• Title/Summary/Keyword: Gas chromatography-mass spectrometer

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The study on the measurement of formaldehyde in saliva and urine by GC-MS (가스크로마토그래프-질량분석기에 의한 타액 및 뇨 중 포름알데하이드 분석법 연구)

  • Shin, Ho-Sang;Ahn, Hye-Sil
    • Analytical Science and Technology
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    • v.19 no.2
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    • pp.149-154
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    • 2006
  • A gas chromatography-mass spectrometric method was developed for the determination of formaldehyde in urine and saliva. In a 20 mL glass tube, 0.2 mL of urine or saliva was taken. Further, 1.8 mL of 0.1 M HCl, 0.1 mL of 2,000 mg/L 2,4-dinitrophenyl hydrazine and $20{\mu}l$ of 500 mg/L acetone-$d_6$ as internal standard were added in the tube and sealed tightly with cap. The solution was shaken for 20 min at room temperature and extracted using 4 mL of toluene. The extract was concentrated and redissolved with $100{\mu}l$ of acetonitrile, and then measured by gas chromatography-mass spectrometer (selected ion monitoring). The detection limit was 2.0 ng/mL and 0.5 ng/mL in saliva and urine, respectively. The calibration curves showed good linearity with r = 0.997 and 0.998 for saliva and urine, respectively. The method was used to analyze formaldehyde in rat urine after oral exposure. The developed method may be use ful to the monitoring for formaldehyde exposure in human.

Studies on the Volatile Components of Platycodon grandiflorus (jacquin) A.De Candolle (도라지의 휘발성분에 관한 연구)

  • Sun, Woo-Sun;Kwon, Jae-Sang;Shin, Pyung-Gyun;Cho, Sung-Hwan;Chung, Jin-Hwan
    • Applied Biological Chemistry
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    • v.39 no.6
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    • pp.517-520
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    • 1996
  • To identify the volatiles of Platycodon roots, the three-year-old and the 24-year-old Platycodon roots cultivated in a local farm were extracted with ethyl ether by SDE method. 54.71mg% and 80.01mg% of volatile components were collected in the three-year-old and in 24-year-old Platycodon roots, respectively. As a result of GC/MS(TIC) analysis, 24 and 28 compounds were identified, respectively; The amounts of volatile components such as hexanol, trans-2-hexenol and nonanal in 24-year-old roots were detected above ten times than those in 3-year-old roots. The Volatiles of 24-year-old roots were fractionated by SCC and identified by GC/MS to be 10 hydrocarbons, 8 alcohols, 10 aldehydes, 5 esters, 6 acids and 1 unknown compound as the major components. The species and total amounts of volatile component in 24-year-old Platycodon roots were considered to be higher than those in 3-year-old Platycodon roots. *Abbreviations 1. Platycodon : platycodon grandiflorus (jacquin) A. De Candolle. 2. SDE : Simultaneous Distillation Extraction 3. SCC : Silicagel Column Chromatography 4. GC : gas chromatography 5. GC/MS : Gas Chromatography-Mass Spectrometer 6. TIC : Total Ion Chromatogoraphy

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Acaricidal effects of herb essential oils against Dermatophagoides farinae and D. pteronyssinus (Acari: Pyroglyphidae) and qualitative analysis of a herb Mentha pulegium (pennyroyal)

  • Rim, In-Sook;Jee, Cha-Ha
    • Parasites, Hosts and Diseases
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    • v.44 no.2 s.138
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    • pp.133-138
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    • 2006
  • This experiment was undertaken to screen the acaricidal effects of herb essential oils (pennyroyal, ylang ylang, citronella, lemon grass, tea tree, and rosemary) at different doses (0.1, 0.05, 0.025, 0.0125, and $0.00625{\mu}l/cm2$) and exposure times (5, 10, 20, 20, 30 and 60 min) on house dust mites Dermatophgoides farinae and D. pteronyssinus. The most effective acaricidal components of pennyroyal (Mentha pulegium) were analyzed using a gas chromatography-mass spectrometer (GC-MS). Of these essential oils, the most effective was pennyroyal, which is composed essentially of pulegone (> 99%), at a dose of $0.025{\mu}l/cm^2$, which at an exposure time of 5 min killed more than 98% of house dust mites. In the pennyroyal fumigation test, the closed method was more effective than the open method and maximum acaricidal effect was 100% at $0.025{\mu}l/cm^2$, 60 min. The results show that herb essential oils, in particular, pennyroyal was proved to have potent acaricidal activity.

Discrimination of Ginseng Habitat by Using Instrumental Analysis Techniques

  • Sohn H. J.;Lee S. K.;Cho B. G.;Kim S. J.;Lee N. Y.;Choi D. S.;Jeong M. S.;Bae H. R.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.238-252
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    • 2002
  • In order to screen out indicators for the discrimination of ginseng habitat, some physical and chemical characteristics of Korean red ginsengs (94 kinds) and Chinese red ginsengs (50 kinds) were analyzed by using a rheometer, an electronic nose system, a combined technique of solid phase micro-extraction (SPME) and gas chromatograph equipped with an electron capture detector (GC/ECD), an X-ray fluorescence spectrometer (XRF), an inductively coupled plasma mass spectrometer (ICP/MS), a near infrared spectrometer (NIRs) and high performance liquid chromatography equipped with evaporative light scattering detector (HPLC/ELSD). The results are summarized as follows: (i) The rhizome strengths of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. (ii) The electronic nose patterns of Korean red ginsengs were significantly different from those of Chinese red ginsengs. (iii) Some unidentified peaks were detected not in the headspace of Korean red ginsengs but in the headspace of Chinese red ginsengs when the headspace volatiles prepared by the SPME technique were analyzed by GC/ECD. (iv) Either the content ratios of K to Ca or Mn to Fe were significantly different between Korean red ginsengs and Chinese red ginsengs. (v) The reflectance ratios of NIRs wavenumbers such as $904\;cm^{-1}\;to\;1088\;cm^{-1}$ for Korean red ginsengs were significantly different from those for Chinese red ginsengs. (vi) The content ratios of ginsenoside-Rg to ginsenoside-Re of Korean red ginsengs were significantly higher than those of Chinese red ginsengs. These results indicate that the rhizome strength, the electronic nose pattern, the occurrence of ECD-sensitive headspace volatile components, the content ratios of K to Ca and Mn to Fe, the NIRs pattern and the content ratio of ginsenoside-Rg to -Re may be indicators for the discrimination of ginseng habitat.

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A survey on pesticide residues of imported fruits circulated in Gyeonggido (경기도내 유통 수입과실류의 잔류농약 실태조사)

  • Cho, Yun-Sik;Kang, Jeong-Bok;Kim, Yang-Hee;Jeong, Jin-A;Huh, Jeong-Weon;Lee, So-Hyun;Lim, Young-Sik;Bae, Ho-Jeong;Kang, Heung-Gyu;Lee, Jeong-Hee;Jung, Eun-Sook;Lee, Byoung-Hoon;Park, Yong-Bok;Lee, Jong-Bok
    • The Korean Journal of Pesticide Science
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    • v.16 no.3
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    • pp.195-201
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    • 2012
  • We tested for pesticide residues in 124 samples of 22 different items of imported fruits circulated in Gyeonggido. Total 218 pesticides were analyzed by multi-residue method using gas chromatography/nitrogen phosphorus detector-electron capture detector (GC/NPD-ECD), time of flight/mass spectrometer (TOF/MS), ultra performance liquid chromatography/photo diode array (UPLC/PDA), high performance liquid chromatography/fluorescence detector (HPLC/FLD) and mass spectrometer (LC/MS/MS). The pesticides were detected in 18 fruits samples, ranging 0.003~0.3 mg/kg and no samples had violative residue. The separation test to 14 sample pesticides detected was conducted to monitor the current status of pesticide residues according to the partial characteristic. The pesticides were detected in 14 peels ranging 0.03~1.5 mg/kg and 2 fleshes in less than detection limits. These results indicate that imported fruits are safe when the human takes normally but even the small amount of pesticides is harmful when the human takes it in a prolonged period. Therefore, the pesticide residual amounts of imported friuts should be constantly monitored for food safety.

Determination of Siderophore from Bacillus Mojavensis Using Liquid Chromatography quadrupole Time-of-flight Tandem Mass Spectrometry (액체크로마토그래피-사중극 비행시간형 탠덤질량분석기를 이용한 Bacillus mojavensis 균주 속 사이드로포어 규명)

  • Cheon, Hae In;Yeo, Mi Seon;Kim, Kang Min;Kang, Jae Seon;Pyo, Jaesung
    • Journal of Life Science
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    • v.29 no.2
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    • pp.198-201
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    • 2019
  • Recently, it has been reported that Bacillus mojavensis possesses antifungal properties and plant growth-promoting activities, which are similar to the characteristics of siderophore. In this study, the siderophore produced by B. mojavensis was assessed using a solid phase extraction (SPE) cartridge and liquid chromatography quadrupole time-of-flight tandem mass spectrometry (Q-TOF MS/MS). After B. mojavensis was incubated in phenol medium for 16 hr and lyophilized, the sample was dissolved in water and loaded to an SPE cartridge to remove interferences. The cartridge was washed with 5% methanol in water and eluted with 2% formic acid in methanol sequentially. The eluted solution was evaporated under a stream of nitrogen gas and reconstituted in methanol. The reconstituted sample was filtered, and $1{\mu}l$ of the sample was assessed using Q-TOF MS/MS. The mass spectrometer was operated using the positive electrospray ionization mode. Based on the mass spectrum and tandem mass spectrum, the siderophore produced by B. mojavensis was bacillibactin, one of the catechol types of siderophore with a molecular weight of 882.2556. This siderophore analysis could provide a justification for the study of B. mojavensis as a functional food and for pharmaceutical applications.

The Characteristics of the Appearance and Health Risks of Volatile Organic Compounds in Industrial (Pohang, Ulsan) and Non-Industrial (Gyeongju) Areas

  • Jung, Jong-Hyeon;Choi, Bong-Wook;Kim, Mi-Hyun;Baek, Sung-Ok;Lee, Gang-Woo;Shon, Byung-Hyun
    • Environmental Analysis Health and Toxicology
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    • v.27
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    • pp.12.1-12.8
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    • 2012
  • Objectives: The aim of this study was to identify the health and environmental risk factors of air contaminants that influence environmental and respiratory diseases in Gyeongju, Pohang and Ulsan in South Korea, with a focus on volatile organic compounds (VOCs). Methods: Samples were collected by instantaneous negative pressure by opening the injection valve in the canister at a fixed height of 1 to 1.5 m. The sample that was condensed in $-150^{\circ}C$ was heated to $180^{\circ}C$ in sample pre-concentration trap using a 6-port switching valve and it was injected to a gas chromatography column. The injection quantity of samples was precisely controlled using an electronic flow controller equipped in the gas chromatography-mass spectrometer. Results: The quantity of the VOC emissions in the industrial area was 1.5 to 2 times higher than that in the non-industrial area. With regards to the aromatic hydrocarbons, toluene was detected at the highest level of 22.01 ppb in Ulsan, and chloroform was the halogenated hydrocarbons with the highest level of 10.19 ppb in Pohang. The emission of toluene was shown to be very important, as it accounted for more than 30% of the total aromatic hydrocarbon concentration. Conclusions: It was considered that benzene in terms of the cancer-causing grade standard, toluene in terms of the emission quantity, and chloroform and styrene in terms of their grades and emission quantities should be selected for priority measurement substances.

The separation of arsenic metabolites in urine by high performance liquid chromatography-inductively coupled plasma-mass spectrometry

  • Chung, Jin-Yong;Lim, Hyoun-Ju;Kim, Young-Jin;Song, Ki-Hoon;Kim, Byoung-Gwon;Hong, Young-Seoub
    • Environmental Analysis Health and Toxicology
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    • v.29
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    • pp.18.1-18.9
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    • 2014
  • Objectives The purpose of this study was to determine a separation method for each arsenic metabolite in urine by using a high performance liquid chromatography (HPLC)-inductively coupled plasma-mass spectrometer (ICP-MS). Methods Separation of the arsenic metabolites was conducted in urine by using a polymeric anion-exchange (Hamilton PRP X-100, $4.6mm{\times}150mm$, $5{\mu}m$) column on Agilent Technologies 1260 Infinity LC system coupled to Agilent Technologies 7700 series ICP/MS equipment using argon as the plasma gas. Results All five important arsenic metabolites in urine were separated within 16 minutes in the order of arsenobetaine, arsenite, dimethylarsinate, monomethylarsonate and arsenate with detection limits ranging from 0.15 to $0.27{\mu}g/L$ ($40{\mu}L$ injection). We used G-EQUAS No. 52, the German external quality assessment scheme and standard reference material 2669, National Institute of Standard and Technology, to validate our analyses. Conclusions The method for separation of arsenic metabolites in urine was established by using HPLC-ICP-MS. This method contributes to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies for arsenic exposure in South Korea.

Installation and Test Run of Comprehensive Analysis System for SF6 in Power Equipment

  • Lee, Jeong Eun;Kim, Kwang Sin;Kim, Ah Reum;Park, Seoksoon;Kim, Kyeongsook
    • KEPCO Journal on Electric Power and Energy
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    • v.3 no.1
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    • pp.41-47
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    • 2017
  • After $SF_6$, which is being used in power equipment as an insulating material, is classified as one of the 6 major greenhouse gases, the maintenance and the refinement of used $SF_6$ started to get attention. In regard to this, KEPCO Research Institute (KEPRI) is developing $SF_6$ recovery and refinement technology starting with establishing a comprehensive $SF_6$ analysis system. With the analysis system, qualitative and quantitative analyses of the purity and the impurities of $SF_6$ before and after recovery, and before and after refinement have been carried out. The analysis system is comprised of GC-DID (Gas Chromatograph -Discharge Ionization Detector) for trace impurities analysis, GC-TCD (Thermal Conductivity Detector) for analyses of $SF_6$ purity and major impurities concentration from several hundred ppm up to percent range, GC-MSD (Mass Selective Detector) for analyses of impurities not included in standard gas, FT-IR (Fourier Transform-Infrared) Spectrometer for analysis of HF and $SO_2$, and moisture analyzer for analysis of moisture below 100 ppm. With this analysis system, complete analysis method of $SF_6$ has been established. This analysis system is being used in the maintenance of power equipment and the development of $SF_6$ recovery and refinement technologies. In this paper, the analysis results of four samples - gas and liquid phase $SF_6$ samples from a $SF_6$ refinement system before and after refinement are presented.

Isolation and Identification of Lipids from the Fruits of Acanthopanax sessiliflorus (오가피(Acanthopanax sessiliflorus Seeman) 열매로부터 지질 화합물의 분리 및 동정)

  • Kim, Su-Yeon;Lee, Dae-Young;Seo, Kyeong-Hwa;Rho, Young-Deok;Kim, Gye-Won;Cheoi, Dae-Sung;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.55 no.2
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    • pp.103-107
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    • 2012
  • Acanthopanax sessiliflorus Seeman fruits (Araliaceae) were extracted at room temperature with 70% aqueous ethanol (EtOH). The concentrated extract was partitioned with ethyl acetate (EtOAc), n-butyl alcohol, and $H_2O$, successively. From the EtOAc fraction, four compounds were isolated through the repeated silica gel and octadecyl silica gel (ODS) column chromatographies. According to the results of physico-chemical and spectroscopic data including NMR, IR, and gas chromatography/mass spectrometer, the chemical structures of the compounds were determined as stigmasterol (1), linoleic acid (2), ${\beta}$-sitosterol (3), and stigmast-5-en-$3{\beta}$,$7{\beta}$-diol (4).