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

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Analysis of Volatile Compounds and Enantiomeric Separation of Chiral Compounds of Dried Sancho (Zanthoxylum schinifolium Siebold & Zucc)

  • Seo, Hye-Young;Shim, Sung-Lye;Ryu, Keun-Young;Jung, Min-Seok;Hwang, In-Min;Shin, Dong-Bin;Kwon, Joong-Ho;Schreier, Peter;Kim, Kyong-Su
    • Food Science and Biotechnology
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    • v.18 no.1
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    • pp.18-24
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    • 2009
  • The volatile compounds of dried sancho (Zanthoxylum schinifolium), an aromatic plant were extracted by simultaneous distillation and extraction (SDE) method and identified by gas chromatograph-mass spectrometry (GC-MS). Selected chiral constituents of sancho oil were characterized by enantiodifferentiation using multidimensional gas chromatograph (MDGC)-MS. A total of 57 compounds were identified and quantified, and the major compounds were identified estragole, nonanoic acid, octanoic acid, $\beta$-phellandrenene, and limonene. Among them, estragol (63.9%) was found as the predominantly abundant component of sancho. $\alpha$-pinene and nerolidol, and $\beta$-pinene and linalool were determined to be enantiomerically pure (100%) for their (S)-form and (R)-form, respectively. The enantiomeric composition of limonene in sancho revealed 83.9% purity for the (S)-enantiomer, whereas (E)- and (Z)-rose oxides showed mixtures of both enantiomers. The enantiomeric excess (%) for citronellal was 22.6% with the (R)-enantiomer as major enantiomer. The enantiomeric composition of these compounds can be used as parameter for authenticity control of sancho.

Comparison of the volatile flavor compounds in different tobacco types by different extraction methods (추출방법에 따른 잎담배 종류별 휘발성 향기성분 특성비교)

  • Lee, Jang-Mi;Lee, Jeong-Min;Lee, Chang-Gook;Bock, Jin-Young;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.32 no.2
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    • pp.77-87
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    • 2010
  • Traditional simultaneous distillation extraction(SDE) and solid-phase micro extraction(SPME) methods using GC/MS were compared for their effectiveness in the extraction of volatile flavor compounds from different tobacco leaves types(flue-cured, burley, oriental). The major volatile flavor compounds of flue-cured and burley tobacco were similar such as neophytadiene, solanone, megastigmatrienone isomers, ${\beta}$-damascenone and ${\beta}$-ionone. On the other hand, volatile flavor compounds such as norambreinolide, sclareolide were specifically identified in oriental tobacco. Each method was used to evaluate the responses of some analytes from real samples and standards in order to provide sensitivity comparisons between two techniques. Among three types of SPME fibers such as PDMS(Polydimethylsiloxane), PA(Polyacrylate) and PDMS/DVB (Polydimethylsiloxane/Divinylbenzene) which were investigated to determine the selectivity and adsorption efficiency, PDMS/DVB fiber was selected for the extractions of the volatile flavor compounds due to its effectiveness. The qualitative analysis showed that the total amount of volatile flavor compounds in SDE method(130 species) was much more than that in SPME method(85 species). SPME method was more efficient for all the highly volatile compounds than SDE method, but on the other hand, low-volatile compounds such as fatty acids or high-molecular hydrocabons were detected in SDE method. SPME method based on a short-time sampling can be adjusted to favor a selected group compounds in tobacco. Furthermore this results could be used to estimate the aroma characteristics of cigarette blending by using a different type of tobacco with more effectiveness and convenience.

The Anti-inflammatory Effect of Cheongyeonsan for Allergic Rhinitis (알러지성 비염에 대한 청연산 추출물의 항염증효과)

  • Kim, Jeong Won;Ahn, Sang Hyun;Kim, Ki Bong
    • The Journal of Pediatrics of Korean Medicine
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    • v.32 no.1
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    • pp.19-29
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    • 2018
  • Objectives This study investigated the effects of Cheongyeonsan for allergic rhinitis. Methods First, the GS/MS was used to analyze the effects of Cheongyeonsan by measuring inflammatory markers. Second, 3 groups of 10 6-week-old BALB/c mice were divided into Ctrl (no treatment), ARE (allergic rhinitis-induced without treatment), and CRT (allergic rhinitis-induced after Cheongyeonsan treatment) groups. Ovalbumin (OVA) was used as an antigen to induce allergic rhinitis and sensitization was performed by intraperitoneal injection of 0.1% OVA solution 21, 14, and 7 days before the onset of allergic rhinitis. Allergic rhinitis was induced by dropping OVA solution on the nasal cavity of each mouse for 5 days after the last sensitization. Seven days after the first induction, second induction was introduced by the same method. After making the section, MMP-9, substance P, $TNF-{\alpha}$, $NF-{\kappa}B$ p65, COX-2, iNOS and Nrf, apoptotic cells were observed by Masson trichrome staining, immunohistochemical staining, TUNEL of nasal mucosal tissues of each group. Results GC/MS results showed undecanoic acid. Masson trichrome results showed that the CRT group had less respiratory epithelial damage. Immunohistochemical staining showed CRT group had 58% decrease in MMP-9, 61% decrease in substance P, 55% decrease in $TNF-{\alpha}$, 38% decrease in $NF-{\kappa}B$ p65, 53% decrease in COX-2, 54% decrease in iNOS, 87% increase in Nrf compared to those of the ARE group. TUNEL showed a positive reaction of 84% increase in apoptotic cells greater than that of the ARE group. Conclusions Cheongyeonsan alleviates nasal mucosal damage and reduces inflammatory mediators from allergic rhinitis-induced mice.

A Rapid Preconcentration Method Using Modified GP-MSE for Sensitive Determination of Trace Semivolatile Organic Pollutants in the Gas Phase of Ambient Air

  • He, Miao;Xu, Qingjuan;Yang, Cui;Piao, Xiangfan;Kannan, Narayanan;Li, Donghao
    • Bulletin of the Korean Chemical Society
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    • v.35 no.10
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    • pp.2995-3000
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    • 2014
  • A sensitive concentration method utilising modified gas-purge microsyringe extraction (GP-MSE) was developed. Concentration (reduction in volume) to a microlitre volume was achieved. PAHs were utilised as semivolatile analytes to optimise the various parameters that affect the concentration efficiency. The injection rate and temperature were the key factors that affected the concentration efficiency. An efficient concentration (75.0-96.1%) of PAHs was obtained under the optimised conditions. The method exhibited good reproducibility (RSD values that ranged from 1.5 to 9.0%). The GP-MSE concentration method enhances the volume reduction (concentration factor), leading to a low method detection limit ($0.5-15ngL^{-1}$). Furthermore, this method offers the advantage of small-volume sampling, enabling even the detection of diurnal hourly changes in the concentration of PAHs in ambient air. Utilising this method in combination with GC-MS, the diurnal hourly flux of PAHs from the gas phase of ambient air was measured. Indeed, the proposed technique is a simple, fast, low-cost and environmentally friendly.

Monitoring of Pesticide Residues on Dried Agricultural Products (건조채소류의 잔류농약 실태 조사)

  • Gang, Gyungri;Mun, Sujin;Kim, Gwang-Gon;Yang, Yongshik;Lee, Semi;Choi, Euna;Ha, Dongryong;Kim, Eunsun;Cho, Baesik
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.49-61
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    • 2017
  • The study was conducted for safety evaluation of 208 kinds of residue pesticides on 200 dried agricultural products, which are distributed in Gwangju. The method of monitoring was the second of Multi Class Pesticide Multi-residue Methods in Korean Food Code, and GC-ECD, GC-NPD, GC-MSD, and LC-MS/MS were used as evaluation equipment to analyze. The residue level in pesticides were 15.5% (31 of 200 samples) and 4 samples exceeded MRLs. 4.5 mg/kg of pyraclostrobin (MRL; 3.0 mg/kg) was detected in red pepper, 1.49 mg/kg of chlorpyrifos (MRL; 0.13 mg/kg) in daikon leaves, 38.26 mg/kg of pyridalyl (MRL; 0.25 mg/kg) in pepper leaves, 0.98 mg/kg of chlorpyrifos (MRL; 0.05 mg/kg), respectively. Pesticides were found on the 15 samples among the 21 samples of red pepper which is a fruit vegetable, and this resulted in high detection rate of 71%. In addition, pesticides were detected on chwinamul, shitake, siler divaricata, daikon leaves and others within MRLs. The frequent detected kinds of pesticides were insecticide (47.6%), fungicide (33.3%), acaricide (14.3%), nematicide (4.8%) in the order named, and pesticides were methoxyfenozide > pyraclostrobin > azoxystrobin, chlorantraniprole > novaluron, trifloxystrobin in frequent order.

Analytical Method of Polycyclic Aromatic Hydrocarbons (PAHs) in Petroleum Contaminated Soils - Focused on the 16 US EPA Priority PAHs (유류오염토양 중 다환방향족탄화수소류(PAHs) 분석방법 연구 - US EPA 16종 PAHs를 중심으로)

  • Kim, Ji Young;Kim, Dongho;Kim, Tae Seung;Han, Jin-Suk;Lee, Jai-Young;Noh, Hoe-Jung
    • Journal of Soil and Groundwater Environment
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    • v.17 no.5
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    • pp.20-30
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    • 2012
  • In case of analyzing PAHs (EPA 16 compounds) in oil-contaminated soils, the lump of peaks may occur because of the aliphatic and polar compounds in oil. This phenomenon is due to the lower accuracy of the analysis. To solve this problem, evaluation of application of silicagel-alumina multi-layer fraction was performed using standard substances and oil-contaminated soils. As a result of application of silicagel-alumina multi-layer fraction cleanup method using standard substances, recovery rates of surrogate standards (5 compounds including Naphthalene-d8) were 83~100% and those of target standards were 75~129%. These were to meet the target values (60~130%) in this study. When used 4% water-silicagel column analyze PAHs in oil-contaminated soils, Some problems were generated for quantitative analysis of PAHs; concentration of PAHs was underestimated due to an upward baseline of internal standard (recovery rate: less than 60%) and overestimated by the lump of peaks which were not purified (the biggest recovery rate: more than 400%). On the other hand, in case of silicagel-alumina multi-layer fraction cleanup method, recovery rate of surrogate standards were 61~101.6%. Therefore this cleanup method was considered a valid method to improve accuracy of analysis of PAHs in oil-contaminated soils.

On study antioxidant effect and aroma component of natural citrus by SC-$CO_2$ Extraction (초임계추출의 천연물 시트러스계의 항산화효과와 향기성분 연구)

  • Lim, Deok-Jum;Chun, Byung-Soo;OH, Dae-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.31 no.2
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    • pp.285-295
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    • 2014
  • Citrus essential oil were extracted from citron peel of cultivated in Gohong (CCP) using environmentally friendly supercritical carbon dioxide method. Antioxidant activity and aroma composition of the essential oils extracted by the SC-$CO_2$ method were evaluated by comparing with those extracted by organic solvent method. Fatty acid composition, DPPH scavenging, and antioxidant activity of the oils obtained by different extraction condition of SC-$CO_2$ method were investigated and their antioxidant activities were compared with commercially available lavender, eucalyptus and tea tree oils. As the results, linoleic acid was most abundantly found from CCP oil extracted by the SC-$CO_2$ method and cis-11,144-eicosadienoic acids was second abundantly found. Radical scavenging ability of DPPH was 98% when the concentration of CCP oil was 50 mg/mL. This scavenging ability increased with the increase of oil concentration. On the other hand, flavonoids content (84 mg/100g) of the CCP oil extracted by the SC-$CO_2$ method was slightly higher than that (75 mg/100g) by hexane extraction. The results, obtained from CCP oil by GC-MS, indicated that, among 66 components, the content of terpenes was 55.8% and limonene was 27.3%.

Assessment on the Extraction Efficiency of Explosive Compounds in Soil for Improving the Working Draft of International Standard (국제표준(안) 개선을 위한 토양 중 화약물질 추출 효율성 평가)

  • Lee, Goon-Taek;Jung, In-Ho;Kim, Bo-Hyun;Kim, Dong-Wook
    • Journal of Soil and Groundwater Environment
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    • v.17 no.1
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    • pp.42-46
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    • 2012
  • The ISO document of ISO/TC/190/SC3/WG11/N11 is a working draft of international standard (WD) dealing with analytical method for the determination of explosives and related compounds using high performance liquid chromatography. The scope of this WD covers the storage of samples, preparing test portion, extraction and instrumentation. The main purpose of this study was to improve the extraction conditions which were already adopted in the WD. For this purpose, mechanical shaking method could be corresponded up to 18 hours of ultrasonic bath extraction in the WD was tested. Methanol was also tested with the intention of being added as an extracting solvent other than acetonitrile in the WD. According to the results, 16 hours of mechanical shaking method showed statistically the same effectiveness as that of 18 hours of ultrasonic bath extraction. In case of extracting solvent, methanol also showed statistically the same extraction capability as acetonitrile for DNB, TNT, 2-A-DNT and 2,4-DNT. However, the recovery rate of TNB with methanol extraction was 40% higher than that of acetonitrile extraction. Through adding mechanical shaking method into committee draft (cf. the next stage draft of the WD during the process for making international standard), ISO standard of analyzing explosives and related compounds in soil would become more useful in dealing with huge number of field samples in the laboratory. In other aspect, adopting methanol as an alternative extracting solvent would be very effective in the terms of exchangeability with GC-ECD/MS method which is being developed by German experts.

Analysis of Chemical Composition of Bulro Kugi (Lycium chinense Mill) Fruit, Leaf, and Root (불로 구기의 부위별 화학적 성분분석)

  • Kim, Eun-Hae;Lee, Joo-Chan;Kim, Hyeon-Wee;Lee, Cherl-Ho;Koh, Kyung-Hee
    • Korean Journal of Food Science and Technology
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    • v.37 no.2
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    • pp.154-163
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    • 2005
  • Chemical and flavor components of Bulro Kugi (Lycium chinense Mill) fruit leaf, and root were compared. Fructose and glucose were detected in fruit and leaf, and sucrose in root, respectively. Citrate was the highest among organic acids in fruits, and malate in leaf and root Capsaicin was detected in leaf and root. Volatile flavor compounds were extracted by simultaneous distillation and extraction method using Likens and Nickerson's extraction apparatus. Concentrated flavor extract was analysed, and 128 compounds, including 22 acids 15 alcohols, 12 aldehydes, 8 esters, 10 furans, 26 hydrocarbons, 4 phenols, 2 pyrroles, 1 pyrazine, and 28 miscellaneous components. were identified by GC and GC-MS. Main volatile compounds were hexadecanoic acid and 2-furancarboxaldehyde in hot-air dried fruit, hexadecanoic acid and 1-hexadecene in fresh fruit, 3, 7, 11, 15-tetranethyl-2-hexadecan-1-ol and hexadecanoir acid in leaf, and hexadecanoic acid in root.

Characteristics of Pesticide Residues in Leafy Vegetables Collected from Wholesale and Traditional Markets in Cheongju (청주지역 도매시장과 재래시장 유통 엽채류 중 농약의 잔류 특성)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Park, Hyo-Kyoung;Park, So-Hyun;Kim, Sun-Ho;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.15 no.4
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    • pp.453-462
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    • 2011
  • This study was carried out to survey the residual characteristics of pesticides and assess their safety. Nineteen agricultural commodities, collected from wholesale and traditional markets in Cheongju. Nineteen agricultural commodities including perilla leaves were collected from the markets on October 29th, 2010. Total 240 pesticides which can be analyzed by multiresidue analysis method by GLC and HPLC were monitored and the pesticides detected were confirmed by GC-MSD and LC-MS. Five pesticides, alachlor, bifenthrin, endosulfan, procymidone and triflumizole, were detected from five samples, such as welsh onion, leek and celery in case of wholesale market and perilla leaves and welsh onion in case of traditional market. Detection rate of 13.2% was obtained as a result of pesticide analysis but 2.6% of the pesticides detected exceeded their maximum residue limits. The estimated daily intakes (EDIs) and maximum permissible intakes (MPIs) of the pesticides detected were less than 26% and 0.05% of their acceptable daily intakes (ADIs) respectively, representing that residue levels of the pesticides detected would be safe.