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Analytical Method for Flusulfamide as Benzenesulfonamide Fungicide, Residues in Major Agricultural Commodities (주요 농산물 중 Bezenesulfonamide계 살균제 Flusulfamide의 잔류 분석법)

  • Ahn, Kyung-Geun;Kim, Gi-Ppeum;Hwang, Young-Sun;Kang, In-Kyu;Lee, Young Deuk;Choung, Myoung-Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.1
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    • pp.57-65
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    • 2018
  • BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice, and soybean. The extract was diluted with large volume of saline water and directly partitioned into dichloromethane to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.

Fermentation Characteristics of Kimchi Treated with Different Methods of Green Tea Water Extracts (녹차의 처리방법에 따른 김치의 발효특성)

  • Kim, Mee-Kyung;Kim, Soon-Dong
    • Food Science and Preservation
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    • v.10 no.3
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    • pp.354-359
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    • 2003
  • This study was conducted to investigate the fermentation characteristics of kimchi treated with different methods of water extracts of powdered green tea(GT). Four different kimchis, the SB-kimchi(control) which was not treatment of the extracts, SG-kimchi prepared with Chinese cabbage(CC) salted in 1% GT containing 10% brine, DG-kimchi prepared with CC dipped in 1% GT for 30 min after salting, MS-kimchi prepared with the salted CC mixed with 1% GT containing seasonings. All kimchis was fermented at 10$^{\circ}C$. The pH of treated-kimchis were maintained higher than those of control products during fermentation, but it showed no big difference between each treated groups. Total microbe of SB-kimchi(6.27-9.37 cfu/mL) was higher than those of GT-treated kimchi(5.17-9.20) during fermentation. The ratio of lactic acid bacteria against total microbe was higher than the treated kimchis. Total polyphenol content of kimchi was 52.75 mg% in DG-kimchi, 47.71 mg% in MS-kimchi, 44.89 mg% in SG-kimchi, 30.70 mg% in SB-kimchi on the 5th days of fermentation. Scores of crispy taste of SG- and DG-kimchi on the 5th days of fermentation was 4.03 and 4.01 points, respectively which was higher than control products. Scores of fishy and hot taste of GT-treated kimchi were lower than those of control products during all fermentation periods.

The Study on Analysis Method and Performance Evaluation of Portable GC/MS (휴대용 GC/MS 성능검사 및 분석방법 연구)

  • Park, Yuonshin;Noh, Hyeran;Yang, Heeseon;Seok, Gwanseol
    • Journal of the Society of Disaster Information
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    • v.9 no.3
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    • pp.249-258
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    • 2013
  • Recieved Mar. 06, 2013 Revised Mar. 29, 2013 Accepted Sep. 11, 2013In this study, we evaluated the method performance and the optimum sample injection method of the portable GC/MS(HAPSITE) which were designed to operate on scene of chemical accidents. Chemicals used for performance test were vinyl chloride(VC), methyl chloride(MC), benzene(Bz), toluene(Tol). CRM(Certified Reference Material) Manufactured by KRISS(Korea Research Institute of Standards and Science) was used as the standard gas. The results showed that 1) Among three sample injection methods(Cylinder, Silico canister, and Bag), bag was identified as the most appropriate sample injection method. Bag material and capacity did not significantly affect the results. The most ideal reproducibility occurred at the 2-minute point of the purge time in the loop and tenax methods. 2) Performance evaluation of HAPSITE was conducted. Evaluation items were reproducibility, linearity, method detection limit, etc. Tenax concentration method was appropriate for larger molecules and Carbopack concentration method was suitable for smaller molecules.

Comparison of Sesquiterpenes in Korean and American Ginsengs (한국인삼과 북미산 서양상의 Sesquiterpene 성분 비교)

  • 위재준;신지영
    • Journal of Ginseng Research
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    • v.21 no.3
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    • pp.209-213
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    • 1997
  • Sesquiterpenes of Korean ginseng (Panax ginseng C.A. Meyer, KG) and American ginseng (Panax quinquefolium, AG) were Isolated by simultaneous distillation and extraction (SDE) with 30% methanol and n-hexane or adsorption using C18 Sep-Pak . The sesquiterpenes in KG and AG were compared each other by using TLC and GC/MS. Thin layer chromatogram of KG gave 4~5 spots of terpenes colored by vanillin-sulfuric acid, while AG did one major spot. Total ion chromatogram of KG showed about 30 peaks of sesquiterpene having molecular weight 204. Among these, 9 components such as alloaromadendrene, germacrene B, isocaryophyllene, $\alpha$-neoclovene, ${\gamma}$-muurolene and $\beta$-panasinsene together occupied 81.5% of total sesquiterpenes identified. In AG, however, only 3 components, i.e., isocaryophyllene, $\beta$-bisabolene, $\beta$-sesquiphellandrene occupied 79.3% of total sesquiterpenes identified. Especially isocaryophyllene was a dominant component of AG occupying 56.6%. Eight sesquiterpenes, including alloaromadendrene, germacrene B and $\alpha$-humulene, were not detected in AG. These results indicate that sesquiterpenes could be used as indices for the chemical difference between KG and AG.

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Superconducting Tunnel Junction Detectors for Mass Spectrometry

  • Ohkubo, M.;Zen, N.;Kitazume, T.;Ukibe, M.;Shiki, S.;Koike, M.
    • Progress in Superconductivity
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    • v.14 no.2
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    • pp.77-81
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    • 2012
  • With conventional mass spectrometry (MS), ions are separated according to mass/charge (m/z) ratios. We must speculate the z values to obtain the m values. Superconducting tunnel junction (STJ) detectors can solve this problem, and true mass spectrometry becomes possible instead of m/z spectrometry. The STJ detectors were installed in MS instruments with a variety of ion sources. As an example, we report fragmentation analysis of a non-covalent protein complex of hemoglobin.

Studies on Chemical Structure Determination of Polygonatum sibiricum Extracts(I) (황정(黃精) 추출물의 화학구조 결정에 관한 연구(I))

  • 신동수;윤중호;박주희;권기락;안철진;주우홍;강진호;문병호
    • Journal of Life Science
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    • v.9 no.2
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    • pp.207-211
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    • 1999
  • Biologically active compounds in Polygonatum sibiricum were extracted using organic solvents as hexane, CHCl$_3$, n-butanol corresponding each component. Compound I was purified from hexane layer and the chemical structure of compound I was characterized using 1H-NMR, 13C-NMR, DEPT135, COSY, HMQC, HMBC spectrum and MS-spectrum. Consequently, the chemical structure of compound I was determined as 9,12-(9E,l2E)-octade cadienoic acid.

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Studies on Chemical Structure Determination of Polygonatum sibiricum Extracts(II) (황정(黃精) 추출물의 화학구조 결정에 관한 연구(II))

  • 신동수;김흥재;조수동;권기락;안철진;주우홍;강진호;문병호
    • Journal of Life Science
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    • v.9 no.2
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    • pp.212-215
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    • 1999
  • Biologically active compounds in Polygonatum sibiricum were extracted using organic solvents as hexane, CHC1$_3$, n-butanol corresponding each component. Compound II was purified from hexane layer and the chemical structure of compound II was characterized using IH-nmr, 13C-nmr, DEPT135, COSY, HMQC, HMBC spectrum and MS-spectrum. Consequently, the chemical structure of compound II was determined as 2-Hydroxy-3-(9,12-(9E,12E)-Octadecadienoyloxy) propanoic acid.

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Survey of Inositol in Infant Formula

  • Patel, A.;Ditiatkovski, M.;Kennedy, L.;Oglobline, A.;Choi, N.;Richardson, G.
    • Mass Spectrometry Letters
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    • v.7 no.1
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    • pp.12-15
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    • 2016
  • Results of free and bound myo-inositol in infant formula (IF) are presented. Inositol was analyzed by HILIC ultra-performance liquid chromatography coupled with mass spectrometer. The levels of free myo-inositol in 27 Australian and 4 EU originated IF samples were 300-600 mg/kg of powder or 1.6-3.1 mg/100 kJ. The amount of bound inositol in lipid fraction of IF was, on average, 10% of free myo-inositol.

Decomposition of Acetonitrile by Planar Type Dielectric Barrier Discharge Reactor (평판형 유전체 장벽 방전 반응기에서 Acetonitrile의 분해 특성)

  • 송영훈;김관태;류삼곤;이해완
    • Journal of the Korea Institute of Military Science and Technology
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    • v.5 no.3
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    • pp.105-112
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    • 2002
  • A combined process of non-thermal plasma and catalytic techniques has been investigated to treat toxic gas compounds in air. The treated gas in the present study is $CH_3$CN that has been known to be a simulant of toxic chemical agent. A planar type dielectric barrier discharge(DBD) reactor has been used to generate non-thermal plasma that produces various chemically active species, O, N, OH, $O_3$, ion, electrons, etc. Several different types of adsorbents and catalysts, which are MS 5A, MS 13X, Pt/alumina, are packed into the plasma reactor, and have been tested to save power consumption and to treat by-products. Various aspects of the present techniques, which are decomposition efficiencies along with the power consumption, by-product analysis, reaction pathways modified by the adsorbents and catalysts, have been discussed in the present study.

Dibenzocyclooctene lignan compounds isolated from the fruits of Schisandra chinensis Baill

  • Piao, LongZhu;Lee, Yu-Joung;PhamPhu, ThanhTruc;Shin, Jae-Kyoon
    • Natural Product Sciences
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    • v.11 no.4
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    • pp.248-252
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    • 2005
  • Schisandra chinensis Baill. (Shisandraceae) is used commonly in traditional Korean herbal medicine. One new dibenzocyclooctene lignan compound, benzoylgomisin Q, was found, for the first time, in the fruits of Schisandra chinensis Baill., together with five known lignan compounds; schisandrin, gomisin A, gomisin G, deoxyschisandrin, and gomisin N, using an ESI-positive MS-preparative HPLC auto-purification system. The structures of these compounds were determined via UV, MS, and NMR spectral studies.