• 농약과학회지
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• 제9권4호
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• pp.292-302
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• 2005

206종의 농약성분을 신속하게 분석하기 위한 가스크로마토그래피-질량분석기 이용방법을 최적화 하였다. Wide-bore 컬럼을 채택함으로써 기존의 캐필러리 컬럼을 이용할 때에 비해 분리능을 비슷하게 유지하면서도 분석시간이 1/2이상 단축되고, 감도는 더욱 개선되었다. 시료의 성분이 복잡하고 분석대상 농약이 많은 경우에도, EI와 CI 스크리닝 결과를 비교함으로써 방해물질에 의한 허위정보(False Positive)를 상쇄할 수 있었다. 허위정보에 대한 위험이 적어지면서 시험용액의 정제를 간소화 할 수 있어 전체적인 분석과정을 간소화 할 수 있었다. 또한 검출이 예상되는 성분에 대해서만 확인실험을 함으로써 검사시간을 절약하고 검사의 정확도를 향상시킬 수 있었다.

• Archives of Pharmacal Research
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• 제27권7호
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• pp.734-737
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• 2004

5,8-Epidioxycholest-6-en-3-ol (1), cholesterol (2), glycerol 1-palmitate (3) and glycerol 1,3-dioleate-2-stearate (4) were isolated from the methanol extract of the sea urchin Diadema setosum, which was collected from the Halong sea, Vietnam. Chemical structures were established based on extensive 1D, 2D-NMR, FAB-MS, EI-MS spectroscopic data and GC-MS analysis. The NMR spectral data of compound 1 were reassigned by using HMQC and HMBC. Compound 1 was found to have strong cytotoxic effect against various cancer cell lines, such as KB ($IC_{50}$, 2.0 $\mu\textrm{g}$/mL), FL($IC_{50}$, 3.93 $\mu\textrm{g}$/mL), and Hep-2 ($IC_{50}$, 2.4 $\mu\textrm{g}$/mL) by in vitro assay.

• Mass Spectrometry Letters
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• 제3권1호
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• pp.15-17
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• 2012

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

• Preventive Nutrition and Food Science
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• 제3권2호
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• pp.111-118
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• 1998

To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

• Journal of the Korean Wood Science and Technology
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• 제41권6호
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• pp.566-575
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• 2013

주목열매에서 분리한 과육과 씨를 95% EtOH 용액을 사용하여 각각 1.15 kg과 0.94 kg을 유리 용기에 침지하여 추출하고, 농축된 추출용액을 용매의 극성에 따라 n-hexane, dichloromethane, ethyl acetate 및 수용성으로 순차 분획한 후, 동결건조하였다. 혼합물로부터 순수한 화합물을 분리하기 위하여 ethyl acetate 및 수용성 분획에 대하여 Sephadex-LH 20 칼럼크로마토그래피를 실시하였다. 단리된 화합물들의 구조는 flavan 화합물의 경우 $^1H$-NMR, $^{13}C$-NMR 및 EI-MS 스펙트럼을 측정하였으며, 탄수화물은 보다 정확한 구조를 결정하기 위해 COSY, HSQC와 같은 2-D NMR과 LC/MS 스펙트럼을 이용하여 구조를 결정하였다. 또한 구성당 분석을 위해 acid hydrolysis, permethylation을 실시하여 구성당의 성분과 결합위치를 확인하였다. 위의 실험을 통하여 (+)-catechin (1), (-)-epicatechin (2), (+)-gallocatechin (3), (-)-epigallocatechin(4) 및 ${\beta}$-D-fructofuranose-($2{\rightarrow}4$)-O-${\beta}$-D-glucopyranose($1{\rightarrow}4$)-O-${\alpha}$-D-glucopyranose-($1{\rightarrow}2$)-O-${\beta}$-D-fructofuranose (5)의 구조를 결정하였다.

• Food Science and Biotechnology
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• 제14권2호
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• pp.223-227
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• 2005

Anti-inflammatory assay was conducted on 20 kinds of traditional Indonesian medicinal herbs using soybean lipoxygenase (SLO) and hyaluronidase (HAse). Cinnamomun burmanni Bl showed highest anti-inflammatory activity. Ethyl acetate fraction from methanol extract of C. burmanni Bl bark showing high SLO inhibitory activity was isolated using silica gel-60 column chromatography. Two compounds were isolated and purified through preparative HPLC. Through analyses of UV, $^1H-NMR$, $^{13}C-NMR$, EI-MS and $FAB^+-MS$, compounds 1 and 2 were identified as coumarin and 2-hydroxy cinnamaldehyde, respectively, among which 2-hydroxy cinnamaldehyde showed SLO inhibitory activity of $IC_{50}\;=\;60\;{\mu}M$. Both compounds did not exhibit HAse inhibitory activity.

• Food Science and Biotechnology
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• 제14권2호
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• pp.255-258
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• 2005

The compounds, 1-Linoleic-2-olein (1), stigmasterol (2), 1,4-glucopyranosyl-1',4'-glucopyranosyl-1",4"-glucopyranoside (3), 2',3'-diphosphoryl-1'-propanoxy-${\beta}$-D-glucopyranoside (4), 1-Linoleic-3-olein (5), l-(N,N,N-trimethyl ethyl amino phosphoryl)-2,3-dilinolein ion (6) and glyceryl phosphate (7) were isolated and identified from the Mushroom of Pholiota adiposa for the first time by column chromatography, TLC, UV, IR, $^1H$ and $^{13}C$ NMR, EI-MS, and FAB-MS. The compounds 1 and 2 were found to have weak cytotoxicity against P388 murine leukemia cells. However, the compounds 6 and 7 did not show any cytotoxicity.

• Bulletin of the Korean Chemical Society
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• 제28권8호
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• pp.1294-1298
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• 2007

Two new compounds lanast-5,8-dien-3β-ol-27-oic acid-3β-D-glucopyranosyl (4'-1'')-10'',11''-dimethoxy anthracene (1), 2-methoxy-6-(n-nonacontan-5'',6''-dionyl)-11-hydroxy-13-methyl-11β-D-rhamnopyranoside anthracene (2) have been isolated from the hairy root cultures of Catharanthus roseus. Their structures have been elucidated with the help of 500 MHz NMR using one- and two-dimensional NMR in combination with IR, EI/MS, FAB/MS and HRFABMS spectroscopy.

• Archives of Pharmacal Research
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• 제27권10호
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• pp.1020-1022
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• 2004

A new ceramide alomacrorrhiza A was isolated from the ethanolic extract of the plant Alocasia macrorrhiza (L.) Schott. Its chemical structure was elucidated as (2S,3S,4R)-2N-[(2'R)-2'- hydroxy-hexacosanoyl]-tetradecane-1,3,4-triol based on extensive 1D, 2D NMR, EI-MS, FABMS, HR-FAB-MS spectroscopic data and chemical degradation studies.

• 패션비즈니스
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• 제13권3호
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• pp.109-117
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• 2009

To set up the outstanding and scientific dyeing method in making the condensed liquid of pigment obtained from onion skins and the improved reliability, the following basic experiments were performed. The pigment was extracted in the distilled water at $70^{\circ}C$ and methanol at room temperature and then it was analyzed with LC/MS/MS system (Liquid Chomatography/Mass Spectroscopy/Mass Spectroscophy, LIQ Advantage Max, Thermo Finnigan, USA) for its pigmental characteristics. The unrefined silk and refined silk were dyed by making use of the derived pigment in such a way. The chromameter (CR-200, Minolta, Japan) was used to measure the change in surface color in textiles to be dyed by the extracting condition and the color difference ${\Delta}E$ was determined according to the color difference formula CIE LAB through measuring the psychometric lightness L* and chromaticity coordinates a* and b*.