• 제목/요약/키워드: GC/MS spectrometry

검색결과 752건 처리시간 0.029초

생체시료 중 Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate의 동시정량 (Simultaneous Determinaton of Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate in Biological Samples)

  • 김종훈
    • 분석과학
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    • 제14권2호
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    • pp.95-102
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    • 2001
  • 쇠고기 돼지고기 속에 포함된 nonylphenol, octylphenol, bis(2-ethyltexyl) phthalate의 동시 정량방법을 연구하였다. 이 방법에서는 밀폐된 배양시험관에서 이염화메탄을 이용하여 추출하고 용매를 이소헥산으로 바꾸고 aminopropyl 칼럼(2g)을 이용하여 분리한 후 GC/MS-SIM 방법으로 분석하였다. 다중점보정을 위한 nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl) phthalate(BEHP)의 회수율에서 NP, OP는 $0.125-12.5{\mu}g/g$, BEHP는 $0.0125-12.5{\mu}g/g$ 범위에서 좋은 회수율을 보였다. 확립된 방법을 전주시와 전주시 근교 마트와 정육점에서 구입한 16점의 쇠고기 돼지고기 시료에 적용하였다. Nonylphenol은 4점의 시료에서 검출되었으며 bis(2-ethlhexyl) phthalate는 전 시료에서 검출되었고, 그 농도범위는 $0.06-0.24{\mu}g/g$$0.36-2.35{\mu}g/g$ 이었다. Octylphenol은 어떠한 시료에서도 검출되지 않았다. 이 방법은 매우 적은량의 생체 시료에도 쉽게 적용이 가능하였다.

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Development of Analysis Condition and Detection of Volatile Compounds from Cooked Hanwoo Beef by SPME-GC/MS Analysis

  • Ba, Hoa Van;Oliveros, Maria Cynthia;Ryu, Kyeong-Seon;Hwang, In-Ho
    • 한국축산식품학회지
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    • 제30권1호
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    • pp.73-86
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    • 2010
  • The current study was designed to optimize solid phase microextraction (SPME)-GC-MS conditions for extraction and analysis of volatile components for Hanwoo beef and to establish a tentative database of flavor components. Samples were taken from Hanwoo longissimus muscle (30 mon old steer, $1^+B$ carcass grade) at 24 h postmortem. Results indicated that the optimum adsorption time for $75{\mu}m$ CAR/PDMS fiber was 60 min at $60^{\circ}C$. Thermal cleaning at $250^{\circ}C$ for 60 min was the best practice for decontamination of the fiber. A short analysis program with a sharp oven temperature ramp resulted in a better resolution and higher number of measurable volatile components. With these conditions, 96 volatile compounds were identified with little variation including 22 aldehydes, 8 ketones, 31 hydrocarbons, 12 alcohols, 8 nitrogen- and sulfurcontaining compounds, 5 pyrazines and 10 furans. A noticeable observation was the high number of hydrocarbons, aldehydes, ketones, alcohols and 2-alkylfurans which were generated from lipid decomposition especially the oxidation and degradation of unsaturated and saturate fatty acids. This implies that these compounds can be candidates for flavor specification of highly marbled beef such as Hanwoo flavor.

기체 크로마토그래피/질량분석법을 이용한 요 중에서의 유기산 분석 (Analysis of Organic Acids in Urine by Gas Chromatography/Mass Spectrometry)

  • 유은아;고선영;김종원;김정욱;명승운
    • 대한화학회지
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    • 제41권9호
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    • pp.471-482
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    • 1997
  • 기체크로마토그래피/질량분석법(GC/MS)을 이용하여 소변 내에 존재하는 유기산들을 동시에 분리 정량분석할 수 있는 최적의 분석조건을 확립하기 위해 액체-액체추출법을 이용하여 분리하였고 이 때 pH의 영향 및 역추출방법과 그리고 옥심화 과정 첨가의 효과를 알아보았다. 그 결과 옥심화 과정 없이 pH가 0.5일 때 회수율이 좋았고 RSD값은 0.3-12.4%로 가장 적었다. 역추출과정을 통하여 방해물질이 제거되어 15-16분대의 머무름 값을 갖는 몇가지 유기산 검출이 확실시 되었다. 이를 토대로 51종의 유기산들에 대한 검량곡선을 작성하여 한국 정상어린이(n=16) 요시료 중의 유기산 함량분포를 얻었다.

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저니토중 Polychlorinated Biphenyls(PCBs) 정량에 관한 연구 (A Study on Quantitation of Polychlorinated Biphenyls (PCBs) in Sediments)

  • 신호상;오윤숙
    • 분석과학
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    • 제12권2호
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    • pp.151-158
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    • 1999
  • 국내 4대강 주요 하천 저니토양중 PCB 오염도를 각 congener별로 또는 총량으로서 GC/MS를 사용하여 정량하였다. 그 결과 4대강의 주요 지천중 SS지점 근처의 저니토에서 총 PCBs가 가장높은 $290.87{\mu}g/kg$이었고 OS지점에서도 비교적 높은 $221.11{\mu}g/kg$이었으며 저니중 유기물 함량과 상관관계가 있었다. Congener-specific analysis에 의해 하천수 및 저니토 시료에서 공통적으로 검출된 대표적 congener는 IUPAC No 66, 74, 90, 101, 105, 110, 118, 138, 149, 153, 180, 187였다. 본 연구결과 저니토에서는 tetraCBs 및 pentaCBs가 다른 polyCBs에 비해 비교적 높은 농도로 검출되었다. 이상의 연구결과를 통해 국내의 주요 하천의 저니토중 PCB의 오염정도는 매우 심각한 정도는 아니나 좀더 많은 시료를 분석하는 정말조사가 필요하다.

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Effect of Charcoal Broiling on the Formation of Volatile Compounds in Gamma-Irradiated Dakgalbi, a Korean Chicken-Based Food

  • Kang, Geon-Ok;Yoon, Young-Min;Kim, Jae-Kyung;Song, Beom-Seok;Byun, Eui-Baek;Kim, Jae-Hun;Lee, Ju-Woon;Park, Jong-Heum
    • 한국축산식품학회지
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    • 제33권5호
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    • pp.603-609
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    • 2013
  • The purpose of this study is to evaluate the change of volatile compounds in Dakgalbi cooked by charcoal broiling. Fresh deboned and marinated chicken meat was cooked by electric-pan frying or charcoal broiling and subsequently irradiated with a dose of 0, 10 and 20 kGy. Volatile components from Dakgalbi were analyzed using solid phase micro-extraction gas chromatography - mass spectrometry (SPME GC-MS) and identified through the comparison of mass spectrum database. SPME GC-MS analysis shows that a total of 32 volatiles were identified. Among them, aldehydes such as hexanal and octanal, which have relevance to off-flavors such as green, paint, metallic, bean and rancid were detected in Dakgalbi cooked by both methods. However, the contents were less detected in the Dakgalbi cooked by charcoal broiling than in the Dakgalbi cooked by electric-pan frying. Gamma-irradiation caused the change in the formation of these aldehydes in cooked Dakgalbi. The irradiation significantly increased the contents of hexanal and octanal in Dakgalbi cooked by electric-pan frying and a similar increase was found in Dakgalbi cooked by charcoal broiling. However, the contents of the off-flavors were much less in the latter. The results suggest that charcoal broiling might be more effective than electric-pan frying for the reduction of the contents of off-flavor such as hexanal and octanal increased in Dakgalbi by gamma-irradiation.

계지(桂枝)에서 정제한 보체계 활성화 다당의 작용양식과 당쇄구조 (Activation Mode and Glycosidic Linkage of Anti-Complementary Polysaccharide Isolated from Young Stems of Cinnamomum cassia Blume)

  • 나경수;안현정;권미향
    • 한국식품영양과학회지
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    • 제26권2호
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    • pp.248-253
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    • 1997
  • 계지에서 분리한 보체계 활성화 다당의 보체 활성화양식과 다당의 당쇄결합에 관하여 검토하였다. 계지 보체계 활성화 다당획분들(CC-IIIa, CC-IIIb, CC-IIIc)들은 정상인의 혈청중에 존재하는 주요 보체성분인 C3를 활성화하여 C3a와 C3b 보체 산물을 생성 시켰는데 이 과정은 anti-human C3를 이용한 면역전기영동을 실시하여 확인하였다. $Ca^{++}$ 유무시의 보체계 활성을 측정한 결과 계지에서 분리된 CC-IIIa-3는 고전적 경로(classical pathway)와 부경로(alternative pathway)를 동시에 활성화시킴을 확인하였다. CC-IIIa-3을 메틸화하여 GC/MS로 분석한 결과 비환원 말단의 galactopyranose와 glucopyranose가 확인되었고 1,2-linked rhamnopyranose, 1,6-linked mannopyranose, 1,3-linked glucopyranose, 1,6-linked galactopyranose 등이 확인되었다.

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Anticholinesterase activity of Cinnamomum zeylanicum L. leaf extract

  • Dalai, Manoj Kumar;Bhadra, Santanu;Chaudhary, Sushil Kumar;Chanda, Joydeb;Bandyopadhyay, Arun;Mukherjee, Pulok K.
    • 셀메드
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    • 제4권2호
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    • pp.11.1-11.6
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    • 2014
  • Cinnamomum zeylanicum (C. zeylanicum) is a tropical evergreen tree of Lauraceae family. It is one of the oldest culinary spices known and used traditionally in many cultures for centuries. In addition to its culinary uses, cinnamon also possesses as a folk remedy of many health disease condition including analgesic, antiseptic, antispasmodic, aphrodisiac, astringent, carminative, haemostatic, insecticidal, and parasiticide and memory enhancing property. This study was aimed to assess the acetylcholinesterase and butyrylcholinesterase inhibitory activity of standardized methanol extract of the C. zeylanicum. Gas chromatography - mass spectrometry (GC-MS) and high performance liquid chromatography (HPLC) analysis were done to identify the presence of eugenol as chemical component and support the neuroprotective activity in the extract. Anticholinesterase inhibitory activity of crude methanol extract of C. zeylanicum leaves and cinnamon oil were evaluated by 96-well microtiter plate assay and thin layer chromatography bioassay detection methods. This study revealed that cinnamon oil ($IC_{50}:45.88{\pm}1.94{\mu}g/ml$) has better anticholinesterase activity than methanol extract ($IC_{50}:77.78{\pm}0.03{\mu}g/ml$). In HPLC analysis, retention time of eugenol in cinnamon oil was found to be 15.81 min which was comparable with the retention time (15.99 min) of the reference standard, eugenol. Seven chemical compounds were identified by GC-MS analysis, in which eugenol as an important phytoconstituents. Thus the phytochemicals from C. zeylanicum methanol leaves extract could be developed as potential source of anticholinesterase activity, with particular benefit in the symptomatic treatment of Alzheimer's disease.

흡착튜브 - 열탈착 정량분석 기법에 기반한 과일시료로부터 자연적 휘발성유기화합물의 배출특성 연구 (Biogenic Volatile Organic Compounds (BVOC) Emissions from Fruit Samples Based on Sorbent Tube Sampling and Thermal Desorption (ST-TD) Analysis)

  • 안정현;김기현
    • 한국대기환경학회지
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    • 제29권6호
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    • pp.757-772
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    • 2013
  • In this study, a combination of sorbent tube (ST)-thermal desorption (TD)-gas chromatography (GC)-mass spectrometry (MS) was used for quantitative analysis of liquid phase standards of 10 BVOC ((1) (+)-${\alpha}$-pinene, (2) (+)-${\beta}$-pinene, (3) ${\alpha}$-phellandrene, (4) (+)-3-carene, (5) ${\alpha}$-terpinene, (6) p-cymene, (7) (R)-(+)-limonene, (8) ${\gamma}$- terpinene, (9) myrcene, and (10) camphene). The results of BVOC calibration yielded comparatively stable pattern with response factor (RF) of 23,560~50,363 and coefficient of determination ($R^2$) of 0.9911~0.9973. The method detection limit (MDL) of BVOC was estimated at 0.03~0.06 ng with the reproducibility of 1.30~5.13% (in terms of relative standard error (RSE)). Emissions of BVOC were measured from four types of fruit samples ((1) tangerine (TO), (2) tangerine peel (TX), (3) strawberry (SO), and (4) sepals of strawberry (SX)). The sum of BVOC flux (${\sum}flux$ (BVOC) in ng/hr/g) for each sample was seen on the descending order of (1) TX=291,614, (2) TO=2,190, (3) SO=1,414, and (4) SX=2,093. If the results are compared between the individual components, the highest flux was seen from (R)-(+)-limonene (265,395 ng/hr/g) from TX sample.

하수슬러지와 토양 중 다핵방향족 탄화수소의 정량 (Analysis for 16 Polynuclear Aromatic Hydrocarbons (PAH) in Sewage Sludge and Soil)

  • 김종훈
    • 분석과학
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    • 제13권3호
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    • pp.357-367
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    • 2000
  • 하수슬러지와 토양시료 중 16가지의 다핵방향족 탄화수소(PAH)를 KOH와 $CHE_3OH$에 녹인 용액으로 Soxhlet 추출후 내부표준물질로 2-ethylantracene을 이용하여 GC/MS-SIM 방법으로 분석하였다. 12종의 PAH가 하수슬러지에서 검출되었고 공업지역 하수슬러지 중 가장 특징적인 화합물은 naphthalene($0.78{\mu}g/g$), 도시 하수슬러지에서는 pyrene($0.26{\mu}g/g$)이었으며, 총 PAH는 각각 $1.74{\mu}g/g$$1.19{\mu}g/g$이었다. 논 토양과 밭 토양에서의 PAH는 phenanthrene을 포함한 8종이 검출되었으며 그 농도범위는 $0.01-0.04{\mu}g/g$이었고, 총 PAH의 양은 각각 $0.19{\mu}g/g$$0.22{\mu}g/g$이었다. 논 토양 중의 총 PAH함량에 비하여 공업지역과 도시지역 하수슬러지 중의 총 PAH양은 각각 9.2배와 6.3배가 높게 나타났다.

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Essential Oil Analysis of Illicium anistum L. Extracts

  • Min, Hee-Jeong;Kim, Chan-Soo;Hyun, Hwa-Ja;Bae, Young-Soo
    • Journal of the Korean Wood Science and Technology
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    • 제45권6호
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    • pp.682-688
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    • 2017
  • Fresh japanese anise (Illicium anisatum L.) tree leaves were collected and ground after drying. The essential oils of the leaves were analyzed by gas chromatography-mass spectrometry (GC-MS) using headspace (HS) and solid phase-microextra (SPME) methods. Volatile components of the leaves were identified 21 and 65 components in HS and SPME, respectively. The main components of the essential oils obtained by HS method were eucalyptol (36.7%), (+)-sabinene (15.61%), ${\delta}$-3-carene (6.87%), ${\alpha}$-pinene (6.07%), ${\gamma}$-terpinen (5.72%), ${\alpha}$-limonene (5.26%), ${\beta}$-myrcene (4.13%), ${\alpha}$-terpinene (4.04%) and ${\beta}$-pinene (3.73%). The other components were less than 3.5%. SPME method also showed that eucalyptol (17.88%) was main. The other were 5-allyl-1-methoxy-2 (13.29%), caryophyllene (6.09%), (+)-sabinene (5.60%), ${\alpha}$-ocimene (4.89%) and ${\beta}$-myrcene (3.73%), and the rest were less amounts than 3.5%. This work indicated that many more volatile components were isolated, comparing to the previous literature data and that SPME method was much more effective than HS method in the analysis of the volatile components.