• Title/Summary/Keyword: gas chromatography/mass spectrometry identification

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

  • Kim, Gun-Joong;Park, Gyu-Yeon;Kim, Jin-Hyun
    • Microbiology and Biotechnology Letters
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    • v.41 no.3
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    • pp.272-277
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    • 2013
  • In this study, the tar compounds derived from the plant cell cultures of Taxus chinensis were first identified and then quantified via gas chromatography/mass spectrometry (GC/MS) and gas chromatography (GC). 2-Picoline, 2,5-xylenol, acenaphthene, 1-methylnaphthalene and o-xylene were found to be the major tar compounds by biomass. These compounds were identified and confirmed by comparing their retention times with those of authentic compounds. Each compound also spiked with the pure standard. The contents of 2-picoline, 2,5-xylenol, acenaphthene, 1-methylnaphthalene, and o-xylene in biomass were 0.2512, 0.1586, 0.1240, 0.0942 and 0.0525 wt%, respectively. Liquid-liquid extraction and adsorbent treatment were able to remove 42% and 94% of the tars from biomass, respectivly. After hexane precipitation, all of the tars were perfectly removed.

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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    • v.34 no.12
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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.

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

  • 최민규;여현규;김태욱;천만영;선우영
    • Journal of Korean Society for Atmospheric Environment
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    • v.18 no.6
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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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    • v.6 no.1
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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.

Studies on Soong-Neung Flavor 2. Identification of Some Volatile Pyrazine and Carbonyl Compounds of Soong-Neung (extract of cooked and roasted rice) (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)

  • Cheigh, Hong-Sik;Nam, Joo-Hyung;Kim, Taeck-Jae;Kwon, Tai-Wan
    • Korean Journal of Food Science and Technology
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    • v.7 no.1
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    • pp.15-21
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    • 1975
  • Soong-Neung is a Korean traditional beverage served after meals and is made from cooked and roasted rice produced on the bottom of the container during the rice cooking process. The volatiles from the extract of cooked and roasted rice were separated into pyrazine and carbonyl fractions and qualitatively investigated. The pyrazine fraction was characterized by gas chromatography and combined gas chromatography-mass spectrometry and five pyrazines were positively identified. Pyrazine compounds identified are 2-methylpyrazine, 2,3-dimethylpyrazine, 2,5-dimethylpyrazine, 2-ethyl-5-methylpyrazine and 2-ethyl-3-methylpyrazine. Carbonyls were converted to their 2,4-dinitrophenylhydrazones and identified by gas chromatography, combined gas chromatography-mass spectrometry and thin layer chromatography. Acetaldehyde, propionaldehyde, iso-butyraldehyde and iso-valeraldehyde were positively identified in the carbonyl compounds. The aroma of the fractions indentified as 2,3-dimethylpyrazine and 2,5-dimethylpyrazine had a nut-like or roasted cereal-like flavor, which is one of the characteristic flavors of Soong-Neung.

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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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    • v.59 no.3
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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.

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

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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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
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.05a
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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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    • v.65 no.4
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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.

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

  • Park, Jun-Young;Kim, Ok-Chan
    • Journal of the Korean Society of Tobacco Science
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    • v.4 no.2
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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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