• Title/Summary/Keyword: GC and GC-MS method

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New Methods for Isolation of Sesquiterpene from Panax ginseng (인삼 Sesquiterpene의 새로운 분리방법)

  • 위재준;신지영
    • Journal of Ginseng Research
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    • v.21 no.3
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    • pp.214-218
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    • 1997
  • New simple methods for the Isolation of sesquiterpenes from Panax ginseng were developed. First, volatile compounds were isolated by simultaneous distillation and extraction (SDE) with 30% methanol and $\alpha$-hexane instead of water and ethyl ether/pentane (1:1). Secondly, head space volatiles in U-shaped tube at 7$0^{\circ}C$ were passed through C18 Sep-Pak by nitrogen gas streaming and the adsorbed volatiles were fluted by $\alpha$-hexane. TLC analysis showed that the volatile concentrates consisted mainly of terpenes when colored by vanillin-sulfuric and. GC/MS data revealed that approximately 30 sesquiterpenes of molecular weight 204 occupied 81.1% or more of the volatile concentrates isolated by those two newly developed methods. Among these, alloaromadendrene, germacrene B, isocaryophyllene, $\alpha$-neoclovene, ${\gamma}$-muurolene, $\beta$-panaslnsene, and $\alpha$-humulene were identified as being major sesqulterpenes by authentic samples or literatme search Key words : Panax ginseng, volatile compound, sesquiterpene, isolation, new method, GC/MS.

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Determination of ethylene glycol in alkali wastewater by gas chromatography/mass spectrometry (GC/MS를 이용한 알칼리 폐수 중 ethylene glycol 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.17 no.6
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    • pp.527-531
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    • 2004
  • Treatment with aqueous sodium hydroxide solution plays an important role to impart certain desirable properties - feel and luster on the surface of polyester fiber. In this process alkali wastewater contains disodium terephthalate, ethylene glycol (EG) and residual sodium hydroxide. In this paper we report a new method containing the pretreatments of derivatization with benzoyl chloride and solvent extraction using pentane. The calibration curve of EG determined by GC/MS-SIM shows a good linearity in the range of 0.1 to $25{\mu}g/mL$ having the standard deviation of ${\leq}8.7%$. The recovery and the detection limit of this method are 91.9-93.7% and $0.05{\mu}g/mL$ respectively.

Study on Metabolism and Excretion of Carteolol in Human Urine using GC/MS (GC/MS를 이용한 carteolol의 대사 및 배설연구)

  • Min, Hye-Ki;Kim, Myungsoo;Cho, Hyun-Woo;Kim, Taek-Jae;Kim, Dong-Hyun;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.15 no.5
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    • pp.482-487
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    • 2002
  • International Olympic Committee (IOC) prohibits the use of carteolol which is one of ${\beta}$-blockers. To prove whether carteolol product was taken or not, the analytical method in urine using GC/MS was established, and metabolism and excretion study were evaluated. As compared with acid hydrolysis, enzyme hydrolysis method was more efficiency. Coefficients of variation for intra-assay precision was around 10%. Error was less than 5% except the concentration of $0.05{\mu}g/m{\ell}$. Recovery was 78.5% at $2{\mu}g/m{\ell}$. Free carteolol, conjugated carteolol, and small amount of p-OH carteolol were found in dosed human urine samples. The conjugated form was being 59.4% of the total carteolol in human urine. The amount of carteolol renal excreted for 72 h after oral dose of 10 mg of carteolol was 49% of the administred dose.

Application of Adsorption Sampling and Thermal Desorption with GC/MS Analysis for the Measurement of Low-Molecular Weight PAHs in Ambient Air (환경대기 중 저분자 PAHs 측정을 위한 흡착-열탈착-GC/MS 방법의 적용)

  • Seo, Seok-Jun;Seo, Young-Kyo;Hwang, Yoon-Jung;Jung, Dong-Hee;Baek, Sung-Ok
    • Journal of Korean Society for Atmospheric Environment
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    • v.30 no.4
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    • pp.362-377
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    • 2014
  • Polycyclic aromatic hydrocarbons (PAHs) have been of particular concern since they are present both in the vapor and particulate phases in ambient air. In this study, a simple method was applied to determine the vapor phase PAHs, and the performance of the new method was evaluated with a conventional method. The simple method was based on adsorption sampling and thermal desorption with GC/MS analysis, which is generally applied to the determination of volatile organic compounds (VOCs) in the air. A combination of Carbotrap (300 mg) and Carbotrap-C (100 mg) sorbents was used as the adsorbent. Target compounds included two rings PAHs such as naphthalene, acenaphthylene, and acenaphthene. Among them, naphthalene was listed as one of the main HAPs together with a number of VOCs in petroleum refining industries in the USA. For comparison purposes, a method based on adsorption sampling and solvent extraction with GC/MS analysis was adopted, which is in principle same as the NIOSH 5515 method. The performance of the adsorption sampling and thermal desorption method was evaluated with respect to repeatabilities, detection limits, linearities, and storage stabilities for target compounds. The analytical repeatabilities of standard samples are all within 20%. Lower detection limits was estimated to be less than 0.1 ppbv. In the results from comparison studies between two methods for real air samples. Although the correlation coefficients were more than 0.9, a systematic difference between the two groups was revealed by the paired t-test (${\alpha}$=0.05). Concentrations of two-rings PAHs determined by adsorption and thermal desorption method consistently higher than those by solvent extraction method. The difference was caused by not only the poor sampling efficiencies of XAD-2 for target PAHs and but also sample losses during the solvent extraction and concentration procedure. This implies that the levels of lower molecular PAHs tend to be underestimated when determined by a conventional PAH method utilizing XAD-2 (and/or PUF) sampling and solvent extraction method. The adsorption sampling and thermal desorption with GC analysis is very simple, rapid, and reliable for lower-molecular weight PAHs. In addition, the method can be used for the measurement of VOCs in the air simultaneously. Therefore, we recommend that the determination of naphthalene, the most volatile PAH, will be better when it is measured by a VOC method instead of a conventional PAH method from a viewpoint of accuracy.

Quantitative determination of 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX) in chlorinated drinking water using sample enrichment followed by liquid-liquid extraction and GC-MS (시료 농축 후 액-액-추출과 GC-MS를 이용한 염소 소독 음용수중 3-chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone(MX)의정량 분석)

  • Kim, Hekap;Song, Byeong yeol
    • Analytical Science and Technology
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    • v.29 no.1
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    • pp.29-34
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    • 2016
  • This study explores the means by which MX can be effectively extracted from chlorinated water 3-Chloro-4-(dichloromethyl)-5-hydroxy-2(5H)-furanone (MX), a potent mutagen commonly found in chlorinated drinking water at concentrations of up to a few hundred ng/L, was quantitatively determined using sample enrichment followed by liquid-liquid extraction (LLE), derivatization to methylated form, and analysis with GC-MS. A 4-L water sample was enriched to a concentration of 0.4 L using a vacuum rotary evaporator at 30 ℃. MX in the water was extracted using ethyl acetate (100 mL × 2) as a solvent and MX in the extract was methylated with 10 % H2SO4 in methanol. MX was recovered at a rate of 73.8 %, which was higher than that (38.1 %) for the resin adsorption method. The limit of quantification and repeatability (as relative standard deviation) were estimated to be 10 ng/L and 2.2 %, respectively. This result suggested that LLE can be used for the determination of MX in chlorinated water as an alternative to more time-consuming resin adsorption method.

Determination of Volatile Organic Compounds in Waste using HS/GC/MS Analysis (Headspace/GC/MS를 이용한 폐기물중 휘발성 유기화합물의 분석)

  • Kim, Kyeo-Keun;Shin, Sun-Kyoung;Ju, Do-Weon
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.72-80
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    • 2000
  • The HS/GC/MS method was performed to analyze the volatile organic compounds in waste sludge samples. This study was performed to establish the fundamental data by studying the effects of salt, equilibrium temperature and time in the volatile organic compounds analysis. The presence of salts have been found to increase the sensitivity. The peak area is increased from 1.07 to 2.61 times by adding the salts to the water sample, compared with a salt tree sample. The recoveries of target compounds have found between 90% and 127% at sample temperature of $85^{\circ}C$ for 30 min. This HS/GC/MS method can be applied to analyze the volatile organic compounds and organohalo compounds in the environmental matrix.

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Methylation Methods on Identification of Phenolics in Chebulae Fructus (Chebulae Fructus중 페놀 물질 확인시의 Methylation법 비교)

  • 김정숙
    • Journal of the East Asian Society of Dietary Life
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    • v.4 no.1
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    • pp.79-86
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    • 1994
  • Food quality in food processing and storage were affected by the kinds of phenolics involved. To analyze phenolics of Chebulae Fructus by the way of GC-MSm methylation and trimethylsilyation(TMS) are necessary. The methods of methylation were dimethyl sulfate method and diazomethane method. so this study was undertaken to research the better methylation method before measuring GC-MS. But dimethyl sulfate method of methylation was not sufficient to analyze phenolics. So the phenolics of Chebulae Fructus were analyzed by the diazomethane methylation method and TMS with the pyridine, N-O-bis-trimethylsilyl-acetamide(BSTFA) and trimethylchlorosilane(TMCS). With the exception of pyrogallol and phloroglucinol in insoluble phenolics of Chebulae Fructus, the greater part of phenolics. analysis could be analyzed by GC-MS in company with diazomethane methylation method and TMS.

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Analysis of trace odorous compounds (geosmin and 2-methylisoborneol) in water by using GC/MS (물 중의 극미량 냄새 유발 물질인 Geosmin과 2-methylisoborneol의 GC/MS 분석법 연구)

  • Kim, Tae-Jon;Kim, Byung-Joo;So, Hun-Young;Kwang, Ho
    • Analytical Science and Technology
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    • v.15 no.6
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    • pp.534-539
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    • 2002
  • We established an analytical method for the measurement of trace amounts of earthy/musty odorous geosmin (GSM) and 2-methylisoborneol (2-MIB) in water using GC/MS. Water samples were extracted with n-hexane (liquid-liquid extraction, LLE) and the extracts were measured by GC/MS. The extraction yields of the two compounds were tested to be ($87{\pm}8$)% and ($78{\pm}8$)%, respectively. The limits of quantitation (LOQs) of the two compounds by this method were greatly improved to ~0.3 ng/L. The analytical methods were applied to analyze water samples from several rivers in Korea and waters after water treatment processes. The highest levels of geosmin and 2-methylisoborneol in raw water from a river were measured to be ($4.2{\pm}0.4$) ng/L and ($44{\pm}4$) ng/L, respectively. The levels only slightly decreased to ($1.3{\pm}0.1$) ng/L and ($18{\pm}2$) ng/L even after water treatment, indicating that the odorous compounds were not properly removed by the treatment processes.

Determination of chlorophenols from the industrial wastewater by GC/MS (GC/MS를 이용한 산업폐수중의 염화페놀류 분석)

  • Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.18 no.4
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    • pp.320-328
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    • 2005
  • The most common five chlorophenols (4-chloro-3-methylphenol, 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, pentachlorophenol) were determined from the industrial wastewater by GC/MS. The samples were collected from the petrochemical company, textile company and leather making company. The developed analytical method was modified by USEPA Method 3510. The samples were extracted with dichloromethane under pH 2 and pH 5-6, and determined by the GC/MS with SIM mode. There were good linearities (above $R^2=0.9943$) on e ranges of the 0.1 ng/mL~10 ng/mL and 0.5 ng/mL~10 ng/mL, and the limit of detection were between 0.1 ng/mL and 0.5 ng/mL. The absolute recoveries were measured at the concentration of 1, 5, and 10 ng/mL, and the recovery was 71.6~98.9% except for PCP. The relative standard deviation (RSD) was 1.2~14.3% and it gave a good reproducibility for the assay. The bias, which shows the accuracy, was a good although it was a little high values (11.3~22.1%) at the low concentration (1 ng/mL).

Dertermination of Alkylphenols, Chlorophenols and Bisphenol A in Various Samples by Freezing Filtration and GC/MS-SIM

  • Kim, Hyub
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.68.1-68.1
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    • 2003
  • A method for determination 11 endocrine disrupting chemicals of phenols in various samples was deloped. The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization method and tert-butyldimethylsilyl (TBDMS) derivatization method. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at -60$^{\circ}C$ for 2 hours (freezing filtration). (omitted)

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