• Title/Summary/Keyword: gas chromatography/mass spectrometry

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Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7179-7188
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    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.

Determination of geosmin and 2-MIB in Nakdong River using headspace solid phase microextraction and GC-MS (HS-SPME-GC/MS를 이용한 낙동강 수계 하천수 중 조류기원성 냄새물질 분석)

  • Lee, Injung;Lee, Kyoung-Lak;Lim, Tae-Hyo;Park, Jeong-Ja;Cheon, Seuk
    • Analytical Science and Technology
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    • v.26 no.5
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    • pp.326-332
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    • 2013
  • Geosmin and 2-methylisoborneol (2-MIB) are volatile organic compounds responsible for the majority of unpleasant taste and odor events in drinking water. Geosmin and 2-MIB are byproducts of blue-green algae (cyanobacteria) with musty and earthy odors. These compounds have odor threshold concentration at ng/L levels. It is needed to develop a sensitive method for determination of geosmin and 2-MIB to control the quality of drinking water. In this study, geosmin and 2-MIB in water samples were determined by gas chromatography-mass spectrometry (GC-MS) with headspace-solid phase microextraction (HS-SMPE). The detection limits of this method were 1.072 ng/L and 1.021 ng/L for geosmin and 2-MIB, respectively. Good accuracy and precision was also obtained by this method. Concentrations of the two compounds were measured in raw waters from Nakdong River in the cyanobacterial blooming season. Water bloom formed by cyanobacteria has been occurred currently in Nakdong River. It is needed to investigate the concentrations of geosmin and 2-MIB to control the quality of drinking water from Nakdong River. Both geosmin and 2-MIB were detected in raw waters from Nakdong River at concentrations ranging from 4 to 24 ng/L and 6 to 16 ng/L, respectively.

Determination of Residue Levels of Ethyl Carbamate in Alcoholic Beverages by Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS) (가스크로마토그래피/질량분석기(GC/MS/MS)를 이용한 주류 중 에틸카바메이트 잔류량 조사)

  • Kim, Dong-Ho;Jang, Han-Sub;Choi, Gu-Il;Kim, Hyun-Jung;Kim, Ho-Jin;Kim, Hyo-Lin;Kim, Keun-Sung
    • Journal of Food Hygiene and Safety
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    • v.28 no.1
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    • pp.63-68
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    • 2013
  • Ethyl carbamate (EC) is a contaminant generated in the fermentation processes of various fermented foods. In this study, residue levels of EC in 95 alcoholic beverage samples were determined by using Gas Chromatography/Tandem Mass Spectrometry (GC/MS/MS). All the samples were purified by a liquid-liquid extraction (LLE) method using dichloromethane. The LLE method enables an improvement in time and cost to detection and specificity over the conventional extraction methods. The limits of detection and quantification (LOD and LOQ) to analyze EC were 1.3 and 4.0 ng/mL, respectively. The recovery rates of EC were ranged from 90.0 to 97.5% at the levels of 50, 100, and 500 ug/L. Among traditional grain-based alcoholic beverage samples (n = 34), the average residue levels of EC in takju, yakju, and cheongju were 0.63, 7.01, and 14.11 ug/L, respectively. Among fruit-based alcoholic beverage samples (n = 48), those of EC in japanese apricot spirits, bokbunjaju, grape wines, and other fruit wines were 79.18, 1.66, 2.64, and 2.39 ug/L, respectively. Among distilled or diluted alcoholic beverage samples (n = 13), those of EC in soju (distilled or diluted), general distillates, liquors, and brandies were 0, 3.30, 8.20, and 8.52 ug/L, respectively. Therefore, this study reports that the residue levels of EC in the alcoholic beverages, distributed in the current domestic markets, did not reach its maximum allowed levels of 30 and 400 ug/L established for grape and fruit wines in Canada, respectively.

Simultaneous Determination and Monitoring of Bisphenols in River Water using Gas Chromatography-Mass Spectrometry (GC-MS 를 이용한 하천수 중 Bisphenol계 화합물의 동시분석 및 모니터링)

  • Kim, Jihyun;Choi, Jeong-Heui;Kang, Tae-Woo;Kang, Taegu;Hwang, Soon-Hong;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.36 no.3
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    • pp.154-160
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    • 2017
  • BACKGROUND:This study was carried out to establish an efficient sample preparation for the simultaneous determination of bisphenols (BPs) in river water samples using gas chromatography-mass spectrometry (GC-MS). Sample preparation was examined with conventional extraction methods, such as solid-phase extraction (SPE) and liquid-liquid extraction (LLE), and their efficiency was compared with validation results, including linearity of calibration curve, method detection limit (MDL), limit of quantification (LOQ), accuracy, and precision. METHODS AND RESULTS:The BPs (bisphenol A, BPA; bisphenol B, BPB; bisphenol C, BPC; bisphenol E, BPE; bisphenol F, BPF; bisphenol S, BPS) were analyzed using GC-MS. The range of MDLs by SPE and LLE methods was $0.0005{\sim}0.0234{\mu}g/L$ and $0.0037{\sim}0.2034{\mu}g/L$, and that of LOQs was $0.0015{\sim}0.0744{\mu}g/L$ and $0.0117{\sim}0.6477{\mu}g/L$, respectively. The calibration curve obtained from standard solution of $0.004{\sim}4.0{\mu}g/L$ (SPE) and $0.016{\sim}16{\mu}g/L$ (LLE) showed good linearity with $r^2$ value of 0.9969 over. Accuracy was 93.2~108% and 97.4~120%, and precision was 1.7~4.6% and 0.7~6.5%, respectively. The values of MDL and LOQ resulted from the SPE method were higher than those from the LLE method, particularly those values of BPA were highest among the BPs. Based on the results, the SPE method was applied to determine the BPs in river water samples. Water samples were collected from mainstream, tributary and sewage wastewater treatment plants (SWTPs) in the Yeongsan river basin. The concentration of BPB, BPC, BPE, BPF and BPS were not detected in all sites, whereas BPA was ranged $0.0095{\sim}0.2583{\mu}g/L$, which was $0.0166{\sim}0.0810{\mu}g/L$ for mainstreams, $0.0095{\sim}0.2583{\mu}g/L$ for tributaries, $0.0352{\sim}0.1217{\mu}g/L$ for SWTPs. CONCLUSION: From these results, the SPE method was very effective for the simultaneous determination of BPs in river water samples using GC-MS. We provided that it is a convenient, reliable and sensitive method enough to monitor and understand the fate of the BPs in aquatic ecosystems.

Comparison of Volatile Compounds from Thymus Magnus Nakai by Three Different Extraction Methods (추출방법에 따른 섬백리향의 휘발성 향기성분 비교)

  • Lee, Sa Eun;Kim, Songmun;Lim, Won Churl;Kang, Ki Choon;Pyo, Hyeong Bae
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.2
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    • pp.171-178
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    • 2014
  • The purpose of this study was to analyse the volatile components of Thymus magnus Nakai extracted by different extraction methods and reproduce scent close to original plant based on the results. For this purpose, the essential oil of T. magnus was extracted by supercritical fluid extraction (SFE), water and steam distillation (WSD) and simultaneous steam distillation and extraction (SDE) methods. The compositions of the essential oil were analyzed by gas chromatography-mass spectrometry (GC-MS). Consequently, linalool (0.1%) and trans-sabinene hydrate (0.9%) contents in the essential oil extracted by SFE method of $40^{\circ}C$ - 400 bar condition were relatively higher than compositions of the essential oil extracted by different conditions. The contents of borneol (3.82%), terpinen-4-ol (0.3%) and caryophyllene oxide (2.2%) were relatively higher at $50^{\circ}C$ - 400 bar and the contents of ${\beta}$-bisabolene (5.88%), 1-octen-3-ol (0.31%), caryophyllene (2.91%), p-cymene (2.04%) and ${\gamma}$-terpinene (0.52%) were extracted relatively higher at $50^{\circ}C$ - 300 bar. The compositions of the essential oil extracted by SFE method of $50^{\circ}C$ - 200 bar condition contained relatively higher contents of thymol (77.63%) and carvacrol (5.65%). The contents of ${\alpha}$-bisabolol (0.17%), caryophyllene (6.46%), cis-${\alpha}$-bisabolene (1.52%) and ${\beta}$-bisabolene (20.65%) in the essential oil extracted by WSD method were relatively higher than compositions of the essential oil extracted by SFE method, and by SDE method we couldn't obtained essential oil. The results of this study could be utilized to reproduce scent close to original scent of T. magnus.

Comparative analysis of volatile and non-volatile flavor compounds in rice paste made by α-amylase according to cultivars (α-amylase를 이용하여 제조한 쌀 페이스트의 품종에 따른 휘발성비휘발성 향미성분 비교분석)

  • Son, Eun Young;Kim, Hye Won;Kim, Sun Ah;Lee, Sang Mi;Paek, Se Hee;Kim, Sun Hee;Seo, Yong Ki;Park, Hye-Young;Oh, Sea-Kwan;Kim, Young-Suk
    • Journal of Applied Biological Chemistry
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    • v.60 no.3
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    • pp.283-291
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    • 2017
  • Rice that the half of population in the world eats as a staple food is mostly produced and consumed in Asia. However, its consumption is nowadays decreasing mainly due to diet diversity. Accordingly, some attempts are in demand to enhance the utilization of rice. In this study, profiling of volatile and non-volatile flavor components in rice pastes obtained by ${\alpha}$-amylase was performed and compared according to nine different rice cultivars domestically cultivated in Korea using gas chromatography-mass spectrometry combined by solid phase microextraction and gas chromatography-time of flight-mass spectrometry after a derivatization, respectively. In total, 46 volatile compounds identified included 6 alcohols, 6 aldehydes, 4 esters, 4 furan derivatives, 4 ketones, 1 acid, 1 sulfur-containing compound, 7 hydrocarbons, 5 aromatics and 8 terpenes. The non-volatile flavor components found were composed of 12 amino acids, 6 sugars and 4 sugar alcohols. In principal component analysis, rice paste samples could be discriminated according to cultivars on the score plots of volatile and non-volatile flavor compounds. In particular, some volatile compounds such as pentanal and 4,7-dimethylundecane could contribute to distinguish Senong 17 white and Senong 17 brown, whereas ethanol, 6-methylhep-5-en-2-one, and tridecane could be highly related to the discrimination of Iipum from other cultivars. Among non-volatile compounds, some amino acids such as glycine, serine and ${\gamma}$-aminobutyric acid and some sugars such as sucrose and fructose were mainly responsible for the discrimination of Danmi from the other cultivars. On the other hand, galactose, arabitol and mannose were more closely related to Senong 17 white than Senong 17 brown.

Determination of Petroleum Aromatic Hydrocarbons in Seawater Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography/Mass Spectrometry (HS-SPME-GC/MS를 이용한 해수 내 유류계 방향족탄화수소 분석법)

  • An, Joon Geon;Shim, Won Joon;Ha, Sung Yong;Yim, Un Hyuk
    • Journal of the Korean Society for Marine Environment & Energy
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    • v.17 no.1
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    • pp.27-35
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    • 2014
  • The headspace solid-phase microextraction (HS-SPME) followed by gas chromatography/mass spectrometry procedure has been developed for the simultaneous determination of petroleum aromatic hydrocarbons such as benzene, toluene, ethylbenzene and xylene isomers (BTEX) and polycyclic aromatic hydrocarbons (PAHs) in seawater. The advantages of SPME compared to traditional methods of sample preparation are ease of operation, reuse of fiber, portable system, minimal contamination and loss of the sample during transport and storage. SPME fiber, extraction time, temperature, stirring speed, and GC desorption time were key extraction parameters considered in this study. Among three kinds of SPME fibers, i.e., PDMS ($100{\mu}m$), CAR/PDMS ($75{\mu}m$), and PDMS/DVB ($65{\mu}m$), a $65{\mu}m$ PDMS/DVB fiber showed the most optimal extraction efficiencies covering molecular weight ranging from 78 to 202. Other extraction parameters were set up using $65{\mu}m$ PDMS/DVB. The final optimized extraction conditions were extraction time (60 min), extraction temperature (50), stirring speed (750 rpm) and GC desorption time (3 min). When applied to artificially contaminated seawater like water accommodated fraction, our optimized HS-SPME-GC/MS showed comparable performances with other conventional method. The proposed protocol can be an attractive alternative to analysis of BTEX and PAHs in seawater.

Characterization of Traditional Korean Unifloral Honey Based on the Mono-, Di-, and Trisaccharides (한국산 벌꿀의 밀원별 단당, 이당 및 삼당류의 정량 특성)

  • Jang, Eun-Sook;Kim, In-Suk;Lee, Eun-jin;Seo, Hyun-Sun;Lee, Hye-joung;Kim, Eun;Kim, Kyung-Tae;Kim, Jong-Bae
    • Korean Journal of Food Science and Technology
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    • v.48 no.1
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    • pp.1-8
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    • 2016
  • Sugar profiles of 45 Korean honey samples (15 acacia, 15 multi-floral, 10 chestnut, and 5 artificial honey samples), which are commercially available in the Korean markets, were analyzed using gas chromatography/mass spectrometry (GC/MS) through TMS-oxime and TMS-methoxime derivatization. The average invert sugar contents in acacia, multi-floral, chestnut, and artificial honey samples were $71.2{\pm}1.05$, $68.7{\pm}3.26$, $63.2{\pm}1.85$, and $68.0{\pm}2.10%$, respectively. Fourteen disaccharides were detected from the samples, and the average content of major disaccharides was higher in order of turanose, maltulose, maltose, trehalulose, kojibiose, isomaltose, and nigerose. The average content of total disaccharides was highest in chestnut and lowest in acacia. Seven trisaccharides were detected from the samples, and the average content of trisaccharides was the highest in artificial honeys, which had high erlose content. The total content of disaccharides and trisaccharides was highest ($16.0{\pm}2.03%$) in chestnut honey and lowest ($9.70{\pm}1.75%$) in acacia honey.

Classification and identification of organic aerosols in the atmosphere over Seoul using two dimensional gas chromatography-time of flight mass spectrometry (GC×GC/TOF-MS) data (GC×GC/TOF-MS를 이용한 서울 대기 중 유기 에어로졸의 분류 및 동정)

  • Jeon, So Hyeon;Lim, Hyung Bae;Choi, Na Rae;Lee, Ji Yi;Ahn, Yun Kyong;Kim, Yong Pyo
    • Particle and aerosol research
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    • v.14 no.4
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    • pp.153-169
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    • 2018
  • To identify a variety of organic compounds in the ambient aerosols, the two-dimensional gas chromatography-time of flight mass spectrometry (GCxGC) system (2DGC) has been applied. While 2DGC provides more peaks, the amount of the generated data becomes huge. A two-step approach has been proposed to efficiently interpret the organic aerosol analysis data. The two-dimensional 2DGC data were divided into 6 chemical groups depending on their volatility and polarity. Using these classification standards, all the peaks were subject to both qualitative and quantitative analyses and then classified into 8 classes. The aerosol samples collected in Seoul in summer 2013 and winter 2014 were used as the test case. It was found that some chemical classes such as furanone showed seasonal variation in the high polarity-volatile organic compounds (HP-VOC) group. Also, for some chemical classes, qualitative and quantitative analyses showed different trends. Limitations of the proposed method are discussed.

A Study on the analysis method and composition characteristics of organic materials in the pottery excavated at the palace site in Yongjangseong Fortress, Jindo (진도 용장성 왕궁지 출토 도기호 내부 유기물의 분석법과 성분 특성 연구)

  • YUN Eunyoung;YU Jia;KIM Kyuho
    • Korean Journal of Heritage: History & Science
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    • v.56 no.3
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    • pp.158-171
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    • 2023
  • Pottery filled with organic materials was excavated from the G-2 building site of Yongjangseong Fortress, Jingo, a relic of the Goryeo Dynasty. In this study, the characteristics of organic material were confirmed by a scientific analysis of organic material in pottery found at the palace in Yongjangseong, Jindo. In addition, it was intended to review the analysis method to identify the natural resin and to secure characteristic components(biomarkers) for each natural resin and use them as basic data in the future. The organic materials in the pottery were analyzed using attenuated total reflectance Fourier-transformed infrared spectroscopy(ATR-FTIR) and gas chromatography mass spectrometry(GC-MS). The infrared spectral characteristics were estimated to be natural resin, and biomarkers of organic materials were identified as sesquiterpene-based compounds(C15H24, MW 204) and derivatives. The lacquer(T.vemicifluum) is composed mainly of alkenes, alkanes, and catechol. Pine resin(P.densiflora), on the other hand, is primarily composed of diterpenoid(abietic acid, pimaric acid) and Whangchil(yellow lacquer) is identified to have sesquiterpenes(such as selinene, muurolene, calamenene) as its main components. So, the organic material in the pottery can be identified as Whangchil by comparing their compounds with modern resin materials from Dendropanax. morbifera that correspond with the results. Whangchil, which is exuded from the Dendropanax. morbifera, has been used as a natural coating materials since ancient times, and it has been confirmed that the characteristic components are well preserved even 700 years later. It can be assumed that the interior Whangchil was stored not for use as a coating, but rather for ritual purposes when the building was constructed, because the pottery was found near the cornerstone. Furthermore, based on simplified sample preparation using pyrolysis-gas chromatography mass spectrometry(Py-GC-MS), the thermal decomposition products were found to be similar to the characteristic components, suggesting that this method can be applied to the identification of natural resins used in historic artifacts.