• Title/Summary/Keyword: Chromatogram

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Identification of Higenamine nad its Metabolites in Rat by Gas Chromatography/Mass Spectrometry

  • Ryu, Jae-chun;Song, Yun-Seon;Kim, Myung-Soo;Cho, Jung-Hyuck;Yunchoi, Hye-Sook
    • Archives of Pharmacal Research
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    • v.16 no.3
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    • pp.213-218
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    • 1993
  • ($\pm$)-Higenamine is known as a cardiotonic principle of aconite root (root of Aconitum spp., Ranunculaceae). A simple and sensitive detection method for higenamine was developed by using gas chromatography-mass spectrometry (GC/MS). The recovery of higenamine after extraction and concentration with XAD-2 resin column was around 95% from rat biological fluids such as bile, plasma and urine. The limits of detection of higenamine in these biological fluids were approximately 0.1 ng/ml each. It has well been suggested that tetrahydroisoquinolines possessing catechol moiety such as higenamine should be subjected to the catechol-O-methyl transferase (COMT) activity in vivo. We detected two major peaks of presumed metabolites of higenamine in the total ion chromatogram obtained from the rat urine sample after the oral adminstration of ($\pm$)-higenamine. The scan mass spectrum of one of the metabolties coincided with those obtained from coclaurine $(C_6$-O-methyl higenamine) and those of the other metabolite are suggestive of isococlaurine $(C_7$-O-methyl higenamine).

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Purification of Anti-allergic Compound from Mori Cortex Radicis Extract (상백피 추출물 중의 항알러지 활성 성분의 분리)

  • Lee, Eun-Ju;Chae, Ok-Hee;Lee, Moo-Sam;Lee, Hern-Ku;Huh, Hoon
    • YAKHAK HOEJI
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    • v.42 no.4
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    • pp.395-402
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    • 1998
  • Mori Cortex Radicis, the root bark of mulberry tree, has been used in the treatment of bronchial asthma and other lung diseases in traditional medicine. There was a recent repor t that the water soluble part with molecular weight of above 10,000 has anti-allergic activity. Therefore, we intended to isolate and purify the anti-allergic compound from hot water extract of the Mori Cortex Radicis. Crude extract of Mori Cortex Radicis was prepared by hot-water extraction, and anti-allergic compound was further purified by alcohol precipitation, successive ultrafiltration, anion exchange chromatography and gel filtration chromatography. This compound had homogeneity which was shown by the sharp single peak in HPLC chromatogram (TSK-GEL G400OPW column, RI detector). The molecular weight of the compound was estimated as 23Kda on the basis of calibration curve plotted against protein standards. This compound was identified as complex of sugar, protein and lignin (19.2: 5.9: 72.7), and proteolysis could not decrease the anti-allergic activity but mild delignification decreased the activity remarkably. Therefore, we concluded that the anti-allergic compound of Mori Cortex Radicis was a lignin-carbohydrate complex.

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Effect of Linker for Immobilization of Glutathione on BSA-Assembled Controlled Pore Glass Beads

  • Chen, Li-Hua;Choi, Young-Seo;Park, Jung-Won;Kwon, Joseph;Wang, Rong-Shun;Lee, Tae-Hoon;Ryu, Sung-Ho;Park, Joon-Won
    • Bulletin of the Korean Chemical Society
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    • v.25 no.9
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    • pp.1366-1370
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    • 2004
  • Controlled pore glass bead was modified with bovine serum albumin (BSA), and glutathione (GSH) was immobilized through three kinds of linkers on top of BSA. Bis(3-sulfo-N-hydroxysuccinimide suberate) sodium salt $(BS^3)$, N-hydroxysuccinimide 3-(2-pyridyldithio)propionate (SPDP), or N-hydroxysuccinimide 4-maleimidobutyrate (GMBS) was introduced into the BSA-bound matrix. Subsequently, GSH was immobilized by addition of thiol side chain into the maleimido moiety, replacing a disulfide group, or formation of an amide group upon releasing 3-sulfo-N-hydroxysuccimide group. It was observed that conjugation methodology played a critical role for activity of the immobilized GSH. SDS-PAGE chromatogram showed that the matrix of glutathione immobilized on BSA through GMBS manifested high selectivity towards glutathione-S-transferase (GST) in cell lysate.

Characterization of Aroma Components in Barley Bran Sauce Using Statistical Analysis

  • Choi, Ung-Kyu;Kim, Mi-Hyang;Kwon, O-Jun;Lee, Tae-Jong;Lee, Nan-Hee
    • Food Science and Biotechnology
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    • v.16 no.1
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    • pp.23-28
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    • 2007
  • A linear correlation was found by stepwise multiple regression analysis between the sensory score of barley bran sauce aroma and the absolute gas chromatogram (GC) data transformed with square root. In spite of highly significant relationship between the quantity of the peak and the sensory score, it is difficult to estimate the aroma quality of barley bran sauce samples on the basis of only one peak. Peak 29 (methyl 9,12,15-octadecatrienoate) contributed most to the aroma of barley bran sauce. This was followed by 27 (methyl 9,12-octadecadienoate), 28 (ethyl 9,12-octadecadienoate), 12 (phenyl acetaldehyde), and 9 (methyl furfural) in terms of absolute value. When it was calculated using absolute value transformed by square root, peak 28 (ethyl 9,12-octadecadienoate) made the highest contribution to the aroma of barley bran sauce of among the peaks. It was followed by 31 (9,12-octadecadienoic acid), 27 (methyl 9,12-octadecadienoate), 12 (phenyl acetaldehyde), and 29 (methyl 9,12,15-octadecatrienoate).

Toxin Produced by Colletotrichum falcatum Causing Red Rot of Sugarcane

  • Saikia, R.;Azad, P.;Arora, D.K.
    • Mycobiology
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    • v.32 no.4
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    • pp.149-154
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    • 2004
  • Toxin produced by Colletotrichum falcatum Went, the incitant of red rot of sugarcane was isolated, purified and assayed to determine host specificity and identify its chemical nature. The toxin was found to be not host specific as it inhibited germination of various seeds(gram, greengram, blackgram, pea, cowpea, rice and sugarcane) as well as different seedlings viz. tomato, coriander, pea and rice. The toxin consists of two distinct fraction-one fraction having $R_f$, value at 0.36 producing identical red rot lesion when inoculated at leaf midrib of sugarcane, and the other having $R_f$, value at 0.72 not showing any red rot lesion. Chromatogram of high performance liquid chromatography(HPLC) of the red rot lesion causing fraction showed a sharp peak at 1.62 min of retention time(RT), and spectral analysis indicated the presence of following chemical $CH_3$ - groups-C-H, C=O, C-N, $-CH_3,\;-CH_2$ -CH and molecular mass of the compound was 203. - ($M^+,\;C_{11}H_{11}N_2O_2$).

Sorption Behavior of 1-Methylcyclopropene on Adsorbing Agents for Use in Extending the Freshness of Postharvest Food Products

  • Lee, Youn-Suk;Shin, Han-Seung
    • Food Science and Biotechnology
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    • v.15 no.4
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    • pp.572-577
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    • 2006
  • The physiochemical interactions of 1-methylcyclopropene (1-MCP) and adsorbing agents can be described using a very powerful tool, inverse gas chromatography (IGC). Sorption behavior of 1-MCP on various adsorbing agents was assessed using the profile peaks of 1-MCP at an infinite dilution concentration using the IGC technique. Chromatogram peaks of 1-MCP adsorption were not observed for the adsorbing agent activated carbon. The forms of sorption isotherms followed Henry's law, and behaved according to the binding site theory. Specific retention volume and distribution coefficients for 1-MCP on the adsorbing agents were determined at 50, 60, 70, and $80^{\circ}C$, respectively. Silica gel had a much higher number of binding sites for 1-MCP compared to Tenax-TA and activated clay agents. Meanwhile, activated carbon proved to be a very strong binding agent for 1-MCP based on 1-MCP efficiency experiments on the selected adsorbing agents. However, as a proper means of delivering 1-MCP molecules to fresh food products, activated carbon is not fit for the binding and release of 1-MCP gas under dry or high humidity conditions because activated carbon has a strong affinity for 1-MCP, even when treated with distilled water.

Changes on the Components of Free Polysaccharide from Cell Wall of Persimmon Fruit by Treatments of Cell Wall Degrading Enzymes (세포벽분해효소의 처리에 따른 감과실의 세포벽 유리 다당류의 변화)

  • 신승렬;김미현
    • Food Science and Preservation
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    • v.2 no.1
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    • pp.173-183
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    • 1995
  • This paper was carried out to investigate changes in chromatograms of polysacctatides and soluble pectins on Sephadex G-50 and non-cellulosic neutral sugars of polysaccharides isolated from cell wall of persimmon fruits treated with polygalacturonase and $\beta$-galactosidase in vitro. The chromatogram pattern of soluble pectins extracted from cell wall treated with $\beta$-galactosidase on Sephacryl S-500 column were similar to those of untreatment, but contents of soluble pectins treated with $\beta$-galactosidase were different from those of untreatment. The patterns of chromatograms In soluble pectins extracted from cell wall treated with polygalacturonase were more complex and lower molecular polymer than those of other cell wall-degrading enzyme treatments. Non-cellulosic neutral sugar of polysaccharides in fraction I of soluble material treated with polygalacturonase was rhamnose, those in fraction II were similar to those in fraction III and contents of arabinose, xylose and glucose were higher than contents of other non-cellulosic neutral sugars. Non-cellulosic neutral sugars of polysaccharides in fraction I in soluble material by $\beta$-galactosidase treatment were rhamnose, arabinose, galactose and mannose. Content of glucose of polysaccharides in fraction II was higher than that in fraction I . Non-cellulosic neutral sugars treated with mixed enzyme were rhamnose, fucose, arabinose, xylose, mannose, galactose and glucose. Compositions of non-cellulosic neutral sugars of polysaccharides in fraction I were similar to those in fraction II and III.

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Studies on unknown methylated compounds of non-histone nuclear protein

  • Lee, Hyang-Woo;Hong, Sung-Youl;Kim, Sang-Duk;Paik, Woon-Ki
    • Archives of Pharmacal Research
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    • v.8 no.3
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    • pp.149-157
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    • 1985
  • The HCL hydrolyzate of the non-histone protein fractionated from the rat liver nuclei which have been incubated inthe presence of S-adenosyl-L-[methyl-$^{14}C$ ]-methionine shows at least four unidentified radioactive peaks on a basic amino acid analysis chromatogram. One of these unknown compounds (designated as compound 3) is also formed by the rat liver homogenated with the exogenous addition of an appropriate protein substrate. Since boiled rat liver homogenate or fresh homogenate in the absence of an exogenous protein substrate failed to form compound 3, its formation can be considered to be enzyme-catalyzed. The enzyme which yields compound 3 shows a preference of protein substrate in the order of reductively methylated hemoglobin > native > histone type II-A. The rat enzyme is nuclear in location associated with chromatin, and exhibits the highest activity in the liver among various rat organs. A compound 3-forming enzyme is also present in Neurospora crassa, since endogenous formation of the compound 3 can be demonstrated with the crude extract of this mold. The chemical identity of compound 3 is not yet known. However, it resisted to the following treatments; 6 N HCL and 0.1 N Na NaOH hydrolysis at $110^{\circ}C$, OR L-amino acid oxidase.

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Development of primary reference gas mixtures of 18 volatile organic compounds in hazardous air pollutants (5 nmol/mol level) and their analytical methods

  • Kang, Ji Hwan;Kim, Yong Doo;Lee, Jinhong;Lee, Sangil
    • Analytical Science and Technology
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    • v.34 no.5
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    • pp.202-211
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    • 2021
  • Volatile organic compounds (VOCs) in hazardous air pollutants (HAPs) have been regulated by the Air Pollution Control Act (1978) and their atmospheric concentrations have been monitored in 39 monitor sites in Korea. However, measurement standards of volatile organic compounds (VOCs) in HAPs at ambient levels have not been established in Korea. Primary reference gas mixtures (measurement standards) at ambient levels are required for accurately monitoring atmospheric VOCs in HAPs and managing their emissions. In this study, primary reference gas mixtures (PRMs) at 5 nmol/mol were developed in order to establish primary national standards of VOCs in HAPs at ambient levels. Primary reference gas mixtures (PRMs) were prepared in pressurized aluminum cylinders with special internal surface treatment using gravimetric method. Analytical methods using gas chromatography-flame ionization detector (GC-FID) coupled with a cryogenic preconcentrator were also developed to verify the consistency of gravimetrically prepared HAP VOCs PRMs. Three different columns installed in the GC-FID were evaluated and compared for the retention times and separation of eighteen target components in a chromatogram. Results show that the HAP VOCs PRMs at 5 nmol/mol were consistent within a relative expanded uncertainty (k=2) of less than 3 % except acrylonitrile (less than 6 %) and the 18 VOCs were stable for 1 year within their associated uncertainties.

Flavonoids analysis in leaves and fruits of Korean mulberry cultivar, Baekokwang having white fruits

  • Lee, Sora;Kim, Soo Hyun;Koo, Bonwoo;Kim, Hyun-Bok;Jo, You-Young;Kweon, HaeYong;Ju, Wan-Taek
    • International Journal of Industrial Entomology and Biomaterials
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    • v.41 no.2
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    • pp.45-50
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    • 2020
  • Morus alba has white and/or purple fruits with a very sweet taste and low acidity. Most Korean mulberry trees have purple fruits. However, Baekokwang is a unique mulberry genetic resource in Korea with white fruits. In this study, flavonoids contents of Baekokwang mulberry leaf and fruit were analyzed using ultrahigh performance liquid chromatography coupled with diode array detection and quadrupole time-of-flight mass spectrometry (UPLC-DAD-QTOF/MS) technique. UPLC-DAD-QTOF/MS chromatogram showed that 15 flavonoids and 9 flavonoids were isolated and identified from the mulberry leaf and fruit. Total flavonoids contents of Baekokwang leaves and fruits were 812.7 mg and 35.0 mg, respectively. Baekokwang leaves had 4 major flavonoids including quercetin 3-O-(6"-O-malonyl) glucoside, 235.3 ppm, kaempferol 3-O-(6"-O-malonyl) glucoside, 132.3 ppm, kaempferol 3-O-rutinoside (nicotiflorin), 108.1 ppm, and quercetin 3-O-rutinoside (rutin), 103.8 ppm. Baekokwang fruits had 3 major flavonoids including quercetin 3-O-(6"-O-malonyl) glucoside, 13.0 ppm, quercetin 3-O-rutinoside (rutin), 7.8 ppm, and kaempferol 3-O-rutinoside (nicotiflorin), 5.7 ppm. From the above results, mulberry leaves have rich flavonoids compared to its fruits.