analyzed VOCs using the GC/MS. As a result of this experiments, cambridge filter used to trap the particulate matter in mainstream smoke did not affect on the trapping of VOCs components, and two impinger method among the trapping methods was the best condition to trap VOCs from mainstream smoke. As the slope of the delivery of VOCs such as isoprene, acrylonitrile and toluene were higher than 1, but that of benzene was lower than other VOCs.

가지제(加脂劑) 생산공정에서 배출되는 악취원인물질 연구 (The Study of Odor-causing Compounds Emitted from a Stuffing Agent Production Process)

  • 서용수;서정민
    • 한국환경과학회지
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    • 제27권9호
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    • pp.781-788
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    • 2018
  • The volatile odor compounds emitted form a stuffing agent production process were quantified by ATD and GC-MS, and then odor causing compounds were identified by the method of EOI using each TLV. As the results, 72 odor compounds were detected and total concentration was turned up 87.6 ppmv level. In these compounds, aldehyde group is higher 45.49 ppmv than others group, the next is turn up the order of aliphatics, alcohols, esters, ketones. The EOA of aldehyde group show up 101,720 and 97.2%, respectively, the odor causing compounds were identified each of odor 2-Octenal 28.31%, Hexanal 24.06%, Valeraldehyde 16.07%, Butyraldehyde 9.69%, Heptanal 4.97%, Propionaldehyde 4.64%, Acetaldehyde 3.31%. The TLVs of 7 major odor compounds are lower value level of 0.001~0.0001 ppmv, odor causing even in trace level. We need to be concerned with reduction of aldehyde compounds in the odor problem by a stuffing agent production process or ironing process of the textile containing a stuffing agent.

SPME법을 이용한 식물정유 성분분석을 통한 유해가스 제거 특성연구 (Study of Toxic Gas Removal Characteristics by Chemical Analysis of Essential Oil using SPME Method)

  • 박영규
    • KSBB Journal
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    • 제19권3호
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    • pp.231-235
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    • 2004
  • 본 논문은 식물정유를 이용해 유해가스를 처리하는 경우에 식물정유의 주요구성성분을 파악하고 이를 통해 처리효율을 규명하는데 연구하였다. 또한 식물정유와 암모니아 가스에 의한 암모니아 제거반응 메카니즘을 규명하였으며 그 결과는 아래와 같다. 1) 암모니아 가스는 중화반응에 의해 처리되는 경우에 식물정유의 화학구조에서 알코올기, 알데히드기 그리고 에스터기가 관여한다는 것을 밝혀냈다. 실험결과 앞서 언급한 화학작용기가 포함되어 있는 경우에 암모니아 가스와 중화반응으로 염을 형성하여 유해가스 제거과정을 갖는다 2) 암모니아가스를 제거하는 중화반응의 경우에 온도와 pH에 따라 처리효율을 크게 달라졌으며 온도는 높은 온도보다는 적정 온도에서 제거효율이 거의 98%이상 제거되었으며 적정 pH는 pH가 중성인 경우에 최고의 처리효율이 얻어졌다. 3) 암모니아 가스의 처리효율은 식물정유을 통해 20분 이내에 암모니아 가스 처리 효율이 98% 이상 처리되는 것으로 나타났다.

유류화재증거물의 정성적 분석 기법 연구 (Qualitative Analysis of Ignitable Liquid Residues in Extracts from Fire Debris Samples)

  • 한동훈;이성룡;김수영
    • 한국화재소방학회논문지
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    • 제25권6호
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    • pp.14-20
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    • 2011
  • 다양한 원인과 우연에 의해 발생하는 화재에 관하여, 화재조사관이 현장의 증거물, 화재패턴으로부터 화재원인을 밝혀내기란 쉽지 않다. 본 연구는 다양한 화재 원인 중의 하나인 유류화재와 관련된 화재증거물에서 잔존물을 추출하여 분석하는 것이다. 본 연구에서는 ASTM E 1618에 근거한 유류화재 증거물 속에 잔존유류를 분석하는 기술(다양한 전처리법을 통한 가스크로마토그래프/매스스펙트로미터 분석)을 이용하여 시중에서 유통되는 유류를 먼저 분석한 후, 유류화재 실험을 통한 증거물을 채집하여 분석을 수행하였다. 화재 후 채집 시간, 전처리 방법에 따라 토탈이온크로마토그램의 패턴이 달라지는 것을 관찰하였다.

고성능 액체크로마토그래피와 질량분석법을 이용한 농산물 중 Phenothrin 및 Silafuofen의 정밀 잔류분석법 개발 (High-Performance Liquid Chromatographic Determination of Phenothrin and Silafluofen Residues in Crops with Mass Spectrometric Confirmation)

  • 이영득;오재호;장상원
    • 농약과학회지
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    • 제15권4호
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    • pp.389-400
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    • 2011
  • 고성능 액체크로마토그래피를 이용하여 농산물 중 살충제 phenothrin과 silafluofen 잔류량을 정밀하게 측정할 수 있는 공정 잔류분석법을 개발하고자 하였다. 현미, 사과, 고추 및 배추의 4종 대표 농산물 시료로부터 분석성분들을 acetone으로 동시에 추출하고 액-액 분배 및 Florisil 흡착크로마토그래피로 정제하는 시료 조제과정을 최적화하였다. 현미 및 고추 시료의 경우 acetonitrile/n-hexane 분배법을 추가하여 유지를 포함한 비극성 간섭물질을 제거하였다. HPLC에서 역상 C18 column과 경사용리법을 사용, 대상 성분들과 시료 중 간섭물질을 완전 분리하였으며 자외흡광검출기를 이용하여 고감도로 분석하는 것이 가능하였다. 확립된 분석법의 정량한계는 회수율 시험을 통하여 명확히 확인한 결과, phenothrin 및 silafluofen이 각각 0.02 및 0.01 mg/kg 이었다. 대표 농산물 4종에 대상 농약을 3수준 3반복으로 수행하여 얻은 분석법의 회수율은 phenothrin 및 silafluofen이 각각 82.4~109.8% 및 83.7~109.8% 범위였으며 분석오차는 농산물 종류 및 처리수준에 관계없이 10% 미만이었다. 시료 중 검출된 대상 성분의 재확인을 위하여 LC/MS 및 GC/MS법을 추가로 확립하여 분석결과의 정성적 신뢰성을 확보하였다. 개발된 분석법은 높은 감도와 양호한 회수율 그리고 낮은 분석오차를 감안할 때 국가 공정분석법으로 충분히 이용 가능하였다.

Studies on the Analysis of Benzo(a)pyrene and Its Metabolites on Biological Samples by Using High Performance Liquid Chromatography/Fluorescence Detection and Gas Chromatography/Mass Spectrometry

  • Lee, Won;Shin, Hye-Seung;Hong, Jee-Eun;Pyo, Hee-Soo;Kim, Yun-Je
    • Bulletin of the Korean Chemical Society
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    • 제24권5호
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    • pp.559-565
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    • 2003
  • An analytical method the determination of benzo(a)pyrene (BaP) and its hydroxylated metabolites, 1-hydroxybenzo(a)pyrene (1-OHBaP), 3-hydroxybenzo(a)pyrene (3-OHBaP), benzo(a)pyrene-4,5-dihydrodiol (4,5-diolBaP) and benzo(a)pyrene-7,8-dihydrodiol (7,8-diolBaP), in rat urine and plasma has been developed by HPLC/FLD and GC/MS. The derivatization with alkyl iodide was employed to improve the resolution and the detection of two mono hydroxylated metabolites, 1-OHBaP and 3-OHBaP, in LC and GC. BaP and its four metabolites in spiked urine were successfully separated by gradient elution on reverse phase ODS $C_{18}$ column (4.6 mm I.D., 100 mm length, particle size 5 ㎛) using a binary mixture of MeOH/H₂O (85/15, v/v) as mobile phase after ethylation at 90 ℃ for 10 min. The extraction recoveries of BaP and its metabolites in spiked samples with liquid-liquid extraction, which was better than solid phase extraction, were in the range of 90.3- 101.6% in n-hexane for urine and 95.7-106.3% in acetone for plasma, respectively. The calibration curves has shown good linearity with the correlation coefficients (R²) varying from 0.992 to 1.000 for urine and from 0.996 to 1.000 for plasma, respectively. The detection limits of all analytes were obtained in the range of 0.01-0.1 ng/mL for urine and 0.1-0.4 ng/mL for plasma, respectively. The metabolites of BaP were excreted as mono hydroxy and dihydrodiol forms after intraperitoneal injection of 20 mg/kg of BaP to rats. The total amounts of BaP and four metabolites excreted in dosed rat urine were 3.79 ng over the 0-96 hr period from adminstration and the excretional recovery was less than 0.065% of the injection amounts of BaP. The proposed method was successfully applied to the determination of BaP and its hydroxylated metabolites in rat urine and plasma for the pharmacokinetic studies.

수증기 증류시 분산매의 조성이 냉이의 휘발성 향기성분의 강도 및 정유 회수율에 미치는 영향 (The Effect of Dispersion Medium on Intensity of Volatile Flavor Components and Recovery of Essential Oil from Capsella bursa-pastoris by Steam Distillation)

  • 최향숙;이미순
    • 한국식품과학회지
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    • 제28권5호
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    • pp.827-833
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    • 1996
  • 연속증류추출(SDE) 장치를 이용하여 냉이로부터 휘발성 향기성분을 추출할 때 분산매의 조성(pH, 당 및 염)에 따른 향기성분의 강도 및 회수율을 조사하였다. 분산매의 pH를 3, 5, 7및 9로 하여, 각 pH에 따른 휘발성 향기성분의 변화 패턴 및 냉이로부터의 휘발성 향기성분 추출에 가장 적합한 pH를 조사한 결과 분산매의 pH가 7일 때 총 51종의 가장 다양한 휘발성 성분이 확인되었으며 냉이로부터 휘발성 향기성분을 추출할 때 중성 pH 부근에서 수증기 증류하는 것이 향기성분의 구성 및 회수율 측면에서 가장 바람직함을 알 수 있었다. 냉이를 수증기 증류할 때 분산매의 sucrose 농도가 10%, 20% 및 40%로 증가함에 따라 획득된 정유량은 각각 18.1 mg, 29.0 mg 및 33.4 mg으로 40% sucrose용액에 의하여 증류할 때 정유 회수율이 가장 높게 나타났다. 또한 sucrose 농도가 증가할수록 확인된 휘발성 향기성분의 종류가 다양하였으며 10%, 20% 및 40% socrose 용액으로 증류할 때 각각 27종, 32종 및 38종이 확인되었다. 냉이의 수증기 증류시 분산매의 surcrose 농도가 증가함에 따라 향기를 구성하는 휘발성 성분의 수는 더욱 다양하였으나 양적인 측면에서는 각 성분마다 다른 양상을 보였다. 2%, 8% 및 15% NaCl용액으로 냉이를 수증기 증류하여 얻어진 정유의 함량은 각각 33.0 mg, 12.5 mg 및 22.4 mg으로 2% NaCl용액을 사용하였을 때 정유의 회수율이 가장 좋았으나 15% NaCl용액으로 증류할 때 가장 많은 수인 22종의 휘발성 성분이 검출 및 확인되었다.

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시설재배 부추(Allium tuberosum R.)와 쪽파(Allium wakegi Araki) 중 α-Cypermethrin과 Deltamethrin의 잔류특성 및 안전성 평가 (Study on Residual Properties and Risk Assessment of α-Cypermethrin and Deltamethrin in the Chives (Allium tuberosum R.) and Spring onion (Allium wakegi Araki))

  • 조영주;최정윤;함헌주;허장현
    • 한국환경농학회지
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    • 제41권1호
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    • pp.55-64
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    • 2022
  • BACKGROUND: This study was conducted to evaluate the residual characteristics and safety assessment of αcypermethrin and deltamethrin in minor crops, chives and spring onion cultivated in greenhouse. METHODS AND RESULTS: The insecticides α-cypermethrin 2% EC and deltamethrin 1% EC used in the experiment were diluted 1,000 times and then sprayed on chives and spring onion twice with 1-week intervals at 0, 7, 14, and 21 days before harvest. The residual insecticides were extracted from the minor crops using QuEchERS method and analyzed by GC-MS/MS. The average initial residues of α-cypermethrin and deltamethrin in chives after 21 days decreased from 2.74 to 0.82 mg/kg and 1.12 to 0.16 mg/kg, respectively. Similarly, in spring onion the residues after the same periods decreased from 0.26 to <0.01 mg/kg for α-cypermethrin and from 0.07 to <0.01 mg/kg for deltamethrin. CONCLUSION(S): The PHIs (pre-harvest intervals) for α-cypermethrin and deltamethrin in chives are recommended as 14 days before harvest with twice applications of the pesticides, whereas for α-cypermethrin in spring onion PHI of 7 days before harvest is recommended with 3 times of applications and PHI of 21 days for deltamethrin. The theoretical maximum daily intakes of cypermethrin and deltamethrin were 68.8% and 64.2%, respectively, indicating that residues of both compounds did not pose considerable health risks to consumers.