• Title/Summary/Keyword: GC/MS spectrometry

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The Screening and Pattern Comparison of Organic Acids in 3 Kinds of Medicinal Herbal Extracts (3가지 약용 허브 추출물에 함유된 유기산 검색 및 조성 비교)

  • Chung, Ha-Yull;Jung, Do-Hyun;Park, Young-Joon
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.997-1001
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    • 2000
  • The organic acids in 3 kinds of medicinal herbal extracts were screened and compared each other according to their organic acid contents by an efficient gas chromatographic method. It involves solid-phase extraction of organic acids using Chromosorb P with subsequent conversion to stable tert-butyldimethysilyl derivatives for the direct analysis by capillary column gas chromatography and gas chromatography-mass spectrometry. Total of 24 organic acids were reproducibly identified from 3 kinds of herbal extracts. When the GC profiles were simplified to their retention index spectra, characteristic patterns were obtained for each herb sample. As expected, three kinds of herbal extracts showed three distinct patterns.

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Simultaneous Analytical Method for the Neomycin, Gentamicin Residues in Seafood (수산물 중 네오마이신, 겐타마이신 동시분석법 개발)

  • Hong, Young-Min;Lee, Seok-Ki;Kim, Hyoung-Ah;Hwang, Yu-Kyung
    • Journal of Applied Biological Chemistry
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    • v.53 no.1
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    • pp.25-30
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    • 2010
  • This paper describes a simultaneous method for the determination of two aminoglycosides (neomycin and gentamicin) using solid phase extraction followed by liquid chromatograph-mass spectrometry. The extract was applied to an WCX and HLB solid phase extraction cartridge. The cartridges were washed with water and methanol, and analytes were eluted with TCA buffer-acetonitrile mixture. The aminoglycosides were separated by ion-pairing reversed phase mode prior to ESI-LC/MS. Under the conditions applied neomycin was almost separated from all the gentamicin compounds. No interfering peaks from endogenous compounds of matrix were noted at the elution position of the analytes. Recoveries of neomycin fortified at levels of 0.25, 0.5, 1.0 and 2.0 mg/kg seafood samples ranged from 92 to 115%. Recoveries of gentamycin fortified at levels of 0.05, 0.1, 0.2, 0.4 mg/kg seafood samples ranged from 99 to 116%. Method detection limits in four seafood sample matrices were between 0.002 and 0.033 mg/kg.

Simple Method in Trace Analysis of Phthalates in Cosmetics : Analytical Conditions and Skills for Better Results (화장품에서 프탈레이트 미량분석을 위한 간편한 분석법 : 향상된 결과를 위한 분석조건과 기술)

  • Kim, Min-Kee;Jung, Hye-Jin;Chang, Ih-Seop
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.1
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    • pp.51-55
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    • 2008
  • Although phthalates aren't used as an cosmetic ingredient, some cosmetics especially nail lacquer, hair spray, and perfume still have phthalates. This is mainly caused by contamination and carryover during manufacturing process, so analysis of phthalates in those cosmetics has became a very important thing for quality-assurance(Q.A). The main phthalates under debate are diethyl phthalate(DEP), dibutyl phthalate(DBP), and bis(2-ethylhexyl) phthalate (DEHP) in domestic market. Gas chromatography-mass spectrometry(GC-MS) coupled with solvent extraction and concentration has been used for ppm level and sub ppm level analysis of phthalates. It requires much time and cost to use mass spectrometric detector and to prepare the test solution. Moreover analysis of phthalates at low concentrations is difficult because of contamination which results in wrong analytical results. In the present study, we showed a simple method using gas chromatography-flame ionization detector(GC-FID) which has fast analysis time, minimum use of solvent, reduced sample preparation steps for minimizing contamination and quantitative range of $2{\sim}50{\mu}g/g(ppm)$ in products. Consequently, this method will be proper for Q.A analysis in related companies.

Essential Oil Composition from Leaves, Flowers, Stems, and Fruits of Vitex rotundifolia L. fil. (순비기나무(Vitex rotundifolia L. fil.)의 부위별 정유성분 조성)

  • Jang, Soo-Jung;Kim, Young-Hoi;Kim, Myung-Kon;Kim, Kei-Whan;Yun, Sei-Eok
    • Applied Biological Chemistry
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    • v.45 no.2
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    • pp.101-107
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    • 2002
  • The essential oils isolated from leaves, flowers, stems, and fruits of Vitex rotundifolia by steam distillation and extraction (SDE) method were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS). A total of 76 components detected by GC, 42 components were identified positively by GC-MS and GC co-injection with authentic standards, and 34 components were identified tentatively by mass spectral data only. They included 16 monoterpene hydrocarbons, 30 oxygenated hydrocarbons, 10 sesquiterpene hydrocarbons, 8 oxygenated sesquiterpenes, 3 diterpenes, and 9 miscellaneous components. The major components in the oil from the leaves were ${\alpha}-pinene$ (30.25%), 1,8-cineole (19.89%), sabinene (9.56%), ${\alpha}-terpineol$ (7.94%), ${\beta}-pinene$ (5.69%), and terpinen-4-ol (2.37%), and those in the flower oil were ${\alpha}-pinene$ (25.47%), 1,8-cineole (7.69%), manoyl oxide (6.21%), ${\beta}-pinene$ (4.20%), ${\alpha}-te.pineol$ (3.76%), and sabinene (2.78%). The major components in the oil from the stems were ${\alpha}-pinene$ (13.24%), ${\alpha}-terpineol$ (10.64%), 1,8-cineole (4.40%), manoyl oxide (4.02%), ${\beta}-pinene$ (2.39%), and terpinen-4-ol (2.21%) while those in the oil from the fruits were ${\alpha}-pinene$ (20.24%), 1,8-cineole (11.47%), ${\beta}P-pinene$ (9.79%), ${\alpha}-terpineol$ (7.08%), sabinene (3.68%), and limonene (2.77%). The percentage composition of monoterpenes in the oils from the leaves and the fruits were higher than in those from the flowers and the stems, whereas the oil from the flowers and the stems were characterized by a large content of sesquiterpenes, diterpenes and other unknown high molecular weight components.

Safety Profile Assessment and Identification of Volatile Compounds of Krill Eupausia superba Oil and Residues Using Different Extraction Methods

  • Haque, A.S.M. Tanbirul;Kim, Seon-Bong;Lee, Yang-Bong;Chun, Byung-Soo
    • Fisheries and Aquatic Sciences
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    • v.17 no.2
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    • pp.159-165
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    • 2014
  • In this study, Krill Eupausia superba oil was extracted using different solvents and supercritical carbon dioxide (SC-$CO_2$). During SC-$CO_2$ extraction, the pressure was set at 40 MPa and temperatures ranged from $40^{\circ}C$ to $55^{\circ}C$. We examined the differences in volatile compounds and safety profiles among extraction methods. Volatile compounds were determined using the thermal desorption system integrated with gas chromatography-mass spectrometry (GC-MS). Heavy metal content was analyzed by inductively coupled plasma mass spectrometry (ICP-MS). According to our results 10 volatile compounds were identified in krill sample. After SC-$CO_2$ extraction of oil, the concentrations of volatile compounds decreased, but increased after solvent extraction. In krill, heavy metal concentrations remained within the permissible limit. Moreover, Zn and Fe which have health benefits were detected at high concentrations. During a 90 days storage period at different temperatures, microbial activity was found to be lowest in SC-$CO_2$ extracted residues. Thus, the quality of krill oil and the residues obtained using SC-$CO_2$ extraction was higher and the oil was safer than those obtained using conventional solvent extraction. These results can be applied to the food industry to maintain high quality krill products.

Analysis of Iridoid Glycoside and GABA Content in the Roots of the Rehmannia glutinosa Cultivars (지황 품종별 뿌리에서 Iridoid 배당체와 GABA 분석)

  • Lee, Sang Hoon;Yoon, Jeong Su;Kim, Jae Kwang;Park, Chun Geun;Chang, Jae Ki;Kim, Yeon Bok
    • Korean Journal of Medicinal Crop Science
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    • v.25 no.3
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    • pp.146-151
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    • 2017
  • Background: Rehmannia glutinosa is a perennial herb belonging to the family Scrophulariaceae. Its roots have been utilized as a traditional medicine. The aim of this study was to elucidate the basic information of the roots of the R. glutinosa cultivars and their utilization. Methods and Results: The roots of R. glutinosa cultivars were harvested in the end of March. The two iridoid glycosides, aucubin and catalpol, were analyzed by liquid chromatography/mass spectrometry (LC/MS), whereas ${\gamma}-aminobutyric$ acid (GABA) was analyzed by gas chromatography/mass spectrometry (GC/MS). The aucubin content was the highest in the Dakang cultivar, whereas no aucubin was detected in the five cultivars. All cultivars had more than 12 mg/g catalpol content, and the maximum catalpol content was found in Jihwang 1. The GABA content was the highest in Suwon 1, and it was 40 times more than that in the Yeongang cultivar. Conclusions: The highest aucubin, catapol and GABA contents were detected in the Dakang, Jihwang 1, and Suwon 1, cultivars respectively. This study provides the crucial information regarding the versatile utilization and pedigree selection of R. glutinosa cultivars.

Determination of trace icing Inhibitors (ether type) in free-floating fuels by gas chromatography-mass spectrometry

  • Shin, Ho-Sang;Ahn, Hye-Sil;Jung, Dong-Gyun
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.04a
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    • pp.196-200
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    • 2003
  • A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of ethylene glycol monomethyl ether (EGME) and diethylene glycol monomethyl ether (DEGME) in spilled aviation fuels. Ethylene glycol monobutyl ether (EGBE) and ethylene glycol monoethyl ether (EGEE) were used as internal standard and surrogate, respectively. The sample preparation consists of back-extraction with 7 mL of methylene chloride after extraction of 50 mL of fuel with 2 mL of water. The extract was concentrated to dryness and dissolved with 100L of methanol and analyzed by CC-MS (SIM). The peaks had good chromatographic properties by using semi-polar column and the extraction of these compounds from fuel also gave high recoveries of 75 and 85 % with small variations for EGME and DEGME, respectively. Method detection limits were 1.3 ng/mL for EGME and 1.0 ng/mL for DEGME in spilled fuel. The method may be useful for fuel-type differentiation between kerosene and JP-8, which may originate from the storage tank.

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Metabolome-Wide Reprogramming Modulated by Wnt/β-Catenin Signaling Pathway

  • Soo Jin Park;Joo-Hyun Kim;Sangtaek Oh;Do Yup Lee
    • Journal of Microbiology and Biotechnology
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    • v.33 no.1
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    • pp.114-122
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    • 2023
  • A family of signal transduction pathways known as wingless type (Wnt) signaling pathways is essential to developmental processes like cell division and proliferation. Mutation in Wnt signaling results in a variety of diseases, including cancers of the breast, colon, and skin, metabolic disease, and neurodegenerative disease; thus, the Wnt signaling pathways have been attractive targets for disease treatment. However, the complicatedness and large involveness of the pathway often hampers pinpointing the specific targets of the metabolic process. In our current study, we investigated the differential metabolic regulation by the overexpression of the Wnt signaling pathway in a timely-resolved manner by applying high-throughput and un-targeted metabolite profiling. We have detected and annotated 321 metabolite peaks from a total of 36 human embryonic kidney (HEK) 293 cells using GC-TOF MS and LC-Orbitrap MS. The un-targeted metabolomic analysis identified the radical reprogramming of a range of central carbon/nitrogen metabolism pathways, including glycolysis, TCA cycle, and glutaminolysis, and fatty acid pathways. The investigation, combined with targeted mRNA profiles, elucidated an explicit understanding of activated fatty acid metabolism (β-oxidation and biosynthesis). The findings proposed detailed mechanistic biochemical dynamics in response to Wnt-driven metabolic changes, which may help design precise therapeutic targets for Wnt-related diseases.

A Study on the Decomposition Characteristics of PVC and PS Mixtures with ZnO in Air Atmosphere (공기분위기에서 ZnO를 첨가한 PVC와 PS 혼합물의 분해특성에 관한 연구)

  • Oh, Sea Cheon;Jung, Myung Uk;Jun, Hyun-Chul;Kim, Hee Taik;Lee, Hae Pyeong
    • Applied Chemistry for Engineering
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    • v.17 no.2
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    • pp.229-234
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    • 2006
  • The effect of ZnO in the decomposition of poly(vinyl chloride) (PVC) and polystyrene (PS) mixtures in air atmosphere has been studied by thermogravimetry (TG) and gas chromatograph-mass spectrometry (GC-MS) under various mixing ratios and reaction temperatures. From this work, it can be seen that the yields of a liquid product were increased with the increase of PS in mixtures, whereas those of gaseous products were decreased. And the yields of a gaseous product and HCl were decreased with the increase of ZnO in mixtures. It was also found that HCl was rarely produced at ZnO/Mixture = 0.5 by the effect of ZnO in dehydrochlorination of PVC.

Gibberellins Production and Identification of Endophytic Fungi Isolated from Aquatic Plant in Fresh Water (담수에 자생하는 수생식물에서 분리된 내생균류의 지베렐린 생산과 동정)

  • You, Young-Hyun;Kang, Sang-Mo;Choi, Yu-Mi;Lee, Myung-Chul;Kim, Jong-Guk
    • The Korean Journal of Mycology
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    • v.43 no.1
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    • pp.71-76
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    • 2015
  • Aquatic plant Hydrocharis dubia (Blume) Backer was collected from the Dalsung wetland in Daegu. Sixteen endophytic fungi with different colony morphologies were isolated from the roots of aquatic plants. Waito-c rice (WR) seedlings were treated with fungal culture filtrates (FCF) for screening plant growth-promoting activity. In the results, HD1008 strain isolated from aquatic plant showed highest plant growth-promoting activity. The FCF of HD1008 strain was analyzed using gas chromatography mass spectrometry (GC/MS) with selected ion monitoring (SIM). Analysis of the FCF of HD1008 strain found that it contained gibberellins (GA) ($GA_1$, 1.2 ng/100 mL; $GA_4$, 5 ng/100 mL). Phylogenetic tree of HD1008 strain was constructed by partial internal transcribed spacer (ITS) region and partial beta-tubulin gene sequences. Therefore, we describe HD1008 strain as a new gibberellin-producing Penicillium trzebinskii based on morphological and molecular characteristics.