• Title/Summary/Keyword: gas chromatography/mass spectrometry (GC/MS)

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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.

Preserving Reliability of Evidence Containers for Fire Debris Containing Ignitable Liquids (유류화재증거물 보관용기의 신뢰성에 관한 연구)

  • Han, Dong-Hun;Lee, Sung-Ryong
    • Fire Science and Engineering
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    • v.27 no.2
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    • pp.70-74
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    • 2013
  • It is very important for the collected samples at fire scenes to be properly preserved for laboratory analysis. Preserving abilities of four type containers, metal cans, glass jars, zipper and heat sealed polymer bags, with the five ignitable liquids (toluene, n-octane, o-xylene, n-decane and n-hexadecane) were examined with gas chromatography-mass spectrometry. The glass jars with Teflon (PTFE) liner were the best ability to prevent the evaporation of the ignitable liquids.

Seasonal Variation in Concentration and Composition of Monoterpenes from Artemisia princeps var. orientalis (쑥에 함유된 monoterpenes 의 함량과 조성의 계절적 변이)

  • Kim, Jong-Hee
    • The Korean Journal of Ecology
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    • v.19 no.4
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    • pp.321-328
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    • 1996
  • The profile and concentration of monoterpene metabolites in the leaf and stem of Artemisia princeps var. orientalis were quantified, and seasonal variation in monoterpenes of Artemisia plant was investigated. Samples were taken from five sites at the campus of Kyungnam University during maturing season. Monoterpenes in leaf and stem were analyzed using gas chromatography-mass spectrometry (GC-MS). The major constituents of A. princeps var. orientalis in both the leaf and stem were 21 monoterpenes.$ {\alpha}-pinene,\;{\beta}-pinene,\;{\beta}-myrcene$, dl-limonene, naphthalene and unknown monoterpenes with 5.49 and 16.27 of retenstion time were present in high concentrations of compounds identified on the leaf and stem of A. princeps var. orientalis. The cmounts of total monoterpenes of leaf were from two to five times higher than stem and rapidly decreased with the time, while that of stem was constnat except early spring. Most of the high percentage of monoterpenes in the leaf were those with later retention time. These results indicated that monoterpenes yields are considered to be more variable than monoterpene composition in responding to the time in both the leaf and stem.

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Determination of Phthalates in Biota Samples Using Gas Chromatography/Mass Spectrometry (기체크로마토그래피/질량분석법을 이용한 생체시료 중 프탈산 에스텔류의 분석법)

  • Seo, Jung-Ju;Na, Yuncheol;Hong, Jongki
    • Analytical Science and Technology
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    • v.14 no.5
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    • pp.400-409
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    • 2001
  • A method for the analysis of most common phthalate acid esters (9 secies) in biota samples by gas chromatography-mass spectrometry-selected ion monitoring mode is described. Phthalates in biota samples are extracted by organic solvent and purified by Florisil column. Phthalates are easily contaminated during extraction prodedure. Since the extraction and cleanup steps for biota samples generally are more complicate than those for water or sediment samples, we compared with contamination state of each sample work-up step. By applying this developed method, the overall recoveries ranged between 79 - 117% in biota sample which was spiked with standards. For phthalates used in this study, the quantitaive accuracy, elution pattern on Florisil column, and detection limits were also investigated.

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SENSITIVE DETERMINATION OF ELEVEN PHENOLIC ENDOCRINE-DISRUPTING CHEMICALS IN HUMAN URINE USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY -SELECTED ION MONITORING

  • Kim, Hyub;Jang, Cheol-Hyeon
    • Environmental Engineering Research
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    • v.12 no.3
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    • pp.93-100
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    • 2007
  • I improved an analytical method for determining trace amounts of eleven phenolic endocrine-disrupting chemicals (11 phenolic EOCs) in human urine. The 11 phenolic EOCs were subjected to hydrolysis and then to solid phase extraction with a XAD-4 column. Alkylphenols, chlorophenols, and bisphenol A in XAD-4 column were eluted with acetonitrile, and the eluate was concentrated under a nitrogen stream, and then tert-butyldimethylsilylation. Separation and determination were done by gas chromatography, using mass spectrometry operating in the selective ion monitoring mode for quantitation. For tert-butyldimethylsily (TBDMS) derivatization the recoveries were $91.2{\sim}125.9%$, the limits of quantitation (LOQ) for the 11 phenolic EOCs in the nanogram-per-milliliter range ($0.025{\sim}1.000\;ng/mL$) were thus achieved by using 1 mL of urine, and the SIM responses were linear with the correlation coefficient varying by $0.9300{\sim}0.9943$. Based on the results for urine samples from unexposed individuals, 4-tert-octylphenol and pentachlorophenol were detected in hydrolysed urine sample. Other alkylphenols, chlorophenols and bisphenol A were not detected.

Phytochemical and Biological Investigation of Spergularia marina (L.) Griseb. Growing in Egypt

  • El-Dien, Omnia Gamal;Shawky, Eman;Aly, Amal H.;Abdallah, Rokia M.;Abdel-Salam, Nabil A.
    • Natural Product Sciences
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    • v.20 no.3
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    • pp.152-159
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    • 2014
  • A phytochemical investigation of Spergularia marina (L.) Griseb. growing in Egypt, has been carried out, which resulted in the isolation of seven compounds from the different extracts of the plant namely; ${\beta}$-sitosterol glucoside, tricin (1) dihydroferulic acid (2), vanillic acid (3), 4-hydroxybenzoic acid (4), uracil (5) and 8-hydroxy cuminoic acid (6) Structure elucidation of the isolated compounds was carried out using different spectroscopic techniques. This is the first report for the isolation of these compounds from genus Spergularia. Furthermore, 8-Hydroxy cuminoic acid and uracil were isolated for the first time from family Caryophyllaceae. The chemical composition of the volatile components present in the petroleum ether extract of Spergularia marina (L.) Griseb. using combined gas chromatography-mass spectrometry (GC-MS) is reported here for the first time. Of the 97 components present, 59 were identified including three sulfur containing compounds which represented about 1.8% of the volatiles of the total petroleum ether extract. This prompted us to study and report its possible antimicrobial activity. In addition, the antibacterial and antifungal screening of different extracts of Spergularia marina (L.) Griseb. as well as some isolates have been performed using agar diffusion method.

Rapid Determination of Chlorostyrenes in Fish by Freezing-Lipid Filtration, Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

  • Kim, Min-Sun;Park, Kwang-Sik;Pyo, Hee-Soo;Hong, Jong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.29 no.2
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    • pp.352-356
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    • 2008
  • An analytical method has been developed for measuring chlorostyrenes in fish tissue sample. Extraction of chlorostyrenes from fish tissue was carried out by ultrasonication using acetone/n-hexane (5:2, v/v) mixture. Most of the lipids in the extract were eliminated by freezing-lipid filtration, prior to solid-phase extraction (SPE) cleanup. During freezing-lipid filtration, about 90% of the lipids extracted from the fish samples were easily removed without any significant losses of chlorostyrenes. For purification, SPE using Florisil was used for the rapid and effective cleanup. Quantification was performed using gas chromatography-mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery was above 80% in the spiked fish tissue sample at 10 and 100 ng/g levels, respectively. The detection limits for chlorostyrenes were ranged from 0.05 to 0.1 ng/g. This developed method is demonstrated to give efficient recoveries and LODs for detecting chlorostyrenes spiked into fish tissue with high lipid content.

Determination of benzo(a)pyrene in Soil, Sediment and Water by Gas Chromatography- Mass Spectrometry (기체크로마토그래피/질량분석기에 의한 토양, 저질 및 수질시료 중 benzo(a)pyrene의 분석)

  • Jeon Ree Kyung;Choi Rae Yeon;Ryu Jae-Chun
    • Environmental Analysis Health and Toxicology
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    • v.20 no.1
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    • pp.47-55
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    • 2005
  • 본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 benzo(a)pyrene(BaP)을 분석하는 방법을 확립하고자 하였다. BaP은 수질 시료(100mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료(l0g) 에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 BaP 회수율은 94.8% 이상이었으며 토양에서의 회수율은 약 93%를 보였고 재현성은 10.49% 이하였다. 검정 곡선은 상관계수(R²)값이 수질과 토양 모두에서 0.996 이상의 좋은 직선성을 보여주었다. 토양 시료의 경우 35지역 중 6지역의 토양에서 0.5~223.5㎍/kg의 농도 범위로 BaP가 검출되었으며 수질과 저질 시료에서는 모든 지역에서 검출한계 이하로 나타났다. 이 분석방법은 환경 중에 미량으로 존재하는 BaP의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

Discovery of Urinary Biomarkers in Patients with Breast Cancer Based on Metabolomics

  • Lee, Jeongae;Woo, Han Min;Kong, Gu;Nam, Seok Jin;Chung, Bong Chul
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.59-66
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    • 2013
  • A metabolomics study was conducted to identify urinary biomarkers for breast cancer, using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS), analyzed by principal components analysis (PCA) as well as a partial least squares-discriminant analysis (PLS-DA) for a metabolic pattern analysis. To find potential biomarkers, urine samples were collected from before- and after-mastectomy of breast cancer patients and healthy controls. Androgens, corticoids, estrogens, nucleosides, and polyols were quantitatively measured and urinary metabolic profiles were constructed through PCA and PLS-DA. The possible biomarkers were discriminated from quantified targeted metabolites with a metabolic pattern analysis and subsequent screening. We identified two biomarkers for breast cancer in urine, ${\beta}$-cortol and 5-methyl-2-deoxycytidine, which were categorized at significant levels in a student t-test (p-value < 0.05). The concentrations of these metabolites in breast cancer patients significantly increased relative to those of controls and patients after mastectomy. Biomarkers identified in this study were highly related to metabolites causing oxidative DNA damage in the endogenous metabolism. These biomarkers are not only useful for diagnostics and patient stratification but can be mapped on a biochemical chart to identify the corresponding enzyme for target identification via metabolomics.

Determination of Mequitazine in Human Plasma by Gas-Chro-matography/Mass Spectrometry with Ion-Trap Detector and Its Pharmacokinetics after Oral Administration to Volunteers

  • Kwon Oh-Seung;Kim Hye-Jung;Pyo Heesoo;Chung Suk-Jae;Chung Youn Bok
    • Archives of Pharmacal Research
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    • v.28 no.10
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    • pp.1190-1195
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    • 2005
  • The objective of this study was to develop an assay for mequitazine (MQZ) for the study of the bioavailability of the drug in human subjects. Using one mL of human plasma, the pH of the sample was adjusted and MQZ in the aqueous phase extracted with hexane; the organic layer was then evaporated to dryness, reconstituted and an aliquot introduced to a gas chromatograph/mass spectrometer (GC/MS) system with ion-trap detector. Inter- and intra-day precision of the assay were less than 15.1 and $17.7{\%}$, respectively; Inter- and intra-day accuracy were less than 8.91 and $18.6{\%}$, respectively. The limit of quantification for the current assay was set at 1 ng/mL. To determine whether the current assay is applicable in a pharmacokinetic study for MQZ in human, oral formulation containing 10 mg MQZ was administered to healthy male subjects and blood samples collected. The current assay was able to quantify MQZ levels in most of the samples. The maximum concentration ($C_{max}$ was 8.5 ng/mL, which was obtained at 10.1 h, with mean half-life of approximately 45.5 h. Under the current sampling protocol, the ratio of $AUC_{t{\rightarrow}last}$ to $AUC_{t{\rightarrow}{\infty}}$ was $934{\%}$, indicating that the blood collection time of 216 h is reasonable for MQZ. Therefore, these observations indicate that an assay for MQZ in human plasma is developed by using GC/MS with ion-trap detector and validated for the study of pharmacokinetics of single oral dose of 10 mg MQZ, and that the current study design for the bioavailability study is adequate for the drug.