• Bulletin of the Korean Chemical Society
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• 제22권7호
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• pp.685-688
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• 2001

A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of benzidine (BZ), N-acetyl benzidine (ABZ) and N,N-diacetyl benzidine (DABZ) in rat urine. BZ, ABZ and DABZ were extracted from urine at pH 8 with ethyl ether. Conjugated urinary metabolites were extracted at pH 8 after hydrolysis with 1 M HCl for 30 min at 100 $^{\circ}C.$ The dried extract was dissolved in 100 ${\mu}{\ell}$ of ethylacetate and then injected in gas chromatography-mass spectrometric (GC-MS) system without further purification or modification. BZ, ABZ and DABZ have good chromatographic properties and offer very sensitive response for the EI-MS (SIM) without any derivatization. The recoveries for BZ, ABZ and DABZ were about 98.0, 81.8 and 71.4%, respectively, at pH 8.0 and the concentration of 5.0 ng/mL. The coefficients of variation of BZ and ABZ were less than 9.5% from 0.1 to 100 ng/mL and that of DABZ was less than 13% in the same concentration range. The detection limits of the assay were 0.01 ng/mL for both BZ and ABZ, and 0.05 ng/mL for DABZ in urine or plasma 1.0 mL.

• 농약과학회지
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• 제2권3호
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• pp.79-84
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• 1998

콩나물중 carbendazim 잔류분을 정량하고 확인할 수 있는 새로운 분석법을 확립하고자 tandem HPLC(UV & FL) 및 APcI를 source로 사용한 LC/MS를 이용하였다. 이를 위해 FL(fluorescence) 검출기를 UV(ultraviolet) 검출기와 나란히 연결하여 UV 검출기의 경우 280 nm 파장을 그리고 FL 검출기의 경우는 excitation파장과 emission파장을 각각 280 mn와 310 nm로 설정하였다. 분석결과 carbendazim의 검출한계는 $0.04{\mu}g/kg$이었다. 콩나물에 carbendazim을 0.5, 1.0 및 2.0 ppm 수준으로 첨가하여 회수율을 측정한 결과 그 평균값은 89.1%이었다. APcI source를 사용한 LC/MS 질량스펙트럼 방법은 콩나물중 carbendazim 잔류분을 최종 확인할 수 있었다. APcI LC/MS 방법은 전자충격에 의한 질량스펙트럼에 비해 훨씬 간단한 fragment를 형성할 뿐 만 아니라 carbendazim의 경우 m/z 133, m/z 159, m/z 191($M^{+}$)의 전형적인 fragment 이온을 형성하므로, 이 방법을 병행한다면 콩나물중 carbendazim 잔류분을 효과적으로 확인할 수 있을 것으로 사료되었다.

• Applied Biological Chemistry
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• 제32권4호
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• pp.344-349
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• 1989

GC/MS를 이용하여 오미자의 chloroform-methanol 추출물로부터 11종의 lignan 성분을 동정하였다. GC column은 SPB-1 fused silica capillary $(0.25mm\;ID{\times}30m,\;Supelco)$를 사용하였고 column oven의 온도는 $200^{\circ}C$부터 $300^{\circ}C$까지 분당 $4^{\circ}C$씩 승온하였으며 MS의 ionization voltage는 70eV (El mode)이었다. 동정된 lignan 성분은 gomisin J, deoxyschizandrin, gomisin N, schizandrin, wuweizisu C, gomisin A, angeloylgomisin H, tigloylgomisin H, angeloylgomisin Q, gomisin B 및 benzoylgomisin H이었으며, GC chromatogram 상에서 이들 화합물의 분리상태는 양호하였다.

• Applied Biological Chemistry
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• 제39권6호
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• pp.506-511
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• 1996

우리나라에서 식용으로 이용되는 진달래꽃으로부터 6성분의 폐놀산 화합물이 분리동정되었다. 이들 화합물의 구조는 IR, UV, $^{1}H$과 $^{13}C$ NMR, FAB-MS, ES-MS와 EI-MS에 의해 얻어진 분광학적인 결과에 근거하여, chlorogenic acid, 3,5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, caffeic acid, ferulic acid, p-coumaric acid인 것으로 밝혀졌다. Chlorogenic acid (0.2 g)는 ethyl acetate과 ethyl ether 분획에 동시에 함유되어 있었고, polyamide C-200 관 크로마토그래피법, 분취용 박층크로마토그래피법, 재결정법, Sephadex LH-20 관 크로마토그래피법을 통해서 양 구분으로부터 최종적으로 회수된 총 페놀산 함량 (0.52 g)의 38.5%를 차지하였다. 항산화성은 티오시안산철의 존재하에서 리놀레산의 에타놀 용액 중에서 측정되었다. 항산화능은 p-coumaric acid<${\alpha}-tocopherol$

• Food Science and Biotechnology
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• 제16권3호
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• pp.349-354
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• 2007

The objectives of this study were to systemically identify phenolic compounds in roasted wild ginseng (Panax ginseng C.A. Meyer) leaves and investigate their radical scavenging activities. Seven phenolic compounds were identified by NMR (H, C, COSY, HMQC, HMBC) and mass (EI-MS, FAB-MS) analyses: 5-caffeoylquinic acid, kaempferol, quercetin, 3,4-dihydroxy-benzoic acid, 4-hydroxy-benzoic acid, 3-(3,4-dihydroxyphenyl)-2-propenoic acid, and 3-(4-hydroxy-3-methoxyphenyl)-2-propenoic acid. Their concentrations ranged from 0.4 (3,4-dihydroxy-benzoic acid) to 7.5 mg (kaempferol) per 100 g of roasted leaves. Among these compounds, 5-caffeoylquinic acid, kaempferol, and quercetin were found exclusively in the leaf portions of the ginseng plants. When their antioxidant activities were measured by DPPH and superoxide anion radical scavenging activity, quercetin, and kaempferol were most effective.

• Toxicological Research
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• 제30권2호
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• pp.109-116
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• 2014

Glucosinolates (GLSs) are abundant in cruciferous vegetables and reported to have anti thyroidal effects. Four GLSs (sinigrin, progoitrin, glucoerucin, and glucotropaeolin) were administered orally to rats, and the breakdown products of GLSs (GLS-BPs: thiocyanate ions, cyanide ions, organic isothiocyanates, organic nitriles, and organic thiocyanates) were measured in serum. Thiocyanate ions were measured by colorimetric method, and cyanide ions were measured with CI-GC-MS. Organic isothiocyanates and their metabolites were measured with the cyclocondensation assay. Organic nitriles and organic thiocyanates were measured with EI-GC-MS. In all treatment groups except for progoitrin, thiocyanate ions were the highest among the five GLS-BPs. In the progoitrin treated group, a high concentration of organic isothiocyanates (goitrin) was detected. In the glucoerucin treated group, a relatively low amount of goitrogenic substances was observed. The metabolism to thiocyanate ions happened within five hours of the administration, and the distribution of GLSs varied with the side chain. GLSs with side chains that can form stable carbocation seemed to facilitate the degradation reaction and produce a large amount of goitrogenic thiocyanate ions. Because goitrogenic metabolites can be formed without myrosinase, the inactivation of myrosinase during cooking would have no effect on the anti-nutritional effect of GLSs in cruciferous vegetables.

• 생약학회지
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• 제27권2호
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• pp.91-95
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• 1996

In the course of searching for acetylcholinesterase inhibitors from crude drugs, it was found that total MeOH extract of Corydalis Tuber showed significant inhibitory effect on acetylcholinesterase. To isolate acetylcholinesterase inhibitors from Corydalis Tuber, total MeOH extract of the the crude drug was subjected to activity guided fractionation. The MeOH extract was suspended in water and fractionated with methylene chloride and subjected to acid-base fractionation. Silica gel column chromatography of the basic fraction which showed significant inhibitory effect on acetylcholinesterase was carried out and 5 subfractions (1-5) were obtained. From subtraction 4, compound I was isolated. The structure of isolated compound I was identified by spectroscopic parameters of $^1H-NMR$, $^{13}C-NMR$, EI-MS and FAB-MS. The compound I was identified as berberine. It was found from the Lineweaver-Burk plot that berberine was a reversible and specific inhibitor of acetylcholinesterase having 90% inhibitory effect at the concentration of $2.5{\mu}M$.

• 한국응용약물학회:학술대회논문집
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• 한국응용약물학회 1998년도 Proceedings of UNESCO-internetwork Cooperative Regional Seminar and Workshop on Bioassay Guided Isolation of Bioactive Substances from Natural Products and Microbial Products
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• pp.134-134
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• 1998

The modulation of glycosidase activity by inhibitors is of great interest. Such compounds have been shown to be important tools in mechanistic studies on glycohydrolase as well as having promising therapeutic application. An ${\alpha}$-glucosidase inhibitor was isolated from culture filterates of Penicillium sp. The inhibitor was active against ${\alpha}$-glucosidase isolated from yeast and porcine small intestine. However, it showed no inhibition to Aspergillus ${\alpha}$-galactosidase, Escherichia coli ${\beta}$-galactosidase, and jack bean ${\alpha}$-mannosidase. The inhibitor was highly soluble in ether, methanol and chloroform. The inhibitor was purified using silica gel, Sephadex LH-20 column chromatography and reverse-phase HPLC. The inhibitory compound designated PA-7(IC$\sub$50/=35$\mu\textrm{g}$) was obtained as white powder. The structure of PA-7 was determined with spectroscopic data of EI-MS, FAB-MS, $^1$H, and $\^$13/C NMR. The inhibitor has a diketopiperazine moiety.

• Bulletin of the Korean Chemical Society
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• 제28권2호
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• pp.229-234
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• 2007

One new compound, 3,7,11,19,23,27-hexamethyl-15-hydroxymethylene-n-octacos-5,8,20-triene-10β,18α- diol-10β-D-glucopyranoside (1), along with the three known compounds, 3-epibetulinic acid (2), n-pentadecanyl octa-dec-19-en-oate (3) and β-sitosterol (4) were isolated from the methanolic extract of the cultured Catharanthus roseus hairy roots. The structures of the one new and three known compounds were elucidated using one- and two-dimensional NMR in combination with IR, EI/MS, FAB/MS. To the best of our knowledge, 3,7,11,19,23,27-hexamethyl-15-hydroxymethylene-n-octacos-5,8,20-triene-10β,18α-diol-10β-D-glucopyranoside, 3-epibetulinic acid and n-pentadecanyl octa-dec-19-en-oate were identified for the first time from the hairy roots of C. roseus.

• Journal of Applied Biological Chemistry
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• 제51권1호
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• pp.17-19
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• 2008

Isoflavanone has been synthesized from the reduction of isoflavone in nearly quantitative yield. Isoflavone with seven equivalents of ammonium formate in the presence of Pd/C in ethanol under $N_2$ atmosphere exclusively produced the two-electron reduced product in two hours. It was characterized by various spectroscopic methods, including UV-VIS, EI-MS, $^1H$-NMR, $^{13}C$-NMR and $^1H$, $^1H$-COSY. The racemic mixture was separated by Sumi-Chiral column chromatography and the absolute configurations of the enantiomers were characterized by circular dichroism spectroscopy.