• 제목/요약/키워드: gas chromatography/mass spectrometry identification

검색결과 108건 처리시간 0.027초

주목 식물세포(Taxus chinensis) 배양 유래 타르 성분 동정 및 정량 (Identification and Quantification of Tar Compounds in Plant Cell Cultures of Taxus chinensis)

  • 김건중;박규연;김진현
    • 한국미생물·생명공학회지
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    • 제41권3호
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    • pp.272-277
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    • 2013
  • 본 연구에서는 gas chromatography/mass spectrometry (GC/MS)와 gas chromatography (GC)를 이용하여 주목 식물세포 Taxus chinensis 유래 타르 성분을 최초로 동정/정량하였다. 또한 식물세포배양으로부터 항암물질 paclitaxel 정제를 위한 전처리 과정에서 이들 타르 성분들의 제거 양상을 확인하였다. GC/MS 분석을 통하여 체류시간을 비교한 결과, 5종류의 타르성분이 체류시간 6.374, 8.208, 15.209, 20.045, 24.474분에서 각각 2-picoline, o-xylene, 2,5-xylenol, 1-methylnaphthalene, acenaphthene이 동정되었다. 또한 표준물질을 이용한 spike testing을 수행한 결과 동일 물질임을 재확인 하였다. GC 분석을 통하여 동정된 5종류 타르성분을 정량한 결과, 메탄올 추출물에 총 0.6805 wt% (2-picoline: 0.2512 wt%, 2,5-xylenol: 0.1586 wt%, acenaphthene: 0.1240 wt%, 1-methylnaphthalene: 0.0942 wt%, o-xylene: 0.0525 wt%) 타르 성분이 존재하였다. 액-액 추출을 수행한 결과, 메탄올 추출물 시료 내 총 타르 성분의 양 대비 42%의 타르 성분이 제거됨을 확인할 수 있었다. 1-Methylnaphthalene, acenaphthene, 2,5-xylenol, 2-picoline의 경우에는 각각 75.90, 59.92, 35.94, 29.74%로 높은 제거율을 보인 반면 oxylene의 경우에는 10.86%의 제거율로 상대적으로 적게 제거됨을 알 수 있었다. 흡착제 처리 후 2-picoline과 o-xylene의 양도 상당히 줄었지만 이들 2 종류의 타르 성분을 제외한 나머지 세 종류의 타르 성분(2,5-xylenol, 1-methylnaphthalene, acenaphthene)은 완전히 제거됨을 확인할 수 있었다. 흡착제 처리 공정에서 제거되지 않은 두 종류의 타르 성분(2-picoline, o-xylene)은 헥산 침전 공정에 의해 완전히 제거 가능하였다.

Rapid Determination of Ginkgolic Acids in Ginkgo biloba Leaf Using Online Column Switching High-Performance Liquid Chromatography-Diode Array Detection and Confirmation by Liquid Chromatography-tandem Mass Spectrometry

  • Lee, Hyounyoung;Lim, Heungyoul;Yang, Juhong;Hong, Jongki
    • Bulletin of the Korean Chemical Society
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    • 제34권12호
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    • pp.3629-3634
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    • 2013
  • In this study, an improved method for the quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba leaf extract was developed. The samples were extracted with a mixture of chloroform and 50 % ethanol, after which the chloroform extract was dried and reconstituted in methanol. GAs with 13:0, 15:1, and 17:1 in the extract were successfully separated within 40 min and determined with high throughput performance using an online column-switching HPLC method using an SP column C8 SG80 ($4.6{\times}150mm$, $5{\mu}m$) and a Cadenza 5CD C18 column ($4.6{\times}150mm$, $3{\mu}m$). The developed HPLC method was validated for Ginkgo biloba leaf extract. The validation parameters were specificity, linearity, precision, accuracy, and limits of detection and quantitation (LODs and LOQs, respectively). It was found that all of the calibration curves showed good linearity ($r^2$ > 0.9993) within the tested ranges. The LODs and LOQs were all lower than $0.04{\mu}g/mL$. The established method was found to be simple, rapid, and high throughput for the quantitative analysis of GAs in ten commercial Ginkgo biloba leaf extract and dietary supplements. The samples were also analyzed in LC-electrospray ionization (ESI) tandem mass spectrometry (MS/MS) - multiple-ion reaction monitoring (MRM) mode to confirm the identification results that were obtained by the column switching HPLC-DAD method. The developed method is considered to be suitable for the routine quality control and safety assurance of Ginkgo biloba leaf extract.

대기 중 PCBs와 유기염소계 살충제의 정량을 위한 분석 방법 개발 (Development of Analytical Method for Polychlorinated Biphenyls and Organochlorine Pesticides in Air)

  • 최민규;여현규;김태욱;천만영;선우영
    • 한국대기환경학회지
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    • 제18권6호
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    • pp.475-485
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    • 2002
  • An analytical method was investigated for the meaiiurement of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) concentrations in air samples. Procedures required for column chromatographic clean up. silicagel (stage I) and gel permeation chromatography (stage II), were discussed. Identification and quantification of PCBs and OCPs were performed using a combination of gas chromatography/mass spectrometry/ selected ion monitoring. Recovery tests calculated from six samples are 68∼137% for PCBs and 58∼130% for OCPs except for endrin aldehyde. Instrumental detection limits determined for the PCBs and OCPs varied from 0.05 to 0.18 pg/m3 and from 0.71 to 16.82 pg/㎥, respectively. The method has been applied to the analysis of air samples collected at Ansung city, Kyonggi province, Korea. This method may serve as a screening protocol for the simultaneous determination of PCBs and OCPs in air.

Analytical Methods of Levoglucosan, a Tracer for Cellulose in Biomass Burning, by Four Different Techniques

  • Bae, Min-Suk;Lee, Ji-Yi;Kim, Yong-Pyo;Oak, Min-Ho;Shin, Ju-Seon;Lee, Kwang-Yul;Lee, Hyun-Hee;Lee, Sun-Young;Kim, Young-Joon
    • Asian Journal of Atmospheric Environment
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    • 제6권1호
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    • pp.53-66
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    • 2012
  • A comparison of analytical approaches for Levoglucosan ($C_6H_{10}O_5$, commonly formed from the pyrolysis of carbohydrates such as cellulose) and used for a molecular marker in biomass burning is made between the four different analytical systems. 1) Spectrothermography technique as the evaluation of thermograms of carbon using Elemental Carbon & Organic Carbon Analyzer, 2) mass spectrometry technique using Gas Chromatography/mass spectrometer (GC/MS), 3) Aerosol Mass Spectrometer (AMS) for the identification of the particle size distribution and chemical composition, and 4) two dimensional Gas Chromatography with Time of Flight mass spectrometry (GC${\times}$GC-TOFMS) for defining the signature of Levoglucosan in terms of chemical analytical process. First, a Spectrothermography, which is defined as the graphical representation of the carbon, can be measured as a function of temperature during the thermal separation process and spectrothermographic analysis. GC/MS can detect mass fragment ions of Levoglucosan characterized by its base peak at m/z 60, 73 in mass fragment-grams by methylation and m/z 217, 204 by trimethylsilylderivatives (TMS-derivatives). AMS can be used to analyze the base peak at m/z 60.021, 73.029 in mass fragment-grams with a multiple-peak Gaussian curve fit algorithm. In the analysis of TMS derivatives by GC${\times}$GC-TOFMS, it can detect m/z 73 as the base ion for the identification of Levoglucosan. It can also observe m/z 217 and 204 with existence of m/z 333. Although the ratios of m/z 217 and m/z 204 to the base ion (m/z 73) in the mass spectrum of GC${\times}$GC-TOFMS lower than those of GC/MS, Levoglucosan can be separated and characterized from D (-) +Ribose in the mixture of sugar compounds. At last, the environmental significance of Levoglucosan will be discussed with respect to the health effect to offer important opportunities for clinical and potential epidemiological research for reducing incidence of cardiovascular and respiratory diseases.

숭늉향미성분(香味成分)에 관(關)한 연구(硏究) 2. 숭늉향기(香氣)성분중 pyrazine 및 carbonyl 화합물(化合物)에 관(關)하여 (Studies on Soong-Neung Flavor 2. Identification of Some Volatile Pyrazine and Carbonyl Compounds of Soong-Neung (extract of cooked and roasted rice))

  • 최홍식;남주형;김택제;권태완
    • 한국식품과학회지
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    • 제7권1호
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    • pp.15-21
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    • 1975
  • 숭늉향기성분(香氣成分)중 carbonyl 화합물(化合物)과 pyrazine 화합물(化合物)에 대하여 살펴 보았다. 숭늉을 질소개스를 유입(流入)하면서 감압(減壓)증류할 때, ice-water trap에 응축된 liquid phase(low volatile flavor)의 증류액을 dichloromethane으로 추출, 농축한 다음 이를 GC, GC-MS로 pyrazine 화합물(化合物)을 분리 동정하였다. 그 결과, 잠정적으로 9개의 pyrazine 화합물(化合物)을 확인하였고 그 가운데 2-methylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine, 2-ethyl-5-methylpyrazine, 2-ethyl-3-methylpyrazine 등 5개의 pyrazine 화합물(化合物)을 동정하였다. 이어 숭늉을 질소개스를 유입(流入), 감압(減壓)증류할 때 얻어진 고휘발성(高揮發性)성분중 carbonyl 화합물(化合物)을 2,4-DNPHs 유도체로 만든 후 이를 GC, GC-MS, TLC 등의 방법으로 carbonyl 화합물(化合物)을 분리(分離) 동정(同定)할 수 있었다. 이들에 대한 관능검사 결과, 특성 pyrazine 화합물(化合物) 특히 2,3-dimethylpyrazine 및 2,5-dimethylpyrazine의 냄새는 구수한 향기(香氣)를 지니고 있는 것으로 보아, pyrazine 화합물(化合物)은 숭늉향기를 이루는 주요한 성분으로 판단되었고 carbonyl 화합물(化合物) 역시 숭늉향기의 일부로서 큰 의의를 지니고 있는 것으로 사료(思料)되었다.

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The chloroform fraction of Citrus limon leaves inhibits human gastric cancer cell proliferation via induction of apoptosis

  • Osman, Ahmed;Moon, Jeong Yong;Hyun, Ho Bong;Kang, Hye Rim;Cho, Somi Kim
    • Journal of Applied Biological Chemistry
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    • 제59권3호
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    • pp.207-213
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    • 2016
  • Little information about the biological activities of Citrus limon (lemon) leaves has been reported, whereas the fruit of Citrus limon (lemon) has been well-documented to contain various pro-health bio-functional compounds. In the present study, the antiproliferative activities of the lemon leaves were evaluated using several cancer cell lines. From the n-hexane, chloroform, ethyl acetate, n-butanol, and water fractions of methanolic extract of the leaves, the chloroform fraction of lemon leaves (CFLL) showed the most potent antiproliferative activity in the AGS human gastric cancer cells. The current study demonstrates that CFLL induces apoptosis in AGS cells, as evidenced by an increase in apoptotic bodies, cell population in the sub-G1 phase, Bax/Bcl-2 ratio, and cleavage of poly (ADP-ribose) polymerase (PARP), caspase-3 and caspase-9. Compositional analysis of the CFLL using gas chromatography mass spectrometry (GC-MS) resulted in the identification of 27 compounds including trans, trans-farnesol (3.19 %), farnesol (3.26 %), vanillic acid (1.45 %), (-)-loliolide (5.24 %) and palmitic acid (6.96 %). Understanding the modes of action of these compounds individually and/or synergistically would provide useful information about their applications in cancer prevention and therapy.

GC/MS에 의한 오미자 Lignan성분의 동정 (Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry)

  • 손현주;복진영
    • Applied Biological Chemistry
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    • 제32권4호
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    • pp.344-349
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    • 1989
  • GC/MS를 이용하여 오미자의 chloroform-methanol 추출물로부터 11종의 lignan 성분을 동정하였다. GC column은 SPB-1 fused silica capillary $(0.25mm\;ID{\times}30m,\;Supelco)$를 사용하였고 column oven의 온도는 $200^{\circ}C$부터 $300^{\circ}C$까지 분당 $4^{\circ}C$씩 승온하였으며 MS의 ionization voltage는 70eV (El mode)이었다. 동정된 lignan 성분은 gomisin J, deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H, tigloylgomisin H, angeloylgomisin Q, gomisin B 및 benzoylgomisin H이었으며, GC chromatogram 상에서 이들 화합물의 분리상태는 양호하였다.

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Identification of urinary metabolite(s) of CKD-712 by gas chromatography/mass spectrometry in rats

  • Jeon, Hee-Kyung;Park, Hae-Yeon;Kim, Youn-Jung;Kwon, Oh-Seung;Ryu, Jae-Chun
    • 한국환경독성학회:학술대회논문집
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    • 한국환경독성학회 2003년도 춘계학술대회
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    • pp.188-188
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    • 2003
  • Examination was made of the urinary metabolite(s) of CKD-712, which is a chiral compound, named S-YS49 derived from higenamine (one component of Aconite spp.) derivatives. First of all, to analyze the metabolite(s) of CKD-712, a simple and sensitive detection method for CKD-712 was developed by using gas chromatography-mass spectrometry GC/MS). Urine was collected from adult male Sprague-Dawley rats 250${\pm}$10g) in metabolic cage for 24hr after oral administration of 100 mg/kg of CKD-712. The recovery of CKD-712 after extraction and concentration with AD-2 resin column was above 90 % from rat urine. The detection limits of CKD-712 in urine was approximately 0.1 ng/mL. It has well been suggested that isoquinoline possessing catechol moiety such as CKD-712 should be subjected to the catechol-O-methyl kransferase activity in vivo. We detected three major peaks of presumed CKD-712 metabolites in the total ion chromatogram obtained from the rat urine sample after oral administration of CKD-712. From these results, it is assumed that the urinary metabolites are mono-methylation in the naphthyl moiety (metabolite I ), methylation at the C-6 or 7 hydroxy group in the isoquinoline moiety and hydroxylation at in the naphthyl moiety (metaboliteII), and methylation at the C-6 or 7 hydroxy group in the isoquinoline moiety (metaboliteIII).

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Chemical properties and antioxidant activity of essential oils of Chrysanthemum morifolium Ramat. and Chrysanthemum indicum L. in Vietnam

  • Thi-Hoan Luong;Dang-Minh-Chanh Nguyen;Thi-Nga Trinh;Viet-Cuong Han;Woo-Jin Jung
    • Journal of Applied Biological Chemistry
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    • 제65권4호
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    • pp.367-374
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    • 2022
  • In recent years, research into medicinal herbs with antioxidative activities has increased. Chrysanthemum morifolium and Chrysanthemum indicum are aromatic herb plants and that have long been used in traditional Vietnamese medicine. This study aims to evaluate the chemical compositions and antioxidative activities of essential oils hydrodistilled from the flower heads of C. morifolium and C. indicum. The chemical compositions of the essential oils were compared using gas chromatography/mass spectrometry (GC/MS) analysis. The antioxidative activity was determined and evaluated spectroscopically by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging, metal chelating activity, reducing power, and total antioxidant capacity assays. According to the GC/MS results, chrysanthenone was predominant in the essential oils of both C. morifolium (64.14%) and C. indicum (32.02%). This is the first report of the identification of chrysanthenone as a major constituent of the essential oil of C. morifolium. Both Chrysanthemum oils were also revealed to possess antioxidant potential, exhibiting high antioxidative activities. In particular, the DPPH radical scavenging activities of the C. morifolium and C. indicum oils at a concentration of 100 mg/mL were 76.9 and 83.2%, respectively. The metal chelating values of C. morifolium and C. indicum were 0.85 and 0.76, whereas the reducing power values of that at 100 mg/mL were 0.76 and 0.71, respectively. This study provides the chemical properties of the essential oils of both C. morifolium and C. indicum grown in Vietnam and their potential antioxidant capacity.

쿠마린의 열분해에 관한 연구 (제1보) -질소기류, $500^{\circ}C$에서 쿠마린의 열분해산물 동정- (A Study on the Pyrolysis of Coumarin (I) Identification of Coumarin Pyrolyzates in a Stream of Nitrogen at $500^{\circ}C$)

  • 박준영;김옥찬
    • 한국연초학회지
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    • 제4권2호
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    • pp.63-66
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    • 1982
  • Coumarin was pyrolyzed at $500^{\circ}C$ in a stream of nitrogen. The pyrolyzates of coumarin were adsorbed on the activated charcoal and then eluded by carbon disulfide. The eluted pyrolyzates were identified using a gas chromatography/mass spectrometry. Benzene, toluene, phenylacetylene, styrene, benzofuran and naphthalene were detected from the pyrolyzates of coumarin on the basis of their mass spectra. The pyrolytic mechanism of coumarin was also discussed.

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