• Title/Summary/Keyword: Gas chromatography/mass spectrometry (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.

A study on the derivatization technique for tamoxifen metabolites in human urine by gas chromatography/mass spectrometry (기체크로마토그래피/질량분석기를 이용한 인체 내 뇨시료에서의 Tamoxifen 대사체 검출을 위한 유도체화 연구)

  • Kim, Yunje;Lee, Yoonjung
    • Analytical Science and Technology
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    • v.17 no.4
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    • pp.322-336
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    • 2004
  • The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride (TFAA), pentafluoroacetic anhydride (PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry (GC/MS) technique use negative ion chemical ionization (NCI), positive ion chemical ionization (PCI) and electron impact (EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at $50^{\circ}C$ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

Analysis of Volatile Flavor Components of Pleurospermum kamtschaticum (누룩치의 휘발성 향미성분 분석)

  • 정미숙;이미순
    • Korean journal of food and cookery science
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    • v.14 no.5
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    • pp.541-546
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    • 1998
  • Volatile flavor components in leaf and petiole of fresh Pleurospermum kamtschaticum H$\_$OFFM/ were extracted by SDE (simultaneous steam distillation and extraction) method using diethyl ether as solvent. Essential oils were analyzed by gas chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Identification of volatile flavor components was based on the Rl of GC and mass spectrum of GC-MS. A total of 31 components, including 15 hydrocarbons, 4 aldehydes, 1 ketone, 5 alcohols, 2 esters, 3 acids and 1 oxide were identified in the essential oils. (Z)-${\beta}$-Farnesene, (Z, E)-${\alpha}$-farnesene and farnesene were the major volatile flavor components in fresh Pleurospermum kamtschaticum. Volatile flavor patterns of Pleurospermum kamtschaticum were analyzed using electronic nose. Sensor T30/1 and PA2 that were sensitive to alcohols had the highest resistance for fresh Pleurospermum kamtschaticum. Resistance of six metal oxide sensors was decreased in dried sample compared with fresh one.

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Monitoring of Preservatives Produced Naturally in Vegetable Raw Materials (식물성 원료 중 천연유래 보존료의 함유량 조사)

  • Soo Bin Lee;Ji Sun So;Geum Jae Jeong;Hye Seon Nam;Jae Myeong Oh;Soon Ho Lee
    • Journal of Food Hygiene and Safety
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    • v.39 no.2
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    • pp.152-162
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    • 2024
  • In this study, we investigated the levels of the natural preservatives, benzoic acid, sorbic acid, and propionic acid, in raw unprocessed vegetables. Quantitative analysis of benzoic acid and sorbic acid was performed using high-performance liquid chromatography with a diode array detector (HPLC-DAD) and confirmed using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Propionic acid was analyzed using a gas chromatography-flame ionization detector (GC-FID) and confirmed using gas chromatography-mass spectrometry (GC-MS). From a total of 497 samples, benzoic acid, sorbic acid, and propionic acid were found in 50 (10%), 8 (0.2%), and 61 samples (12.3%), respectively. The highest quantity of benzoic acid, sorbic acid, and propionic acid was found in peony root (1,057 mg/kg), nut-bearing torreya seeds (27.3 mg/kg), and myrrha (175 mg/kg), respectively. The background concentration range of naturally occurring preservatives in raw vegetables determined in this study could be used as standard inspection criteria to address consumer complaints and trade disputes.

Determination of Volatile Organic Compounds (VOCs) Using Tedlar Bag/Solid-phase Microextraction/Gas Chromatography/Mass Spectrometry (SPME/GC/MS) in Ambient and Workplace Air

  • Lee, Jae-Hwan;Hwang, Seung-Man;Lee, Dai-Woon;Heo, Gwi-Suk
    • Bulletin of the Korean Chemical Society
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    • v.23 no.3
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    • pp.488-496
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    • 2002
  • SPME techniques have proven to be very useful tools in the analysis of wide VOCs in the air. In this study, we estimated VOCs in ambient and workplace air using a Tedlar ba /SPME/GC/MS system. The calibration curve was set to be linear over the range of 1-30 ppbv. The detection limits ranged from 10 pptv to 0.93 ppbv for all VOCs. Reproducibility of TO-14 target gas mixtures by SPME/GC/MS averaged at 8.8 R.S.D (%). Air toxic VOCs (hazardous air pollutants, HAPs) containing a total of forty halohydrocarbons, aromatics, and haloaro-matic carbons could be analyzed with significant accuracy, detection limit and linearity at low ppbv level. Only reactive VOCs with low molecular weight, such as chloromethane, vinylchloride, ethylchloride and 1,2-dichloro-ethane, yielded relatively poor results using this technique. In ambient air samples, ten VOCs were identified and quantified after external calibration. VOC concentration in ambient and workplace air ranged from 0.04 to 1.85 ppbv. The overall process was successfully applied to identify and quantify VOCs in ambient/workplace air.

Glycosyl glycerides from the stems of 'Baekma' cultivar of Chrysanthemum morifolium (국화 '백마'(Chrysanthemum morifolium) 줄기로부터 glycosyl glyceride 의 분리 및 동정)

  • Oh, Hyun-Ji;Kim, Hyoung-Geun;Pak, Ha-Seung;Baek, Yun-Su;Kwon, Oh-Keun;Shin, Hak-Ki;Baek, Nam-In
    • Journal of Applied Biological Chemistry
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    • v.61 no.2
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    • pp.131-134
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    • 2018
  • The stem of Chrysanthemum morifolium, 'Baekma', were repeatedly extracted with 80% aqueous MeOH and the concentrates was partitioned into ethyl acetate (EtOAc), n-butyl alcohol and $H_2O$ fraction. The repeated silica gel and octadecyl silica gel column chromatographies for the EtOAc fractions led to isolation of two glycosyl glycerides. The chemical structures of the compounds were determined as (2S)-1-O-${\beta}-{\text\tiny{D}}$-galactopyranosyl-2,3-dilinoleoylglycerol (1) and (2S)-1-O-${\beta}-{\text\tiny{D}}$-galactopyranosyl-2,3-dipalmitoylglycerol (2) based on spectroscopic data anlyses including nuclear magnetic resonance, mass sperctrometry, and infrared spectrometry and gas chromatography mass spectrometry.

Flavor Components of the Fruit Peel and Leaf Oil from Zanthoxylum piperitum DC (초피(Zanthoxylum piperitum DC)의 과피와 잎의 방향성분)

  • Kim, Jung-Han;Lee, Kyung-Seok;Oh, Won-Taek;Kim, Kyoung-Rae
    • Korean Journal of Food Science and Technology
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    • v.21 no.4
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    • pp.562-568
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    • 1989
  • The essential oils from ripe fruit peel and leaf of Zanthoxylum piperitum DC were extracted by gas co-distillation method and analyzed by gas chromatography/mass spectrometry (GC/ MS) and retention index matching. The experimental results revealed the presence of over 100 volatile components. Major components were 1,8-cineol (25.47%), limonene (11.91%), geranyl acetate (9.01%), myrcene (6.15%) in fruit peel and citronellal (23.11%), 1,8-cineol (18.38%), citronellol (6.04%) in leaf. Among the components identified were the following; in fruit peel, ${\alpha}-pinene$ and 13 hydrocarbons, linalool and 8 alcohols, citronellal and 3 aldehydes, carvone and 2 kotones, methyl salicylate and 7 esters, and 1,8-cineol and oxides, and in leaf, ${\alpha}-pinene$ and 7 hydrocarbons, linalool and 7 alcohols, citronellyl acetate and 5 esters, citronellal and 1 aldehyde, carvone, and 1,8-cineol and 1 oxide.

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Analysis of Phytochemicals in Popular Medicinal Herbs by HPLC and GC-MS (HPLC와 GC/MS를 활용한 약용식물 유래 phytochemicals 분석)

  • Cho, Hyun-Jung;Yoo, Dong-Chan;Cho, Hyun-Nam;Fan, Lu-An;Kim, Hee-Joon;Khang, Kong-Won;Jeong, Ho-Soon;Yang, Seun-Ah;Lee, In-Seon;Jhee, Kwang-Hwan
    • Korean Journal of Food Science and Technology
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    • v.40 no.3
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    • pp.277-282
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    • 2008
  • Oriental herbs are reported as having potent functions for preventing many types of diseases. They also appear to have positive effects and potential capabilities for skin care. Among the many oriental herbs that are available, we chose to analyze four medicinal herbs, Korean red ginseng, Artemisia capillaries Thunb, Schizonepeta tenuifolia Briq, and Foeniculum vulgare Mill, because all are popular and considered as favorite medicinal plants in Korea. Extracts of the herbs were obtained by various methods such as using distilled water, ethyl ether, methanol, ethanol, benzene, 1-butanol, and chloroform. Nine phytochemicals were detected in the extracts: maltol, adenosine, b-pinene, menthone, pulegone, limonene, anethole, estragole, and fenchone, which reportedly have multi-functionalities. All phytochemicals were analyzed quantitatively by various chromatographic techniques such as HPLC and gas chromatography-mass (GC-MS) spectrometry. This article also presents the optimum conditions for extracting these 9 targeted phytochemical compounds that were derived from 4 popular oriental herbs, which could be useful for the efficient preparation of each phytochemical.

GC-MS analysis of Salicornia herbacea L. extracts with trimethylsilyl derivatization (Trimethylsilyl 유도체화 방법을 적용한 함초 추출물의 GC-MS 분석)

  • Kyoung-In Lee;Geun-Jik Lee;Young-Seung Yoon
    • Journal of Marine Bioscience and Biotechnology
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    • v.15 no.2
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    • pp.96-102
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    • 2023
  • Salicornia herbacea, a noted halophyte, has been widely researched for its diverse physiological activities. The continuous exploration of its compounds is essential. This study employed gas chromatography (GC) coupled with mass spectrometry (MS) for qualitative analysis. This involved pretreatment including trimethylsilyl (TMS) derivatization of the S. herbacea extract, facilitating its GC analysis. Five compounds, including various fatty acids and β-sitosterol, were identified by direct analysis of the methanol extract of S. herbacea without pretreatment by GC-MS. Conversely, the analysis of the TMS-derivatized extract revealed 28 distinct peaks. Quantitative analysis further indicated that the predominant compounds in the S. herbacea extract were sugars and sugar derivatives, notably glucose, fructose, and glucitol. The collective concentration of these sugars and its derivatives amounted to 116.45 mg/g, representing 11.6% of the dry weight of the raw S. herbacea. Following sugars and their derivatives, fatty acids constituted the next most abundant group of compounds. However, the presence of amino acids and organic acids was relatively low.

Alternative Sample Preparation Techniques in Gas Chromatographic-Mass Spectrometric Analysis of Urinary Androgenic Steroids

  • Cho, Young-Dae;Choi, Man-Ho
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1315-1322
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    • 2006
  • The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.